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(This story first ran at PressConnects.com) BALTIMORE — At 26 years old, UFC light-heavyweight champion Jon Jones admits it is difficult even for him to realize he could soon be considered the best fighter in the history of mixed martial arts. But it's a reality (…)
The highly anticipated co-main event of "Bellator 154: Davis vs. King Mo" between Josh Thomson and Michael Chandler has been cancelled. read news >>
Following an erratic couple years, Titan FC veteran Kevin Croom believes he's back on track towards the UFC. read news >>
Thirty-two-year-old mixed martial artist Blas Avena was found deceased in his apartment. Police are investigating his passing as a possible suicide. read news >>
Former Bellator and WEC mixed martial artist Blas Avena was found dead at the age of 32 in his Las Vegas apartment just before noon PT on Wednesday, per TMZ Sports. The Las Vegas Metro Police Departm read news >>
Fight fans got an ugly sight on Sunday afternoon at UFC Fight Night 87 in the lightweight bout between Josh Emmett and Jon Tuck. In the latter half of their three-round fight, Emmett was clearly favo read news >>
In the midst of a career resurgence, Pride veteran Sergei Kharitonov is hunting a Bellator championship. read news >>
An injury has forced Julia Budd to withdraw from her inaugural Bellator women's featherweight championship bout against Marloes Coenen at Bellator 155. read news >>
The hits just keep on coming for Bellator 154, as veteran Pride heavyweight Sergei Kharitonov has been forced out of his promotional debut. read news >>
Back in January, after a scheduled matchup between Stipe Miocic and Fabricio Werdum was postponed due to a Werdum injury, the Brazilian UFC heavyweight champ threw a little shade in the direction of read news >>
Chris Weidman is out of his rematch with Luke Rockhold at UFC 199, but Michael Bisping quickly let it be known that he is prepared to step in and take his place. read news >>


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Watch more videos at http://FilmOn.com/TV/MMA-Now-Live Follow on Twitter at http://twitter.com/MMANowTV Like us on Facebook at http://facebook.com/MMANowTV watch video >>
Today we take a look back at the 1992 Cannes Film Festival. Jean Claude Van Damme along with Dolph Lundgren were there to promote their new film Universal Soldier. There were plenty of rumors at that watch video >>
GLORY 30 LA - Tiffany Van Soest Post-Fight Interview watch video >>
It is the new school vs the old guard when Dricus du Plessis faces Martin van Staden for the vacant welterweight title. watch video >>
Tiffany van Soest vs Esma Hasshass
GLORY 30 Super Fight Series watch video >>

subset: commoncrawl


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- Tuesday 12 August 2014
- Two Gunditjmara women, Christina Saunders and Sandra Aitken, are among 35 finalists in this year's Victorian Indigenous Art Awards....Friday 18 July 2014
- Art can challenge, inspire, question, and provoke, and in the case of Patricia Piccinini her creations can do all of those things at the same time....Friday 4 April 2014
- Deborah Sims and Matt Dickson have spent the past five years putting together an impressive collection of Indigenous art which is on show at the Warrnambool Art Gallery....Thursday 5 December 2013
- Gippsland-based artist Ray Thomas takes out the top prize in the 2013 Indigenous Art Awards with a portrait of his Mum; meet the other artists from across VIctoria recognised in the first Indigenous Art Awards event held in Ballarat....Monday 4 November 2013
Explore by Topic
Latest Sculpture stories on ABC South West Vic
Latest Sculpture stories on ABC Online
- Thursday 12 May 2016
- A Japanese artist arrested in 2014 has been found guilty of breaking the country's obscenity laws after she sent data which enabled people to 3D print a cast of her vagina. Megumi Igarashi produced a series of artworks modelled on her vagina, which were deemed obscene under the Japanese criminal ...Tuesday 10 May 2016
- Members of an Aboriginal community affected by the nuclear bomb tests at Maralinga in the 1950s are connecting with nuclear bomb survivors in Japan. A group of artists from Yalata in South Australia are flying to Nagasaki today to unveil a sculpture for its peace park - it will be the first ...Thursday 14 April 2016
- We look at the life of the Chinese artist Ai Wei Wei....Wednesday 30 March 2016
- Have we warmed to the sculpture dubbed 'The Yellow Peril' when it first took pride of place in Melbourne's city square? Artist Ron Robertson-Swann reveals the echoes of Vault hidden around the city....Friday 19 February 2016
Explore ABC South West Vic by Topic
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- Coles managing director John Durkan on setting up a fund for struggling dairy farmers
- Call for jump racing to banned after two horse deaths at Warrnambool
- Veterinarian Dr David Rendell talks about his Parkinson's disease diagnosis and his lifelong exposure to agricultural chemicals
- Commercial fisher Lisle Elleway and Fisheries Victoria executive director Travis Dowling discuss the possibility of a pipi fishery near Portland
- Solid confidence on lamb prices


