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Fancy yourself a bold Gaijin investigating Meiji-era Japan (and fucking a few geisha along the way)? Or perhaps you've dreamt of being a football coach (with easy access to willing legal cheerleaders)? Does a trip to visit your favorite ER nurse send your blood rushing straight to Mr. Happy? POV Fantasy aims to scratch any pornographic itch you've been having by inviting today's boldest ladies to dress up and act the part of [DREAM WOMAN] in your very own sordid [LOCATION or SCENARIO] fantasy. It's the next best thing to living it, so indulge!
Your own penis might have seen you through some tough times and even managed to satisfy a woman or two. Had you been born an inanimate (but otherwise very happy) sex toy, though, you'd be expanding the pussies of porn's babiest babes at New Sensations' most depraved masturbation site, Stretched Out Snatch. Pornstars lining up to throw every dildo, vibrator, and molded fist in Southern California up their wahoos for your entertainment? You're in, right?
Grabbing a few friends and heading out for some brewskis at the local sports bar is fine if you're into light social engagements, but those truly outgoing and adventurous souls might require something a little extra. Gang AV shows how the more gregarious Japanese get their social kicks and it's an entirely hardcore affair. Hosting over 300 exclusive threesomes, gangbang, and orgy scenes rife with face-pasting bukakke cumshots, exploratory anal digging, and as many squealing, writhing women as you can handle, Gang AV makes a compelling argument for group bonding.
You and I might urinate everyday, flushing our yellow waste liquid straight down the drain, thinking nothing of its erotic potential. The women and men seen bathing and cavorting in VIPissy's scenes of intense urine fetishism, however, know full well how much can be enjoyed from a simple pissing. Whether letting themselves go into a lover's mouth or instead acting as the urinary receiver, VIPissy's European babes are as dripping wet and thoroughly adventurous as, well, perhaps you.
Submissiveness, porcelain skin, restrictive vaginal cavities, a fondness for designer handbags… These might be things that spring to mind when you think of a Japanese woman, but you're not likely to think of huge milk-filled bosoms bouncing around and knocking some guy in the face as he fills their owner's pussy with a steaming load. Such bosoms, however, are the bread and butter of AV Tits! Inside this site you'll find almost 300 scenes are hardcore jug-fucking, nipple-pinching, mothers-milk-squirting sex as only the Japanese can deliver. Now, doesn't that sound a treat?
Farting used to be something that would undoubtedly cause an otherwise promising courtship to end abruptly. Nowadays, though, with all kinds of sexual perversions making inroads to the mainstream, perhaps the passing of gastric gasses will pop up in a future Miley single. Ok, perhaps not, but FartDom is at least trying to bring aggressively, dominantly farting women closer to the AVNs. Kudos to you, FartDom for embarking on what most would see as an impossible mission. Kudos and good luck! (Something tells me you're gonna need it.)
Playboy continues its dominance of the softcore realm with Playboy Plus, a site that serves up thousands upon thousands of incredibly stimulating galleries, centerfolds, steamy short movies, and compilations celebrating the bustiest, blondest, boldest, and most bodacious Playboy bunnies and models of all time. A relatively simple site aiming not at tricks and toys, but at your largest erogenous receptor (your mind via your eyes), Playboy Plus doesn't flit around, instead showcasing its multitude of truly incredible women.
If you're thinking of going back to college to complete your degree but remain unconvinced of the fun you'll supposedly have in the dorms, perhaps Dick Dorm will change your mind and speed up your enrollment. Presenting group sex more wild that anything you can imagine, Dick Dorm is an all-male, all-college-themed hardcore extravaganza that must be seen (and heavily criticized) at least once. After all, it might have plenty of dicks dipping into shot glasses beneath blacklights, but professionalism has never been heavy on Dick Dorm's mind.


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Carving comrades
The name of Harlan Englund's shop, "He Me We," seems fitting. Because the dusty woodcarver's haven in Evansville isn't just a place - it's people. And friendships. And camaraderie.
But it certainly isn't about making a profit.
"It's a non-profit organization, I guarantee you," Englund said with a grin. "A bunch of baloney goes on here. There might be five or 10 guys here having coffee and talking politics."
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Since business partners Jason Green and Greg Watkins set out to revive Paradise Visuals in 2005, there have been many obstacles in the way. Things started strong when the first title they released: Ginger Lynn the Movie won the AVN Award for best classic DVD. The release was followed up by Wpink TV and John Holmes final film, the Devil in Mr. Holmes. The Paradise team even found time to shoot their first new movie in nearly 15 years, ''The Make Up''
It was after acquiring the exclusive rights to John Wayne Bobbitt Uncut: That things went awry.
''We made a deal with a company to distribute our titles and it was a waste of time and money to say the least. That deal all but killed Paradise Visuals for two years. Said Jason Green - co owner of Paradise Visuals.
''We release these movies, because we want preserve the classic history of the adult business. We are probably the only company left, whose catalog has still never been released on DVD'' Green added.
Paradise Visuals still has over 60 movies that have never been released outside VHS. Currently Paradise is in the process of re-launching a brand new website, where the entire catalog will be available for purchase. The company also just released the lost classic Getting L.A.d starring Nina Hartley and Amber Lynn and Paladin Video is helping with distribution.
Paradise Visuals co-owner Jason Green has kept busy in the industry writing & directing ''Sunnys Slumber Party'' for Sun Lust Pictures and distributed by Vivid, under his nom de plum Spencer Benedict.
''I said the only way I would direct a movie outside Paradise Visuals was if I could shoot a feature and have total creative control and thats what Sunny Leone and Sun Lust Pictures gave me.''
''I think we made a great comedy, its a throw back to when movies had a fun story. I even got to include some of my classic friends, Ron Jeremy and Randy West.''
Green is currently developing another project for Sunny Leone in addition to a new Paradise Visuals feature.
Distributors interested in carrying Getting L.A.d and other Paradise Visuals DVDs should contact Paladin Video at 1 800 228 8395.
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text:
Pronunciation: 基诺族
Added on: 2010-05-17 Listened: 3 timesin: 民族
Pronunciation in Cantonese [yue]
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基诺族 pronunciation in Mandarin Chinese [zh]
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- Random word: 詳情
by Yandex Translate English translation:
基诺族 = Based commitment to racial
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Product Details
  A fest of trees grows on this beautiful comforter set that takes a fresh approach to spring. Take a look at our blankets and bedspreads for even more stylish ways to stay warm in bed. • A BrylaneHome Exclusive®! • Available in 4 sizes: Twin Set, 8-pc. 66 x 86; Full Set, 10-pc. 76 x 86; Queen Set, 10-pc. Set 86 x 86; King Set 10-pc. 102 x90 • Polyester • Machine wash • Imported • Shop our site for more pretty bedding ideas 10-piece set includes: comforter, bedskirt, 2 standard shams (1 with twin, 2 king with king), 4 pc. sheet set (3-pc. with twin) and 2 decorative pillows Why Buy? You can't go wrong with this comforter set if beauty and comfort are the things you seek. Our quality of comfort doesn't waver throughout this collection and it brings beautiful colors to your living space.
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Product Title: Brylane Home Lavender Fields Multi Pieced Comforter Set
Manufacturer: Brylane Home
Additional Specifications
tableware type: sets
blanket type: comforters
Kitchen Bar Type: bar set
cutlery type: knife sets
Bed Frame Type: sets
Product Type: Sets


text:
Hilary Swank and Joel Schumacher will participate in HIFF's "A Conversation With..." series.Read More »
When season one of "House of Cards" premiered on Netflix February 1st of last year, it arrived with a major filmmaker attached -- David Fincher, who made his television directing debut with the first two episodes, and remains attached in the upcoming second season as an executive producer.Read More »
Michael Fassbender has had a good run of it these past few years. It's a hot streak (one which saw him the recipient of the "staggering honor" that was Playlist Man of the Year 2011) that looks set to continue with the Irish/German actor moving between critically adored arthouse films and broad-appe...Read More »
This weekend "The Wolverine," starring Hugh Jackman as the adamantium-clawed avenger (is he ever not playing Wolverine?), will be slashing its way onto screens nationwide. But as fans know, this wasn't the original vision that Jackman and Fox had in mind. No, that version was to be helmed by Darren ...Read More »
With Sony confirming last week that "The Girl Who Played With Fire" would not be hitting screens in 2013 (hardly a shock considering no casting or greenlight or any other movement had happened on "The Girl With The Dragon Tattoo" followup), speculation brewed as to whether or not...Read More »
Vampires are pretty much everywhere these days, with the "Twilight" franchise and TV's "The Vampire Diaries" gripping the imagination of teen audiences the world over. In part, it's because of the element of sexuality inherent in vampires, something that's been present ever since the archetype was b...Read More »
Hot off the heels of delivering one of 2011's biggest turkeys, the almost-direct-to-video Nicolas Cage/Nicole Kidman home invasion thriller "Trespass," Joel Schumacher has been removed from the Troika Pictures' thriller "The Hive" and replaced by "The Machinist"...Read More »
With a speaking voice that often (and unexpectedly) devolves into histrionic yelps and an assortment of goofy, ever-changing hair pieces, Nicolas Cage has become such a creative loose cannon you often want to check in on his latest effort in the off chance that he's delivered some creative crazy goo...Read More »


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B L T anyone!?!