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Gorgeous! Andres Iniesta back heel flick pass v Real Betis (second half – not the assist)
Grab more information on: Andres IniestaBarcelonaFootball skills
Watch Live Stream
Latest on Andres Iniesta
- Watch Andres Iniesta's spellbinding performance v Sevilla set to Beethoven (Video)May 23rd, 2016
- Andres Iniesta sets a new football record after Barcelona's title winMay 14th, 2016
- Andres Iniesta filmed crying on Barcelona team bus after Atletico defeat (Video)April 14th, 2016
- Barcelona stars Neymar & Andres Iniesta pay tribute to Basketball player Kobe Bryant (Video)April 12th, 2016
Latest on Barcelona
- Dani Alves agrees deal to leave Barcelona for Juventus [Cadena SER]May 25th, 2016
- Barcelona's Leo Messi talks openly about his affection for NBA star Steph Curry (Video)May 25th, 2016
- Spanish press issue mixed reports over Juventus' attempts to sign Barcelona's Javier ...May 25th, 2016
- Barcelona have decided to release Spurs target Sandro Ramirez [Mail]May 24th, 2016
Latest on Football skills
- France star Paul Pogba pulled off 3 awesome pieces of skill v Spain [Video & Vines]September 5th, 2014
- Showboat! Real Madrid & Spain's Sergio Ramos awesome juggling skills in training [Video]September 4th, 2014
- Barcelona's Neymar produces unreal piece of skill in Brazil training today [Vine & Video]September 3rd, 2014
- A SICK nutmeg from the Argentine 2nd tier! Pity Martinez (Huracan) v Sportivo [Video]September 3rd, 2014


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Contemporary conformistsThe ITC Sangeet Research Academy organised an evening of dhrupad on 20 April at its auditorium featuring Pandit Uday Bhawalkar, who was groomed in the age the old Guru-Shishya Parampara and now follows the same traditional path as a guru with the ... The Statesman, 2 weeks ago
Steeped in tradition - The Hindu, 2 months ago
Young practitioners of old tradition - The Statesman, 1 month ago
2 images for "dhrupad"
Flavours of Dhrupad
The performance of German musician Hannah Louise was the highlight of Dhrupad Samaroh in New Delhi. Dhrupad Sansthan, Bhopal, the Gurukul or residential institute of Dhrupad, established by the Gundecha Brothers Ramakant, Umakant and Akhilesh Gundecha, is ...The Hindu, 2 months ago
'More than music, Dhrupad is a philosophy extending all genres'
| Mar 14, 2016, 03.58 AM IST Nagpur: "A lot of cheap and substandard music and films are being dished out under the guise of popular demand. Artists today cover up for their shortcomings by blaming it on audience and saying that this is what people want to ...Times of India, 2 months ago
Assam team for U-11 national chess
GUWAHATI, April 18 - Dhrupad Kashyap of GTC Chess Foundation, Ahiron Kaushik Saikia of Golaghat, Adreeja Sinha of Guwahati and Tanisha AR Som of Jorhat will represent Assam in the 30th National U-11 Chess Championship to be held at Raipur, Chattisgarh from ...The Assam Tribune, 1 month ago
ujjval panchal & kinny soni design mango tree house in india
apr 13, 2016 ujjval panchal & kinny soni design mango tree house in india all images courtesy of dhrupad shukla bhavik satish kadecha the mango tree house, is a private residence in bhopal, india designed by architects ujjval panchal and kinny ...Designboom, 1 month ago
Joy sheer joy…
Simhastha Kala Utsav saw stalwarts performing before devotees. Ujjain, the abode of Mahakaal, witnessed a deluge of devotees rejoicing the holy dip on the banks of river Shipra, on the rare occasion of the Simhastha Kumbh Mahaparva that occurs ...The Hindu, 1 day ago
At the lotus feet of revered gurus
Music flowed in the veins of Professor Dhyanesh Khan, grandson of Baba Alauddin Khan and son of Ustad Ali Akbar Khan. Despite being surrounded by such legendary musicians and despite the heavy burden of this musical family's unmatched status on his ...The Statesman, 6 days ago
When innovation meets tradition
Projects on jewellery and other designs by students of the National Institute of Fashion Technology (NIFT), Hyderabad saw the merger of creativity and new ideas with traditional crafts recently. Can Geisha performances from Japan inspire ...Deccan Chronicle, 6 days ago
A digital success story
The Digital Library of India makes access easy to rare books on literature, science, art, culture and music In early 2000, the Union government initiated a unique project to establish the Digital Library of India (DLI). Its vision was to create a ...Livemint.com, 1 week ago
The legend lives on
Home » Weekend Magazine » December 31, 2011 The Kasur-born nightingale - Noor Jehan, lovingly known as Melody Queen contributed so much to the shaping of Pakistani melodic culture that it is not possible to encompass all that in this short ...Business Recorder, 1 week ago
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Have Gun, Will Travel TV Show Watchlist
Season 1, Episode 3 The Great Mojave Chase
A wager has Paladin riding through the Mojave Desert---on a camel. Kane: Lawrence Dobkin. Paladin: Richard Boone. First Gunman: Claude Akins.
Guest Cast
Claude Akins Claude Akins First Gunman
Cast & Details See all »
- Rating: None
- Premise: One of TV's most successful Westerns told of the hired gun Paladin, who plied his trade in 19th-century San Francisco with a calling card (`Have Gun, Will Travel...') that belied the compelling loner's cultured manner. When he wasn't eating fine food, enga… (more)
Trending TonightSee all »
America's Got Talent8:00 pm | NBCI'll Watch155 Watching
Person of Interest10:00 pm | CBSI'll Watch154 Watching
Roots9:00 pm | A&E, LIFE, HISTI'll Watch65 Watching
Popular Shows
- 1. Game of Thrones
- 2. Castle
- 3. Jane the Virgin
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- 5. Empire
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Popular Movies
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- 1. Kit Harington
- 2. Gina Rodriguez
- 3. Emilia Clarke
- 4. Tom Hiddleston
- 5. Hayley Atwell
- 6. Michael Weatherly
- 7. Melissa Benoist


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Hey, I like the way you think, but to say that "everything in the schedule" sets up for us to have a great year . . .well, I don't see how you can say that when all three main rivalry games are on the road. Now, in 2015 . . .
landing spot. will be interesting to see how he does.