Just happened to see a smidgen of red on the tomatoe bushes &sure enough I got 4 beautiful red Roma maters. Couldn't hardly wait for lunchtime to have that first BLT of the season. Well let me say this...the bread, mayo, bacon, lettuce were delicious, the tomatoes had absolutely no taste at all, I mean no taste! The bushes are loaded, so maybe as they mature, flavor will be coming or am I whistling Dixie?
Well, dang it! I hope your tomatoes get a flavor boost soon, Pat! I've had some of the locally grown tomatoes (Romas) from the fields around here, and they sometimes don't have much taste, either. Not sure why. BLTs have to be one of the best sammiches on earth!
My dad is playing farmer this year. Mom reports that he has a nice crop going of cucumbers, tomatoes (hopefully!), watermelon, cantaloupe....I'm sure I'm missing something. I asked Mom to please save some for her favorite (ok, only...LOL) daughter! :)
Gee Pat that's too bad. Nothing like expecting a mouth watering BLT and no taste on the "T".
DH has one tomato plant growing out there with some green ones on it, don't know what he has? He has a green pepper plant he already ate one and pronounced it good and a strawberry plant he's been eating the berries from:)
Bell peppers (thanks, Leslie!), that's another one Farmer Dad is growing! LOL Mom says they've already had one or 2, and they're delicious. My mouth is watering (thanks, Westelle! :D)! I'm thinking of slices of moist, springy mozzarella with slabs of tomato...drizzled with olive oil and sprinkled with basil and/or oregano. *sob* LOL
Hey Mikey, I've tried fried green tomatoes and I don't think I'm doing something right cause they just didn't impress me to much. How about sharing your preparation of them with us, please, please, please. It's got to be me, not knowing what I'm doing! Of course I'm still hoping that the tomatoes I have will ripen up with a good flavor!
Oh, man. I'd never heard of fried green tomatoes until the movie came out. My mom made up a batch back then, and it was delicious! I haven't had any in years, though! From what I remember, she just used the same recipe she'd use for fried zucchini - I think she dipped them in egg, then dredged in flour with some salt and pepper, maybe some ground up crackers. Cripes, I'm going to have to call and get that recipe now. LOL
Thanks for making me drool, Mike! :D
Balsamic vinegar! I KNEW I was forgetting something, Westelle! LOL
Brenda, be sure to call your Mom for that recipe!
Westelle, Balsamic is the greatest. I had some in Portugual that had been aged, the lady served about a tablespoon of it over a scoop of vanilla ice cream. That is when I found out that buying aged Balsalmic is as intrigate as buying fine wine. My niece cooks her "B" down till it is a thick sauce, it's o.k. but it turns out to be just that, boiled down vinegar!
Pat, I asked Mom today, and...bad memories run in the family. LOL She figures she must have dipped the slices in flour first, then into an egg and milk mixture, then into either some flour and salt & pepper, cracker crumbs, or a mixture of both. She's sure she fried them in veggie oil or equivalent...but can you imagine using bacon grease? Oh, MY! I'm having chest pains just thinking about it, but I'd love to try them like that once. LOL
Here's the recipe I use for Fried Green Tomatoes.
Fried Green Tomatoes Parmesan
3 medium green tomatoes, sliced
1/4 cup yellow cornmeal
1/4 cup grated Parmesan cheese
2 Tablespoons all-purpose flour
3/4 teaspoon garlic salt
1/2 teaspoon dried oregano
1/8 teaspoon black pepper
1 egg, beaten
1/4 cup vegetable oil
1.(This is an important step--do not skip)
Lightly sprinkle both sides of green tomato slices with salt (not the garlic salt); drain on paper towels for 30-60 minutes or I use a wire rack for them to drain from. You may have to change out the paper towels if they get too saturated. Blot all excess liquid from the tomato slices with paper towels.
2. Meanwhile, combine cornmeal, grated Parmesan cheese, flour, garlic salt, oregano, black pepper in a shallow dish.
3. Dip each tomato slice into the beaten egg, then into the cornmeal mixture.
4. In a medium skillet, heat oil over med-high heat.
5. Fry tomatoes, a few at a time, for 2 minutes per side or until golden brown.
6. Drain on a paper towel-lined wire rack.
7. Serve immediately with or without dipping sauce such as Ranch dressing.


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Peak intensity prediction in MALDI-TOF mass spectrometry: A machine learning study to support quantitative proteomics
1 Applied Neuroinformatics Group, Bielefeld University, Germany
2 Friedrich-Schiller-University, Jena, Germany
3 Simulation of biological systems, Center for Bioinformatics Tübingen, Eberhard Karls University, Tübingen, Germany
4 Intl. NRW Graduate School for Bioinformatics and Genome Research, Bielefeld University, Germany
BMC Bioinformatics 2008, 9:443 doi:10.1186/1471-2105-9-443Published: 20 October 2008
Mass spectrometry is a key technique in proteomics and can be used to analyze complex samples quickly. One key problem with the mass spectrometric analysis of peptides and proteins, however, is the fact that absolute quantification is severely hampered by the unclear relationship between the observed peak intensity and the peptide concentration in the sample. While there are numerous approaches to circumvent this problem experimentally (e.g. labeling techniques), reliable prediction of the peak intensities from peptide sequences could provide a peptide-specific correction factor. Thus, it would be a valuable tool towards label-free absolute quantification.
In this work we present machine learning techniques for peak intensity prediction for MALDI mass spectra. Features encoding the peptides' physico-chemical properties as well as string-based features were extracted. A feature subset was obtained from multiple forward feature selections on the extracted features. Based on these features, two advanced machine learning methods (support vector regression and local linear maps) are shown to yield good results for this problem (Pearson correlation of 0.68 in a ten-fold cross validation).
The techniques presented here are a useful first step going beyond the binary prediction of proteotypic peptides towards a more quantitative prediction of peak intensities. These predictions in turn will turn out to be beneficial for mass spectrometry-based quantitative proteomics.


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Yellowstone National Park, WY
... and then left for a hike at Mt. Washburn. As a wildlife preservationist, Ben knows a lot about the animals in the area, especially birds (which he studied in college and grad school). Both he and Chris had brought binoculars and a high-power scope which proved very useful on our hike. But before we even got to the hike, we got caught in a huge bison jam. There must have been 100 bison in the fields and on the road in the Hayden Valley. Several passed in front ...
Deciding on the Best Route to Charleston
Since we were flying with a 3-year-old and 8-month old, we decided it might be easiest on them and us to split the flights into two days. The first would be the longest, Salt Lake City to Atlanta, an overnight near the Atlanta airport, followed by an early morning quick flight ...
Wild Blue Yonder!
... it was a great idea, then I noticed a decaying squirrel in the bottom of the tub and made a note not to mention it to Chris. Duke and I made our way to the smaller stream at the back of the house and I found a prime spot to take some hummingbird photos while he dined on more grass and dipped his paws in the water. It was still amazing to me to see so many hummingbirds surrounding the feeder! They're so zippy and reflective! When we got back inside the cabin, Chris and Steve ...
Getting Stuck, Hitching into the Canyon, Hiking
... always make sure to have some kind of rain jacket and some extra clothes to deal with the rain and drop in temperature that sometimes accompanies a storm.
The forecast for the week showed a storm moving into the Salt Lake City for late Thursday and Friday. It was Tuesday in Heber. I had planned on this day to cycle up to Park City, stay there overnight and then ride back through Big Cottonwood Canyon to SLC on Thursday. Not wanting to take the chance of riding in the canyon during ...
... there so we called in then ate in Park City – Kevin had Buffalo burger!!! On the way home, Mark took a detour and drove us to a mountain top in the dark to look over the valley where the twinkling lights of humanity could be viewed beneath us, just like in the movies.
A real treat the next morning when we awoke to music and knowing Mark is a Neil Young fan I thought he was playing a CD. When I went to see, it was Mark – guitar, harmonica ...


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I'm not signed yet, so I'm still budgeting
from Drake – The Presentation Lyrics on Genius
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GET YOUR GEAR ON: The Bison Airlighter
We've all used those cheapo fire-starting wands that inevitably conk out after just a handful of lights and never seem to work when we really need them.
Either that or — and this is even worse — we've burned our fingertips on lighters or matches that burn down too quickly.
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Thanks for checking out Eastview Sports. All of our leagues and programs are here for YOU! Everything we do is open to anyone in the community. Whether it's coming out to join a league, playing in some pick-up games, or participating in an exercise class, we're sure you'll meet some friendly faces and have a good time. So don't just sit there - DO something!
WEATHER UPDATE 2/4/14 - Due to inclement weather, all Eastview activities have been cancelled for the evening. This includes Upward basketball practices and adult open gym.


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I am trying to decide where to stay when in Rome. Any suggestions on which neighborhood I should focus on?
Neighborhoods in Rome, Italy
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What do you want to visit?
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we are staying for 10 days so all the hot spots.
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would like to stay some place near the majority of the sites
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OK, I say this all the time: Campo Marzio is my favorite. Why? Good food, great shops, near the sites, plenty of transport options. Atmosphere too.