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Kodak Flash Bantam Camera & Model B Flasholder *NICE*
This is a Flash Bantam in very good working condition and very good cosmetically. The lens is clear with no scratches or fungus. Included is the leather carrying case, the original instruction manual, a 828 film box (sorry no film) and a vintage Kodak metal film can.
Also included is a Kodak Model B Flasholder in the original box with all the necessary parts with the original instruction ...
May 27 -
2 Vintage, Worn Ammo Boxes , one is Burrowes
2 vintage ammo boxes, both are worn with some rust. One box is marked "Burrowes," and "reject."
May 27 -
1999 Coca-Cola Anheuser-Busch Santa Character Stein Limited Edition
1999 Coca-Cola Anheuser-Busch limited edition of 10,000 Santa Character Stein, made in Germany. Still have original box, certificate of authenticity and its still protected in original styrofoam. Is about a foot high and in great shape, see pics.
May 26 -
Vintage Milk Can
An older metal milk can in very good condition. Pick up only.
May 25 -
Small Wooden Cabinet
This is a small wooden cabinet. In very good condition. Pick up only.
Portable Crank Up Record Player
This is an older Silvertone Portable Crank Up Record Player. In pretty good condition for it's age. This still plays. There are two records and some paperwork about the player. Pick up only.
Two Small Wooden Tables
Two small wooden tables. In good condition.$25.00 for both. Pick up only.
Small Wooden Table
This is a small wooden table with a magazine rack. In good condition. Pick up only.
Metal Amish Family Group
This is a metal Amish arrangement with a village background. In very good condition.Pick up only.
Older Wooden High Chair
This is an older child's high chair. In very good condition for its age. Pick up only. $45.00.
Wooden Table
This is the shell of a sewing machine. In pretty good condition. I removed the machine. Can still be used. Pick up only.
Gone With The Wind Commemorative Plates
ASHLEY 14310D 2nd Is. - BONNIE AND RHETT 11063A 8th Is.- MAMMY LACING SCARLETT 3211B 5th Is. - MELANIE 1544D 3rd Is.- MELANIE GIVES BIRTH 7292B 6th Is. - SCARLETT 5945H 1st Is. - SCARLETT AND RHETT"'THE FINALE"832B 9th Is. - SCARLETT'S GREEN DRESS 18615C 7th Is. - RHETT 2321J 4th Is. - They are 8 1/2 wide and in excellent condition. Comes with original box and certificate. Never been ...
May 21 -
White Oak
MTH train
MTH Millennium GG1, Gold plated 2K series- not mint because it was opened and sits in a display case- other then that, its like NEW! this includes the PA GG1 and 4 car passenger set (one car shows in image)- beautifuk train! the image doesnt do it justice, im just sizing down my collection- john
May 20 -
Vintage Glass Ferrari Framed Mirror, 19" wide X 15" tall
Vintage glass Ferrari framed mirror, in good shape. Measures 19 inches wide by 15 tall. Lists Ferrari and has Ferrari logo, and reads "Ferrari BB 512, Production Sports Car Champions, Dvr C. Meek." Mirror was handmade in England, see mark.
May 16 -
2 Hand Colored Mezzotint Sets -
Hand Colored Mezzotint Sets Manufacturer/Markings 2 Graces, probably late 19th century. Muses of Literature and music. (Music -- 'Brevi Complector Singula) w/ Cherubs. Borders are barouque/Rococo style (shell forms and classical mask at top) Pattern/Color Golden frame Dimensions 15.5" x 17.5" long.
May need re-framed, but are beautiful!
$35 cash only, you pick-up
please leave name, phone ...
May 15 -
This is from an old Gulf Service Station , was used to test your car battery. In very good condition and would look great in your garage or collection of Gulf items. 4135.00 Steve 724-628-7146
May 15 -
Vintage Star Wars Glasses, Board Game, Sketchbook, Prints, etc.
8 Vintage Star Wars Burger King glasses, 3 from 1980 and 3 from 1983. Two extra of the same glass from 1983. 1977 Darth Vader Metal Necklace, copyright 1977 "20th Century Fox" on back. 1977 complete Kenner Star Wars Escape from the Death Star board game. 1995 Kenner Star Wars Die Cast Metal Toys, 4 piece. Still in packaging, but packaging is beat up. 1983 Ballantine First Edition Star Wars ...
May 14 -
(10) Corvette 1/18 Die Cast Cars , some very rare , all like new in original boxes , would make a great XMAS gift. $40.00 each . Steve 724-628-7146
May 10 -
AEG Westinghouse/People Mover- Skybus, Atlanta Luggage Tag 1980-1990
AEG Westinghouse Transportation Systems Inc,
Hartsfield Atlanta International Airrport 1980-1990 luggage tag $4
People Mover, Skybus
Pittsburgh, PA.
text only 412-807-1115
May 10 -
Lledo Diecast Chevron Red Crown 1927 Gasoline Truck, diecast 1/64
Lledo Diecast Chevron Red Crown 1927 Gasoline Truck 452, Standard the Gasoline of Quality
1/64, Made in England
I have 14 various ones, a few doubles, $3 each or $28 for all.
pittsburgh pa. text only 412-807-1115