On a budget, I'll take Trastevere, but not too far from river or transportation on the Viale.
I don't like the Campo de Fiori area that much because I don't love crossing and using the Corso Vittorio Emmanuele so often, and the crowds can be overwhelming.
Crowds nearer the Pantheon and Piazza Navona can be oppressive.
These are all my opinions from many stays in Rome. Others will think differently.
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hi, wanttohavefun,
i looked at your profile to see if you were new to fodors but find that if I may say so you've been here long enough to know your way about.
the destination button for Rome above should give you a start on what you might want to see, but I have to ask, if you are so clueless about what you want to see in Rome, why are you going?
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we do have a list of things that we want to see and do but my main concern is to find a place to stay that is not far from a bus stop of the metro. I have heard so many things about the different neighborhoods I just want to make sure I am not spending all my time traveling insteading of seeing
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I have found this new site called AIRBNB and it seems like something cool to do and rent a cottage instead of staying in a hotel. Where do you stay when in Campo Marzio
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We like staying near the Pantheon - or perhaps the Spanish Steps.
Crowds don't bother us - since they're certainly no worse than home. And we like being able to walk to so many places.
Won;t comment on Air BnB - but you can't rent a cottage in the center of Rome - it's all apartment houses. Any "cottage" would be in the distant countryside.
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I meant an apartment. Does anyone have any place they are willing to suggest?
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To be more AND less exact, I'm most willing to stay any place from Piazza del Popolo, down to about via Condotti, and from there west to the sort of triangle bordered to the east by Corso, the west by the Tevere and to the south from about Piazza Colonna to via Sant Agostino.
That's insane, I know, but after many trips to Rome, this is the area I'm most drawn to.
Google map Campo Marzio and the area to the north and/west. That's more general but you can probably trace my area.
I really like the Hotel Portoghesi, and have stayed at the due Torri. We have rented twice in the area between Piazza del Popolo and Piazza Spagna. I once stayed at Hotel Condotti, which was expensive and very poorly run, but that was a long time ago.
Other stays in other places, but the area I've tried to detail above is my favorite.
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Oh, what's your budget? How many people?
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Me and young son. So we need two beds and would like to pay under $100 a night since it will be for 9 nights
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That's only 75€ a night which is very low for the center of Rome. I suggest you try a few convents. Even then, doubles run about 80€ at many. You might try Fraterna Domus. They might be in the price range and are very central (with AC), but tend to book up fast. Here's some pics.
Their e-mail is firstname.lastname@example.com
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- 7 Hoping to stay cool this summer - any comments on my northern itinerary?
- 8 A taste of Scotland and Ireland
- 9 Mont St. Michele?
- 10 Siciliy - travel from Taormina to Siracusa via public transportation
- 11 What is the perfect day in Bruges?
- 12 Norway and Denmark Itinerary Critique Please
- 13 Best town for 3 nights on the Costa Brava?
- 14 Our first trip to Europe
- 15 18 days driving trip Rome>Spain>Rome
- 16 Best driving map for Greece?
- 17 Train from Monterosso to Padua
- 18 Help re: Driving from Venice Airport to Kobarid, Slovenia
- 19 Welltravbrit's London Sojourn - An Ongoing Trip Report
- 20 Gift for my European Friends- How about Hershey?
- 21 Is there immigration/customs check between Edinburgh and London?
- 22 Genealogy travel in Lithuania?
- 23 Paris Perfect Soap
- 25 Train tickets within Italy


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Frost & Sullivan
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Tel: (877) 463-7678
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Marketing Automation to Hit $1.9 Billion by 2020
Marketing automation software is on track to become a multi-billion dollar business within six years, a new study says.
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Home > Press > Harris & Harris Group Shareholder Report on Website
Harris & Harris Group Shareholder Report on WebsiteNew York, NY | Posted on August 9th, 2007
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Harris & Harris Group Reports Financial Statements as of December 31, 2014 and Posts Annual Letter to Shareholders on Website March 17th, 2015
Arrowhead to Present at 2015 Barclays Global Healthcare Conference March 4th, 2015
Arrowhead to Present at 2015 RBC Capital Markets' Global Healthcare Conference February 17th, 2015
Iran 1st among Islamic Nations in Scientific Production, Nanotechnology February 16th, 2015
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Novel nanoparticle therapy promotes wound healing March 27th, 2015
Designer's toolkit for dynamic DNA nanomachines: Arm-waving nanorobot signals new flexibility in DNA origami March 27th, 2015
Using magnetic fields to understand high-temperature superconductivity: Los Alamos explores experimental path to potential 'next theory of superconductivity' March 27th, 2015


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In Scala, I'm trying to produce a generic set of checks to run on some data.
My base trait looks something like this:
trait Check[T]
def complete() : Boolean = ...
def passed() : Boolean = ...
def update[T]( data : T ) : Unit
Then I've got two sub-traits which look a bit like this:
trait CheckFoo extends Check[Foo]{ val baz = 1 }
trait CheckBar extends Check[Bar]{ val baz = 2 }
which are designed to avoid me defining baz in each Foo and Bar check.
Then I've got some actual Foo checks, e.g.
class CheckFooOne extends CheckFoo
def update( data : Foo ) : Unit = ...
But this doesn't compile: it tells me that CheckFooOne must be abstract, as method update is not defined.
What have I done wrong? I'm sure there's some subtlety I've missed. I'm sorry if there's another question like this already, but I can't think of what to search for, and I've checked the list of similar questions without joy.


text:
A low-temperature foam compositions and that are produced from an epoxy compound and an acid source can be substantially free of polyurethane or isocyanate chemistry. The disclosed compositions and precursors thereof reduce, if not eliminate, the presence of conventional undesirable compounds and by-products thereof.
1. A method for producing a foam comprising:
(a) combining at least one epoxy component with at least one acid source component and at least one encapsulated blowing agent under conditions sufficient to provide an exothermic reaction; and
(b) utilizing heat from the exothermic reaction so as to expand the combined components to form a foam.
2. The method according to
3. The method according to
4. The method according to
5. The method according to
6. The method according to
7. The method according to
8. The method according to
9. The method according to
10. The method according to
11. The method according to
12. A foam composite comprising a foam according to
13. The foam composite of
14. A foam precursor comprising:
(a) an A-side foam precursor composition comprising an epoxy compound, and an encapsulated blowing agent, and;
(b) a B-side foam precursor composition comprising an acid source.
15. The foam precursor according to
16. The foam precursor according to
17. The foam precursor of
18. The foam precursor of
19. The foam precursor of
20. The foam precursor of
[0001] This is a continuation-in-part of U.S. patent application Ser. No. 09/197,124, filed on Nov. 20, 1998, that is a continuation-in-part of Ser. No. 09/081,967, filed on May 20, 1998 and entitled �Novel Foaming Compositions and Methods For Making and Using the Composition�. The disclosure of these prior filed patent applications is hereby incorporated by reference.
[0002] The subject matter herein claims benefit under 35 U.S.C. 111(a), 35 U.S.C. 119(e) and 35 U.S.C. 120 of U.S. Provisional Patent Application Serial No. 60/047,273, filed on May 21, 1997, entitled �A Room Temperature Foaming Composition�; and U.S. Provisional Patent Application Serial No. 60/079,205, filed on Mar. 24, 1998, entitled �Novel Foaming Compositions and Methods For Making and Using the Compositions�. The disclosure of the aforementioned Provisional Patent Applications is hereby incorporated by reference.
[0003] The subject matter of the instant invention is also related to Non-Provisional Patent Application Serial Nos. 09/081,966, filed on May 20, 1998 and Serial No. 09/197,107, filed Nov. 20, 1999, both filed in the name of Jeffrey Pachl et al., and entitled �Curable Sealant Composition�. The disclosure of these Non-provisional patent applications is hereby incorporated by reference.
[0004] The invention relates to foam compositions, precursors thereof and methods for making foam compositions and foam containing articles.
[0005] Foams are employed in a wide range of commercial applications including applications requiring thermal and sound insulation such as automotive and construction environments, among others. In the automotive industry, foams are typically formed in situ, and can be used to fill cavities such as pillars and rocker panels, and to dampen sound transmission. In situ foam formation has typically been accomplished by using a polyurethane foam based on isocyanate chemistry. Certain polyurethane foam components and by-products thereof are believed to have an undesirable environmental impact. Consequently, there is a need in this art for a low-temperature foam which is cost-effective and substantially free of undesirable materials.
[0006] The invention is capable of solving problems associated with conventional foam formulations by providing foam compositions and precursors thereto which do not require the use of isocyanates. The inventive compositions and precursors can thereof reduce, if not eliminate, the presence of conventional undesirable compounds and by-products thereof while providing benefits associated with conventional foams, e.g, sound/vibration dampening, thermal insulation, structure reinforcement, floatation, energy dissipation, among other benefits. In addition, the inventive foam has a reduced cured and tack time in comparison to conventional polyurethane foams. These properties in turn improve the efficiency of manufacturing processes that employ foam.
[0007] One aspect of the invention relates to a method of reacting an epoxy compound and a hydrogen donor or acid compound at ambient conditions to produce a foam. This reaction can produce a relatively large exotherm. The heat released by the exothermic reaction can be sufficient to drive an endothermic blowing agent, thus creating a foam virtually instantaneously. In fact, the exothermic reaction can be sufficiently large to cause a blowing agent entrapped within, for example, thermoplastic powders to expand thereby forming a foam.
[0008] Another aspect of the invention relates to a method of containing the foam during expansion by expanding the foam within a containment or control means. The control means confines the expanding foam and determines the direction of expansion. While any suitable control means can be employed, a polymeric bag or sack is desirable. If desired, the polymer bag comprises an adhesive material, e.g., the bag adhesive is activated by the exothermic foam reaction and affixes the resultant foam to a substrate. The polymeric bag can be fabricated from a virtually unlimited array of materials and configured into any desirable shape, e.g., a honeycomb structure, replicating an automotive cavity, etc.
[0009] The inventive foam can be employed in a wide array of end-uses. Examples of such uses include thermal insulation such as appliances, e.g., refrigerators, hot water heaters, etc; aircraft; commercial or residential construction such as spray or rigid insulation for walls, doors, cavity/widow sealant, acoustical control, etc.; packing material, e.g., foam-in-place; marine foams; environmental control, e.g., spill containment; footware; furniture; toy and consumer goods; protective equipment such as pads, helmets, etc.; fluid filtration; transportation industry uses, e.g., sound dampeners, structural supporting material, etc. for cars, trucks and heavy duty vehicles; vehicle repair; gasketing material; medical uses such as casts, emergency immobilization, etc.; artistic medium such as decorative brick/block, figures, etc.; among others.
[0010]FIG. 1 is a graphical representation of the foam reaction rate and temperature as a function of percent acid.
[0011]FIGS. 2A and 2B are a schematic drawings of assemblies that can be employed for dispensing the inventive foam within a defined cavity or area.
[0012] The invention is based, at least in part, on the surprising discovery that superior foam compositions can be produced from epoxy compounds and acids or hydrogen donor compounds, and in particular, a reaction of the epoxy compounds with the acid source.
[0013] Moreover, the inventive compositions can be polyurethane and/or isocyanate free. By �free� it is meant that the inventive compositions before or after foaming contain less than about 10 wt. % polyurethane and/or isocyanurates, isocyanate, and in most cases 0 wt. %. While the presence of such compounds does not adversely affect the reaction described below in greater detail, these materials can be obviated by employing the inventive formulations. The instant invention, therefore, provides a foam which can be used with or instead of urethane/isocyanate based foams and foaming systems.
[0014] The inventive foam composition is typically obtained from the reaction of one or more foam precursors. The precursor(s) comprise (i) at least one epoxy compound, and (ii) at least one acid source, i.e., a hydrogen donor or an acid, e.g., phosphoric acid, or a compound such as a photoinitiator which can upon activation provide a hydrogen donor or an acid, and (iii) at least one expansion or blowing agent, among other components. An exothermic reaction between the epoxy and hydrogen donor or acid can activate the expansion or blowing agent thereby producing a foam.
[0015] The foam precursor(s) can comprise a single phase system that is activated in response to a source of energy, e.g., heat, UV or electron beam or laser radiation, among other energy sources, or a two component system (an A side precursor and a B side precursor) that are contacted together to produce a foam. When a two component system is employed the epoxy and acid source are provided in separate �side� components.
[0016] Alternatively, the foam precursor(s) can comprise a two component system that is activated in response to a source of, e.g., heat, UV or electron beam or laser radiation, among other energy sources. The two component system can include an acid source as well as a photoinitiator.
[0017] The first component of the precursor(s), an epoxy compound, comprises about 10 to about 80 wt % of the precursor(s). Examples of suitable epoxy compounds include bis-phenol A epoxy, bis-F epoxy, epoxy-modified elastomers, epoxy-modified polybutene, epoxy-modified polybutadiene, epoxy-modified ethylene-propylene-diene rubber (EPDM), cycloaliphatic epoxy, novolack compounds, and mixtures thereof, among others. When a two component system is employed, the epoxy is located on the A-side, or otherwise prevented from prematurely reacting with the acid or other precursors.
[0018] The first component of the precursor can be tailored by adding one or more modifiers. For best results, the modifier is solublized by the epoxy or miscible with the epoxy. Examples of suitable modifiers can comprise at least one member selected from the group consisting of styrene and co-polymers thereof, vinyls and co-polymers thereof, elastomers such as nitrile, ethylene acrylic rubber, mixtures thereof, among others compounds that do not adversely impact the exothermic reaction. Some commercially available materials that can be employed as a modifier comprise Kraton� (Shell Chemical), Vamac� (DuPont), Piccolastic� (Hercules), Phenoxy� (Paphen), SAA� (styrene-allyl-alcohol copolymer (ARCO), G-Cryl� (Henkel), Rohagum� (Rhomtech), acrylate modified acidic adhesion promoting agent (acid functional oligomer, RadCure�), mixtures thereof, among others. Normally, the epoxy modifier comprises about 2 to about 50 wt. % of the composition prior to foaming.
[0019] A second component of the precursor(s) is the acid source. When a two component precursor system is employed, the acid source is present in the �B side� of the foam precursors. The hydrogen donor or acid usually comprises about 1% to about 30 wt. % of the precursor, and in particular, about 3% to about 15% of precursor B-side precursors. Examples of suitable acid sources include Lewis acids such as sulfonic acids, phosphoric acid, citric acid, carboxylic acid, glycolic, tannic, 1,2,4,5-Benzenenetracarboxylic acid, citraconic acid, L-(+)-Citrulline, fumaric, maleic, azelaic, oxalic acids, and mixtures thereof, among others. Particularly desirable results have been achieved by employing at least one of sulfonic, phosphoric acids and other acid functional compounds, e.g., acid functional acrylics. Depending upon the desired reaction rate and resultant foam characteristics, a relatively concentrated acid can be employed. An example of such a concentrated acid comprises a phosphoric acid that is substantially free of water. By �substantially free� it is meant that the acid contains less than about 10 wt. % and normally less than about 5 wt. % water. Substantially water free acid can be obtained by distilling commercially available acids, e.g., 75% phosphoric acid can be concentrated by distillation. If desired, the acid can comprise an acid functionally equivalent to the hydrogen donor released by a UV photoinitiator, e.g., replace a portion of the photoinitiator with its corresponding acid.
[0020] In one aspect of the invention, an acid substantially free of water is employed to obtain a foam precursor that generates foam having improved structural properties, e.g., foam having a flexural strength 50 to 100% greater than many conventional materials such as wooden particle board. By employing a substantially water free acid as a foam precursor, the resultant foam has a lower expansion and water absorption, and greater structural strength and adhesion, e.g., to a painted or primed metal surface, wood, Formica�, Masonite�, thermoplastics such as polystyrene, among other surfaces. Substantially water free acids can also permit using a wider range of precursors, e.g., non-polyol carriers.
[0021] In another aspect of the invention, the hydrogen donor comprises a photo-initiator that becomes active when exposed to a source of energy. While any photoinitiator capable of becoming a hydrogen donor upon activation can be employed, specific examples of a suitable photo-initiators include a UV catalyst such as UVI 6974 (Union Carbide) that is described in greater detail in the aforementioned copending and commonly assigned U.S. Non-Provisional Patent Application Serial Nos. 09/081,966, filed on May 20, 1998 and Serial No. 09/197,107, filed Nov. 20, 1999, both filed in the name of Jeffrey Pachl et al., and entitled �Curable Sealant Composition�. When such an initiator is employed, the foam precursors can be utilized in a single phase system.
[0022] For example, such a single phase system can be dispensed, exposed to a UV light source or other suitable source of energy that causes the UV catalyst to generate an acid thereby permitting the epoxy reaction to occur. The heat released by the exothermic epoxy reaction in turn activates an expansion or blowing agent, e.g., a hydrocarbon encapsulated within a thermoplastic, thereby producing a foam. While any suitable single or two phase system can be employed, normally a single phase system produces a foam that is thin relative to a two phase system. Similar to other foam precursors, the radiation activated precursors can be modified for controlling the properties of the precursors or resultant foam, e.g., about 3 to about 20 wt. % polystyrene is added to the epoxy component.
[0023] The blowing agent can comprise one or more of the blowing agents recognized in the foam-forming field. Example of suitable blowing agents include water, hydrazide, diphenyloxide-4,4-disulphohydrazide, carbonamide, azocarbonamide, hexamethylene diamine carbamate, sodium bicarbonate, dimethyl ether, methyl chloride, carbon dioxide, fluorocarbons such as difluoroethane, tetrafluoroethane, HFC-4310, azeotropes and isomers thereof, among others; and hydrocarbons such as butane, propane, pentane, isopentane, alcohol, isomers thereof; mixtures thereof, among other known blowing agents. Normally, the expansion or blowing agent comprises about 5 to about 40 wt. % of the foam precursor(s). The blowing agent can be present in either the A or B side of a two component system, although the B-side precursor is preferred.
[0024] The foam precursor(s) can also include at least one carrier component, e.g., a polyol, and optional components such as thermoplastics. A carrier usually comprises about 20 to about 40 wt. % of the precursor, e.g., preferably about 30 wt. %. The carrier typically serves to deliver a component, e.g., an acid, expanding agent, catalyst, mixtures thereof, among others for contact with the epoxy. Examples of suitable carriers comprise at least one member selected from the group of polyols including polyester polyols, polyether, polycarbonate and caprolactone; alcohol, polyvinyl alcohol, synthetic or natural oils such as castor, soy, linseed, glycerin and glycols; water, among other carriers that are preferrably miscible with the epoxy and mixtures thereof. When a two component precursor system is employed, these carrier materials are typically added to the acid side or �B side� component of the foam precursors In addition to the aforementioned epoxy modifiers, the components of the precursor can be tailored by adding one or more modifiers in order to control viscosity, improve stability, physical properties, reaction rates, color, odor, among other characteristics. For best results, the modifier is solublized by the carrier or miscible with a carrier. Examples of suitable modifiers can comprise at least one member selected from the group consisting of natural and synthetic oil such as castor, soy, canola, linseed, polybutene, among other oils. For example, by adding castor oil to the carrier, e.g, Part B-polyester polyol, a relatively hard foam can be obtained. Normally, the carrier modifier is used about 2 wt. % to about 50 wt. % of the composition prior to foaming.
[0025] Moreover, the density, moisture and temperature resistance among other physical properties of the final foam product can be modified or tailored by adding a thermoplastic, theromset, plastic or resinous material to the epoxy-containing precursor. While any suitable modifying material can be employed, examples of such modifying materials include dicyandiamide (Dicy (Amicure CG 1400)), ethylene vinyl acetate, polypropylene, polyethylene, rubber, phenoxy resin, phenolics, powdered wax, solid epoxy such as bis-A epoxy or modified epoxy, novalack compounds, mixtures thereof, among others. For example, depending upon the relative concentration of the components of the precursor, polyvinyl alcohol, hydroscopic polyolefin such as modified polypropylene (as well as other suitable materials) can be employed as modifiers and for absorbing steam or water generated by or during the exothermic reaction. About 1 to about 60 wt. % of modifying material can be added relative to the epoxy, e.g., about 2 wt. % of the precursor(s). The modifying material will normally comprise a powder having a particle size less than about 20 microns and a melting point from about 200 to about 400 F. The modifying material will become fluid and normally melt when exposed to the exothermic reaction temperature. When a two component precursor system is employed, these materials are normally, but not necessarily, combined with the epoxy or �A side�.
[0026] The foam precursors can also include a thermoplastic component that can function to modify the properties of the resultant foam, reduce material cost, increase precursor shelf life, among other desirable results. The thermoplastic component of the foam precursor(s) can comprise at least one member selected from the group consisting of acrylonitrile, polyethylene, phenolic, wax, EVA, polypropylene, GMA, acid modified polyethylene, polybutadiene, modified polyethylene blend (such as Bynel� supplied by DuPont Company), SIS or SBS or SEBS blocked copolymers (such Kraton� supplied by Shell Chemical), oligomers, polyolefin, hydroxyl or epoxy functional compounds, among other thermoplastic materials that can be dispersed in a foam precursor and have a melting point less than about the aforementioned exothermic reaction and mixtures thereof. Normally, the thermoplastic component of the precursor will comprise about 1% to about 60 wt. % of the precursor. The thermoplastic component can possess any desirable configuration or particle size. In some cases, the thermoplastic component can form a film or skin upon an exterior surface of the foam thereby improving the resistance of the foam to fluids, e.g., water, gasoline, among other fluids.
[0027] In one particularly useful aspect of the invention, a liquid or gaseous blowing agent is combined with or encapsulated within a thermoplastic particle or powder, e.g., a hydrocarbon encapsulated within an acrylonitrile shell as in Expancel� that is supplied by Expancel Inc., a division of Akzo Nobel Industries. When a two component precursor system is employed, the shells are normally combined on the B side along with the carrier. These shells can, however, be combined with the A side or in a single phase system so long as the composition of the shells is not substantially affected by the epoxy, e.g, the acrylonitrile or vinylidene chloride shells may be soluble within the epoxy. For example, the shells can be fabricated from polyethylene, nylon, EVA, polypropylene, polyolefin, among other materials not soluble in the epoxy component, and mixtures thereof could be present in the epoxy component of a two phase precursor system. The shells are selected to expand, rupture or retain their physical configuration depending upon whether or not an open or closed cell foam is desired. Specific examples of suitable encapsulated blowing agents comprise at least one member selected from the group of hydrocarbons such as isobutane and isopentane and fluorocarbons such as 1-1dichloroethene that are encapsulated within a thermoplastic such as 2-methyl 2-propenioc acid methyl ester polymer with 2-propenenitrile and vinylidene chloride polymer and polyvinylidene fluoride. These materials are supplied commercially by Expancel, Inc., a division of Akzo Nobel as Expancels� 051WU, 051DU, 091DU80, 820WU, 820DU, 642WU, 551WU, 551WU80, 461DU or Micropearl� F30D supplied by Pierce and Stevens. These materials can be supplied in either dry or wet form. When the A and B sides are contacted (or in the case of a single phase system exposed to an energy source), the epoxy reacts with the hydrogen or acid thereby releasing heat and causing the expansion agent within the shells to foam. The foam can be characterized by a composite wherein the epoxy reaction product (including of the aforementioned modifying materials) forms a matrix that embeds the expanded shells. Depending upon the physical characteristics desired in the foam, the shells can be open or closed cells.
[0028] The foam characteristics can also be modified by adding one or more filler materials to the precursor(s). Conventionally used filler materials comprise at least one of talc, mica, magnesium silicate, oxidized polyethylene, sodium silicate, alcohols, petroleum jelly, aromatic acid methacrylate-mixed half esters, methacrylated polybutadiene, concrete mix (supplied commercially as Quickrete�), arylalkoxy silane, hollow ceramic spheres, inorganic microspheres, dispersants, conventional blowing/expansion agents, flame retardants such as phosphates, borates and halogenated compounds; plasticizers, diluents, pigments, colorants, metal or ceramic powders, antimicrobial agents such as fungicides, fumed silica, abrasive materials, magnetic materials, anti-static or conductive materials, mixtures thereof, among others. If desired calcium carbonate can be added to the foam precursor for increasing the hardness and density of the resultant foam. When included the filler comprises about 1 to about 60 wt. % of the foam precursors.
[0029] The inventive foam can be matrix that embeds or contacts other materials in order to obtain a composite structure. The compositing materials can comprise the aforementioned filler materials, previously formed preform or structures, e.g., honeycomb, fiberous mat, shaped particulates member, honeycomb structures, syntactic materials such as described in U.S. Pat. No. 4,568,603 hereby incorporated by reference; among others. The compositing material can be added to a foam precursor and/or introduced when foaming the precursors. In one aspect, the compositing material comprises stryene pellets, e.g., recycled packaging material, that is ground and added to the previously described carrier. These pellets function to reduce weight and cost of the resultant foam. In another aspect, the compositing material comprises a material for improving the compressive strength of the foam and/or spacers for limiting the degree to which the foam can be compressed, e.g., nylon, polyolefins, polyethylene, among other materials. The compressive strength improving materials can be of any suitable form such as cubes, beads, mixtures thereof, among other shapes.
[0030] In one aspect of the invention, one or more foam precursors interact to form an intermediate foam precursor. The intermediate foam precursor can correspond to a Part A and/or Part B. The intermediate foam precursor can be contacted with another precursor or another intermediate foam precursor in order to obtain a foam. A carrier such as a polyol, e.g., a polyester polyol, can interact with at least one member selected from the group of an acid source, e.g, phosphoric acid; a modifier, e.g., styrene; among other precursor components. An epoxy can interact with at least one member selected from the group of an acid source, e.g., phosphoric acid; a modifier, e.g., styrene; among other precursors that are miscible with the epoxy. If desired the aforementioned carrier containing intermediate product is contacted with the aforementioned epoxy containing intermediate product to obtain a foam. The intermediate precursor can be self-supporting. The combined intermediate products can produce a gel-like product that in turn is converted to a foam, e.g, the intermediate product can comprise a gel that can be shaped prior to onset of foam formation.
[0031] The precursor(s) and/or intermediate products thereof can be pre-blended and stored in separate containers prior to use. To this end, an A-side or first precursor mixture is typically obtained by combining the epoxy and modifying material, e.g, polyvinyl alcohol and polypropylene, and a B-side or second precursor mixture can be obtained by combining the carrier, e.g., a polyol, hydrogen donor/acid and thermoplastic, e.g., encapsulated blowing agent.
[0032] The precursor(s) can be produced using any suitable apparatus that imparts an amount of shear sufficient to obtain a substantially homogenous precursor. Examples of suitable apparatus comprise hand mixing, static tube mixtures, the structures described illustrated by FIGS. 2A and 2B (described below in greater detail), impingement spraying precursors, extrusion, e.g., a twin screw extruder, among other conventional apparatus. Normally, the samples are mixed for about 1 to about 40 seconds depending upon the composition and mixing environment, e.g., a 1:1 A:B composition can be mixed for about 1 to about 10 seconds in a static tube mixer.
[0033] The inventive method involves contacting the epoxy compound and acid or hydrogen donor under conditions effective to provide an exothermic reaction. The heat produced from the reaction can then cause the blowing agent(s) to expand in forming the desired foam. For example, where two precursors, A and B are employed, the two compositions can be combined- to obtain a foam by using conventional foam manufacturing equipment. For example, A-side and B-side can be contacted as two high pressure streams within a mixing chamber of an external mix-head. While heat can be added to the precursors, the reaction between �A� and �B� can occur under ambient conditions, e.g., to control viscosity, adjust reaction rate, etc. The ratio of A-side to B-side normally ranges from about 1:1 to about 10:1 or 1:10.
[0034] An example of a combined A and B side precursor composition is set forth in the following Table.
[0035] The pH of the A-side component (containing the epoxy compound(s)) is normally about 6 to at least about 8. The pH of the B side of the foam precursor comprising an acid and a carrier is normally about 0.5 to about 4, e.g., the pH of phosphoric acid when mixed with polyol. Normally, the pH prior to reaction with A-side precursors is about 1.6. The composition and concentration of the foam precursors can be modified to achieve a predetermined reaction rate e.g., by tailoring the concentration of the acid. The affects of the pH or acid concentration of the B side are better understood by reference to FIG. 1 which illustrates the affects upon the composition demonstrated in Example 9.
[0036] Referring now to FIG. 1, FIG. 1 is a graphical representation of % acid in the precursor versus foam reaction time and temperature. FIG. 1 illustrates that as the acid concentration increases the reaction temperature increases and the reaction time decreases. FIG. 1 also illustrates that the precursor can be selected to a predetermined reaction time/temperature. For example, by selecting a higher reaction temperature (higher acid concentration) a wider range of modifying materials can be employed whereas by selecting a slower reaction time (lower acid concentration) the foam has easier handling characteristics.
[0037] The viscosity of a foam precursor can be tailored to enhance the resultant foam characteristics. The viscosity of the �A-side� or epoxy component of the foam precursor is normally controlled, for example, so that a modifying material, e.g., a plastic powder, becomes or remains dispersed within the �A- side� precursor. While any suitable viscosity control agent can be employed desirable results can be achieved by using a solid polymer (in particulate form) to produce a foam precursor gel.
[0038] Examples of suitable solid polymers comprise at least one member selected from the group consisting of waxes, polyethylene, EVOH, PVOH, fluoropolymers and dispersions thereof such as polytetrafluoroethylene (supplied as Teflon� by the DuPont Company), among others. The viscosity control agent can range in particle size of about 20 to 50 microns, e.g,. less than 325 mesh. An example of a controlled viscosity composition comprises about 5 to about 10 wt. % solid epoxy, about 5 to about 15 wt. %, powdered polyethylene and about 25 to about 30 wt. % blowing agent. In addition to viscosity, the characteristics of the foam can be tailored by varying the temperature, pressure, foam pH, foam density, among other parameters known to those skilled in this art. Also, the �A-side� of the system can be thickened into a gel by the addition of a surfactant such as any commercially available liquid detergent or titanate such as Kenrich KRTTS, e.g., about 0.5 to about 3 wt. % surfactant. This enables a more complete rheological control, included insuring the homogeneity of the system.
[0039] As discussed above, the foam can be produced from a single-phase system, e.g., only an �A-side� mixture. An example of such a system comprises an epoxy, a polyol, thermoplastic spheres, modifying materials, phenoxy, polypropylene, mixtures thereof, among other components. This one component system can be heat activated. In other words the system expands by being exposed to elevated temperature, e.g., about 125 C. If desired the single phase foam system can be initiated by employing a photo-initiator instead of, or in conjunction with, an elevated temperature. Examples of such initiators comprise at least one member selected from the group consisting of Union Carbide UVI 6974 among others. Normally, the amount of such an initiator corresponds from 0.5 to about 5 wt % of the foam precursor. More details regarding photoinitiators can be found in �Photopolymerization Behavior of Several Cationic Photoiniators in Catatonically Cured Resin Systems� by Edward Jurczak; that is hereby incorporated by reference.
[0040] Single phase systems are especially useful when applied upon a substrate by being sprayed. For example, the single phase system can be sprayed upon an automotive subassembly for reducing the amount of sound transmission to the interior of the car. In a further example, the single phase system can be sprayed upon a first component, e.g., a plastic fascia, exposed to UV to cause foaming and affixed upon a second component, e.g, metal support member, wherein the foam functions to reduce vibrations between the components.
[0041] A composite foam structure can be obtained in accordance with the instant invention. A structural modifier such as fibers, particles, rods, tubes, powders, mixtures thereof, among others, can be incorporated as a component of the foam precursor. The structural modifier can be employed for tailoring the chemical and/or physical properties of the resultant foam. Examples of suitable structural modifiers, normally as chopped fibers, ceramic or glass spheres or powders, can comprise at least one of nylon, carbon, carbonates, polymers such as polyethylene and polypropylene, graphite, Kevlar�, Dyneon, ceramic, fiberglass, mineral fillers, e.g., mica, metals, among other materials. The amount of such structural modifiers normally comprises about 1 to about 60 wt. % of the uncured foam precursor.
[0042] Any suitable commercially available foam production equipment can be employed for mixing and dispensing the inventive foam precursors to obtain the inventive foam. Examples of such equipment comprises DoPag (ECONO-MIX) supplied by Kirkco Corporation, Monroe, N.C.; as well as equipment supplied commercially by Jesco Products Company, Inc, Sterling Heights, Mich. Another example comprises using an Econo-Mix pump in combination with an Albion static mix head. The foam precursors can also be mixed by employing a power mix gun such as supplied by Sealant and Equipment Company, Oak Park, Mich. If desired, the inventive foam can be expanded with in a cavity, e.g., an automotive A pillar, by employing a dispensing apparatus having a replaceable/disposable static mix head. That is, the static mix head can comprise a replaceable plastic tubing having a center piece with a helix or vortex configuration, that is connected to a pump discharge flange and inserted into the cavity for foaming the precursors.
[0043] Another static mix head design has a valve type of arrangement that is illustrated in FIGS. 2A and 2B. Referring now to FIG. 2A, FIG. 2A illustrates a one-way value type of arrangement wherein the foam or precursors thereof are introduced or injected via a one-way valve 1 (commonly known as a zerk) that is positioned within a cap 2. Valve 1 can also include a flap or secondary valve 1A that prevents foam from escaping by reverse flow through valve 1. The cap 2 seals or defines one end of a cavity being filled with foam. The cap 2 can include hooks or locking tabs 3 for securing the position of cap 2, e.g, within the so-called A pillar of an automobile thereby permitting foam to be dispensed within the automotive cavity in a controlled manner. Normally, one end of the valve 1 is connected to a mixing zone 4 such as the aforementioned static mixers having helical vanes 5. After traveling through the valve 1 and static mixer 4, the foam is released into the cavity to be filled with foam. The area and direction into which the foam expands can be control and/or defined by using a containment means such as a polymeric bag 6 (the containment means is described below in greater detail).
[0044] Referring now to FIG. 2B, this type of arrangement provides a longer mixing time for the foam precursors before the foam is released into the cavity to be filled. The arrangement illustrated in FIG. 2B can also be employed as a cap 10 to seal or define one end of the cavity to be sealed. After delivering the foam precursors, a mix head 11 or previously described valves (4 and 5 of FIG. 2A). The foam precursors travel through mix head 11 and are released at the opening defined at 12 as foam. The opening 12 can also be within the aforementioned containment means. The caps 1 and 10 can remain associated with the foam product within the cavity. By using such a replaceable mix head, any problems associated with clogged mix heads are avoided. Two pressure streams can also be employed, to converge in a mix chamber or cavity to be foamed and mix action occurs without use of additional mixing apparatus. In addition to the foregoing, the inventive foam composition and precursors thereof can be injected, extruded, shaped, sprayed, cast, molded, among other conventional processes in order to obtain a desirable foam article. The configuration of the foam article can be virtually any shape including continuous shapes such as films or webs, discrete forms, among other shapes.
[0045] While the above description emphasizes particular foam compositions, the inventive compositions (and precursors thereof) can include additives such as dyes, fillers, surfactants, pigments, nucleating agents, among other conventional employed foam additives. If desired a pH indicator can be added to the precursor in order to provide a visual detection means for a reaction product. An example of a suitable pH indicator comprises at least one member selected from the group consisting of methyl red, methyl blue, chlorophenol red, bromothymol blue. That is, as the foam precursor react, e.g, acid-epoxy, the acid is consumed thereby changing the pH and causing the pH indicator to change color.
[0046] If desired, the inventive composition can be laminated or joined with other articles, e.g., laminated onto metal foil, Mylar, fiberboard, veneer, Formica� etc. In one aspect of the invention, the inventive foam precursors can be applied between two such laminating materials in order to form components that are useful in fabricating furniture. For example, the inventive foam is expanded between two laminating materials, one of which comprises the upper surface (e.g., a wood veneer) and the second the lower surface of a table top. Any excess foam can be removed by conventional methods such as sawing, scraping, etc. The foam imparts structural integrity to the article while reducing weight and fabrication time.
[0047] The inventive composition can also be expanded within a control or containment device or bag having a predetermined shape thereby forming a foamed article that replicates the bag, e.g, refer to U.S. Pat. Nos. 4,269,890 (Breitling), 4,232,788 (Roth), 4,390,333 (Dubois); the disclosure of each of which is hereby incorporated by reference. When expanding the foam into a bag, the previously described valves illustrated in FIGS. 2A and B; those supplied commercially by Inflatable Packaging as part no. IP04, or any other suitable delivery means can be employed at the opening in the bag in order to control introduction of the foam into the bag.
[0048] For example, a bag replicating a cavity such as an automotive cavity or any other desirable configuration unrolls or expands into the cavity as foam is introduced into the bag via the valve. If desired, the bag may comprise or be coated with a heat sensitive adhesive wherein the heat generated by the exothermic foam reaction activates the adhesive. The adhesive can permanently affix the foam containing bag at any desirable location. The bag can also include predetermined areas having weakened seams or perforations that are designed to rupture as the foam expands thereby directing the expanding foam. Similarly, the bag composition can be selected such that the bag melts when exposed to the foam. The melting bag can direct the expanding foam, form a coating upon the foam, and function as an adhesive, among other utilities. Further, a plurality of bags can be employed wherein one bag is surrounded by another bag. The inner and/or outer bag can possess the aforementioned predetermined properties. Furthermore, the bag can comprise areas having distinct chemical and/or physical properties, e.g., a bag comprising one sheet of polyethylene heat sealed around its periphery to a sheet comprising polybutadiene. At least a portion of the bag can be fabricated from one or members selected from the group consisting of polyethylene, polyester, vinyl, nylon, Surlyn�, ethylene vinyl acetate, styrene-isoprene-styrene, styrene-butadiene-styrene or other blocked copolymers, polybutadiene, among other plastic materials with melt points corresponding to temperature range of reaction, polyamide, modified EVA's, modified polyethylene, modified polybutadiene, GMA, SBR, among other plastic materials suitable for bag or bladder construction and seaming capability. The bag or containment means can be utilized with a wide range of foam compositions in addition to the previously described epoxy containing foams. Examples of foams that can be expanded into the previously described containment bags or means comprise at least one of epoxy amine, acrylic, and phenolic among others.
[0049] The foam precursors can be removed from surfaces, equipment, among other articles by employing non-hazardous cleaning materials. An example of suitable cleaning material comprises water, isopropyl alcohol, 2-butoxyethanol and a chelating agent. The cleaning material can be dispensed as an aerosol by using a propellant such as DME, hydrocarbons and carbon dioxide.
[0050] Moreover, the inventive foam can be fabricated to possess a substantially uniform or varying density throughout one or more of its dimensions. The ability to tailor foam density in individual articles as well as throughout an article is a marked improvement in the art. Foams having varying densities can be employed for attenuating or focusing sound, various forms of electromagnetic radiation, radar, etc.
[0051] While the above description emphasizes a reaction between an epoxy containing compound and one or more acid or hydrogen donor, the inventive method can be employed by employing other polymer systems such as silicones, urethanes, silanes, hydroxyl modified elastomers, hydroxyl or epoxy functional compounds, among others. That is, a polymer system is contacted with an acid that generates an exothermic reaction which in turn activates an expansion or foaming agent.
[0052] The following Examples are provided to illustrate not limit the scope of the invention as defined in the appended claims. Unless indicated otherwise, commercially available apparatus and materials were employed in these Examples.
[0053] A foam product was produced by mixing a 2-part system (A-side precursor and B-side precursor) through a conventional foam production apparatus comprising a static mixer that was manufactured by Albion (Model No. 535-1 or equivalent). The constituents of the foam were maintained in two separate supplies of materials, an A-side precursor and B-side precursor.
[0054] The A-side precursor comprised a blend of the epoxy and the thermoplastic microspheres including a blowing agent, in ratio of 30 parts to 15 (100 parts total). The B-side precursor comprised a blend of the phosphoric acid and the polyol in a 30 part to 50 part ratio (also 100 parts). The feed ratio of A-side precursor to B-side precursor to the mixer head was 1:1. The pH of the B-side precursors was about 1.6 prior to reaction with A-side precursor.
[0055] A pressurized flow through the mixing chamber produced a polymer which rapidly expands and released an amount of exothermic heat sufficient to produce a foam.
[0056] The process of Example 1 was repeated with the exception that the ratio of epoxy to thermoplastic microspheres in A-side precursor was 2:1, and the ratio of phosphoric acid to polyol in B-side precursor was 3:5. The feed ratio of A-side precursor to B-side precursor to the mixer head was 3:1.
[0057] The process of Example 1 was repeated with the exception that the A-side precursor and B-side precursor components were mixed together by hand (instead of using the static mixer).
[0058] This example demonstrates the formation of a composite foam. The process of Example 1 was repeated with the exception that about 5 wt. % polytetrafluoroethylene powder (TEFLON� supplied by the DuPont Company) was added to the A-side precursor composition. The A-side precursor and B-side precursor were contacted in the manner described in Example 1. A composite foam was recovered wherein the composite foam had greater flexibility or pliability in comparison the foam obtained by the process of Example 1.
[0059] A two phase system was used to produce a foam. The A-side precursor was composed of epoxy and microspheres in a 2:1 ratio (67% epoxy, 33.3% microspheres) by weight. (It is noted that for best results, the mix should be used within in 4-8 hours of mixing since epoxy can dissolve certain spheres). The A-side precursor was hand-stirred to a smooth consistency.
[0060] The B-side precursor was composed of Polyol (Tone 0301) and Phosphoric acid (10%) by weight). The acid was blended into the polyol. A-side precursor to B-side precursor ratio of 1:1 was contacted in a static tube mixer and produced a foam. The ratio of A to B can be from 1:1 to 4:1 depending on acid concentration.
[0061] A two phase system was used to produce a foam. The A-side precursor comprised an of epoxy (UCB-Radcure UVACURE 1500). The B-side precursor was comprised of a polyol (50 wt. %�Tone 0301), phosphoric acid diluted with water (approximately 50% acid in a commercially available solution) at 20%, and 30% microspheres. The spheres were hand-stirred into the polyol to a smooth consistency. The acid mixture was blended by hand-stirred into the sphere-polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was contacted in a static tube mixer and produced a foam. The ratio of A to B can be from 1:1 to 4:1 depending on acid concentration.
[0062] A two phase system was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure1500) While the B-side precursor comprised polyol (Tone 0301), polyvinyl alcohol and water blend (PVOH: H20 3:1 blend that corresponded to 20% of the polyol) and microspheres 30% by weight of polyol and acid can be 10% of total �B� mixture. The spheres were hand-stirred into the polyol to a smooth consistency. The PVOH and water are hand-stirred. The PVOH/water solution temperature was 140� F. The PVOH blend was added to the polyol by hand stirring. The acid was hand-stirred into the sphere-PVOH-polyol mix. The A-side precursor to B-side precursor ratio of 1:1 was contacted in a static tube mixer and produced a foam. The ratio of A to B can be from 1:1 to 4:1 depending upon acid concentration.
[0063] A two phase system was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure 1500) and a phenoxy resin (Paphen PKHP-200 that corresponded to 25% of A-side precursors, epoxy is 75% of A-side precursors). The B-side precursor comprised 45% polyol (Tone 0301), 23.5% polyvinyl alcohol (Airvol 203S) and 23.5% microspheres. Phosphoric acid was 10% by wt. of the B-side precursor. Spheres are hand-stirred into the polyol to a smooth consistency. The PVOH, microspheres, and polyol are blended by hand stirring. The phosphoric acid was hand-stirred into the sphere-PVOH-polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was used contacted in a static tube mixer to produce a foam. The A to B ratio can range from 1:1 to 4:1 depending on acid concentration.
[0064] A two phase system, namely an A-side precursor and a B-side precursor, was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure 1500) 60 wt %, polypropylene powder (Equistar FP 800-00) 20 wt %, polyvinyl alcohol (Airvol 203S) 20 wt %. The B-side precursor comprised polyol (Tone 0301) 60 wt % and microspheres 30%. Phosphoric acid was 10%. Spheres are hand-stirred into the polyol until a smooth consistency was obtained. The microspheres and polyol are blended by hand stirring. The phosphoric acid was hand-stirred into the microspheres and polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was used and contacted in a static tube mixer to produce a foam. The A to B ratio can, however, range from 1:1 to 4:1 depending on acid concentration.
[0065] This Example employed a two phase system wherein the A-side precursor comprised a gel. A two phase system, namely an A-side precursor and B-side precursor, was used to produce a foam. The A-side precursor comprised an epoxy (UCB-Radcure UVACure 1500) 59 wt %, polypropylene powder (Equistar FP 800-00) 20 wt %, polyvinyl alcohol (Airvol 203S) 20 wt % and surfactant (gelling agent) at 1 wt %. The B-side precursor comprised polyol (Tone 301) 60 wt % and microspheres 30%. Phosphoric acid was 10%. Spheres are hand-stirred into the polyol until a smooth consistency was obtained. The microspheres and polyol are blended by hand stirring. The phosphoric acid was hand-stirred into the microspheres and polyol mix. An A-side precursor to B-side precursor ratio of 1:1 was used and contacted in a static tube mixer to produce a foam. The A to B ratio can, however, range from 1:1 to 4:1 depending on acid concentration.
[0066] A bag or containment device approximately 8�8 inches in size and having a one-way valve located on one end of the bag was constructed from two sheets of high density polyethylene film. The seams of the bag were designed to rupture at specific locations, which directs foam expansion into cavity area adjacent to weak seams. The sheets were joined by heating on a TEW Electric Heating Company Ltd sealing apparatus. The seams were selectively reinforced by double sealing or weakened to provide multiple points for foam direction from the same bag. The foam composition demonstrated by Example 9 was introduced into this bag. As the foam expanded, the foam escaped from the bag through the relatively weak seams.
[0067] A bag or bladder composed of each of polyethylene, ethylene vinyl acetate, polybutadiene were fabricated by using the apparatus described in Example 10. The foam of Example 9 was introduced into these bags. The bags, having a melting point less than the exothermic reaction temperature of the foam, failed and released the foam.
[0068] A bag or bladder composed of each of modified EVA (Bynel�), modified polyethylene (Primacor� supplied by Dow Chemical Company), modified butadiene, glycidal methacrylate (GMA) were fabricated by using the apparatus of Example 10. The foam of Example 9 was introduced into these bags. The heat released from the exothermic reaction of the foam caused the bags to melt. The melting bag material adhered to the foam thereby modifying the surface of the foam. The melting bag also adhered the foam to any surrounding surfaces or articles.
[0069] A bag or bladder composed of each of polypropylene, polyethylene, woven nylon mesh, aluminized fiberglass mesh was fabricated by using the apparatus of Example 10. Each of the bags was further processed to possess multiple perforations (25-100 holes/in.). The foam of Example 9 was introduced into each of these bags. The perforations allowed the foam to escape in controlled quantities while also generally retaining the shape of the bag.
[0070] Two bags or bladders, namely an inner and outer bag were fabricated by using the apparatus of Example 10. The inner bag comprised modified butadiene and the outer bag comprised high density polyethylene. The inner bag was placed within the outer bag and the outer bag was sealed. The foam of Example 9 was introduced into the inner bag. Inner bag or bladder melted during the foam reaction. The inner bag was of sufficient size to contain the required amount of mixed foam precursors to fill the out bag. Outer bag construction was of material and size to contain reaction within the cavity.
[0071] The insertion loss or sound dampening characteristics of the foam produced in accordance with Example 9A was tested in accordance with Society of Automotive Engineers (SAE) J 1400. The sample size was 3�3�10 inches and placed within an E-coated metal channel. An increase in insertion loss corresponds to an increase in sound dampening properties that in turn corresponds to less noise within the passenger compartment of an automobile.
[0072] These data illustrate the desirable sound absorbing characteristics of the inventive foam compositions.
[0073] The viscosity of the Part A foam precursor fabricated in accordance with Example 9A was tested in accordance with conventional methods and apparatus (Brookfield Viscometer, Spindle 27, Thermal-Cell). The viscosity as a function of temperature is listed below.
[0074] The viscosity of the Part B foam precursor fabricated in accordance with Example 9A was tested in accordance with conventional methods and apparatus (Brookfield Viscometer, Spindle 27, Thermal-Cell). The viscosity as a function of temperature is listed below.
[0075] This Example illustrates foam formation as a result of being activated by exposure to an energy source, e.g, UV light. A radiation curable foam having the following components was prepared:
[0076] The above components were combined as follows. The Uvacure and polyol were added together in a mixing vessel and mixed until the solution was clear. The UVI 6974 was added to the mixture, and mixed until substantially completely dispersed (about 2 minutes). The Expancels spheres were added to the mixture and mixed until substantially lump free. For best results, the minimum amount of mixing time, and shear were employed.
[0077] The foam precursors were placed onto a conveyor and exposed to a source of UV light. The method for exposing the precursors to UV light is described in the previously identified U.S. patent application Ser. No. 09/197,107, filed Nov. 20, 1999, both filed in the name of Jeffrey Pachl et al., and entitled �Curable Sealant Composition�.
[0078] This UV activated foam was modified by adding an acrylic monomer or acrylated oligomer. This modified UV activated foam was prepared as described above and comprised:
[0079] The resultant foam possessed a pressure sensitive adhesive characteristic. The tacky pressure sensitive characteristic was removed by adding an acrylate compound. A tack-free formulation comprised:
[0080] The following Table lists the Components, Trade Names and Suppliers for the foam precursors that were employed in Examples 18 through 22. The foam in Examples 18-22 was prepared by contacting the Part A with the Part B listed in the tables below in a 2.75″ diameter by 1.92″ height ointment can and mixed by hand. Reaction Time and Temperature were determined in accordance with conventional methods. The percent vertical expansion as well as the shrinkage was determined visually. The Shore A test was conducted using a Type A-2 Shore Durometer Hardness test unit that meets ASTM D2240 requirements. The Shore A test was conducted about 4 hours after foam formation. The instantaneous peak reading was recorded.
[0081] The following terms and definitions are referenced in Examples 18-22.
[0082] Tin Ointment Can: Dimensions 2.75″ d�1.92″ h
[0083] Initial Rxn Time: Time that initial expansion is observed (includes mix time, does not include time to pour part A into part B
[0084] Final Rxn Time: Time for reaction to go to completion (includes �Initial Rxn Time�) Rxn Temp: The peak temperature observed during the reaction
[0085] % Ht Expansion: % HE=[(hf-hi)/hi]�100
[0086] Density: Weight of 1 in3 block of expanded material (g/in3)
[0087] H2O Absorption 1: 100�(W3-W2)/(W2-Wc):Wc=weight of aluminum coupon only W2=weight of coupon+material before submerging in water W3=weight of coupon+material after submerging in water: Mix material, apply to a 3″�3″ aluminum coupon, allow to cool to room temperature, submerge in water for 24 hrs, wipe off excess and immediately calculate water absorption.
[0088] H2O Absorption 2: Take a 1.5 inner diameter�h Polyvinyl chloride (PVC) pipe: use Daubert #2-76GSM paper as the release liner inside the PVC pipe (use some means to cap the bottom so that material does not exude out): mix part A & B and pour into the pipe and allow to expand and cure: cool to room temperature: cut 1.5″ lengths so that the sample size is ≈1.5″ d�1.5″ h: sand the edges: submerge in water for 24 hrs: remove the sample, wipe off excess water and immediately calculate % water absorption. % Water Absorption=100�(WF-WI)/WI
[0089] H2O Absorption 3: �Open Chunk�: Mix part A & B in a polystyrene plastic cup: allow to expand and cure: cool to room temperature: Cut a �chunk� of foam from the top surface: submerge in water for 24 hrs: remove the sample, wipe off excess water and immediately calculate % water absorption: % Water Absorption=100�(WF-WI)/WI
[0090] Hardness: Shore A: The foam surface may be irregular: Take highest instantaneous reading from top surface after conditioning at room temperature for 4 hrs minimum
[0091] Shrinkage: Rating: 0=none 1=<1 mm from edge 2=1-2 mm from edge 3=2-3 mm from edge 4=3-4 mm from edge 5=4-5 mm from edge 6=5-6 mm from edge (shrinkage is usually not symmetrical: take the largest gap and divide by 2 if it did not shrink equally from the outer perimeter. Other values listed will be visually results: Rating 1=very slight, Rating 2=noticeable, Rating 3 & 4=significant, Rating 5 & 6=very significant
[0097] This Example illustrates the ability to tailor the inventive foam compositions and obtain foams having a wide range of characteristics. A foam of relatively low density was produced by in accordance with Example 18. The foam was obtained by combining the following foam precursors:
[0099] Each component (Part A & B) was individually mixed by hand using a hand driven paddle in a cup or ointment can. The two were brought together in a single vessel, again mixed by hand, and allowed to react. The foam produced was similar in appearance to other types listed above, but had a final specific gravity 0.16 g/ml.
[0100] The following Example demonstrates employing the inventive foam as a structural material between two laminates to fabricate furniture. The components listed in the following Table were combined in accordance with Examples 18-22.
[0101] The following Table lists components employed in the above Table for making foam.
[0102] Sample No. 1 above was combined and introduced into a mold comprising standard 1″�4″�12″ boards and laminating materials comprising wood-grain Formica� and fiber-reinforced paper board that were maintained a defined distance about by wood spacers, i.e., a distance of about � inch. The boards and laminating materials were placed into �C� clamps and a vise. The foam composition was prepared and poured between the laminating materials. Once the foam reaction was completed and the foam had cooled to room temperature, the assembly was visually inspected. The foam had adhered to the laminating materials and provided structural support.
[0103] A skilled person in this art would understand that these exemplary processes an be modified by manipulating process variables such as time and temperature of each aforementioned mixing step, mixing rate (RPM), time under vacuum, radiation source (e.g., UV light) and length of exposure and distance from source, and level of vacuum (mm Hg) as well as operating a continuous process. While the above Examples illustrate a batch process a skilled person in this art after having reviewed and understood the instant disclosure, would be capable of manipulating the aforementioned process variables to tailor the instant composition for a virtually unlimited array of product applications.
[0104] While the present invention has been described in certain preferred embodiments thereof, it will be apparent that various substitution, omissions, modifications, and other changes which may be made without departing from the spirit of the invention. Thus, the present invention should be limited only by the scope of the following claims including equivalents thereof.
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