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BANGLADESH: Smart Garment owners arrested
Two owners of the unlicensed Smart Export Garments factory have been arrested after seven workers died in a fire at the facility at the weekend.
Factory chairman Sharif Ahmed and managing director Zakir Ahmed were arrested today (30 January), police said.
Workers at Smart Garment earlier this week alleged that all exits at the factory were closed. While fire service and civil defence authorities said no fire extinguishers or fire exits were found at the site, and that the factory owners had never applied for a fire certificate.
An interactive databank with intelligence on the major apparel sourcing countries
Most Popular
- Yarn-forward rules weigh on Vietnam TPP potential
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- M&S to see "departure" of sourcing chiefs?
- Gap accused of rights violations in supply chain
- Gap to close 75 stores amid "disastrous" Q1
- US Q1 in brief - Sears, Abercrombie & Fitch
- H&M criticised for India, Cambodia labour abuses
Market research


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Written on: 25/03/2013
They were selling Elizabeth grant collagen diamond for £24.99 on the net you can purchase this for £22.99 and the red shoe perfume is £11 on the net double that price on bid , don't be ripped off look on net before you purchase anything.
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Stray cats in SLO's North CountyView All Slideshows
Special Features
New Times / Strokes & Plugs
The following articles were printed from New Times [newtimesslo.com] - Volume 28, Issue 38
What's all the HUBbub?
By BEN SIMON
Among the new additions to ThreadHUB's inventory are brands like HUF, 10 Deep, Pink Dolphin, Popular Demand, Young and Reckless, Dimepiece, Joyrich, Forte, and Cote de Nuits, many of which are hugely popular with up-and-coming celebrities. The store likewise deals in designer jean brands including Rock Revival, Crooks & Castles, and Dream Monstar while also carrying decidedly non-designer brands like Levi's. These aforementioned brands span the English-speaking globe from the United Kingdom to Australia while specializing in everything from footwear and socks to hats. Several of these brands, such as the Los Angeles designer company Dimepiece, are exclusively manufactured for women, with "high school moms" as their target demographic. On the contrary, Rock Revival, ThreadHUB's main brand of blue jeans, can only be found in their rare male sizes.
Despite all of its endeavors into higher-end manufacturers and its change in name, ThreadHUB will continue to carry the underground Radlife brand and still displays certain artifacts of its past life including its mural of deceased East Coast rapper The Notorious B.I.G. clad in Radlife fabrics. Furthermore, while its newfound abundance of merchandise renders the store's ability to continue its former tradition of hosting DIY hip-hop and dubstep concerts virtually impossible, the store still sells tickets to similar shows at The Graduate including trance performer Markus Schulz. As per before, the ThreadHUB store will be open from 11 a.m. to 7 p.m. on Mondays through Saturdays, and will be closed on Sundays.
For more information on ThreadHUB or any of its diverse selection of brands, email Micaela Hichborn at email@example.com or call 543-2432.
Fast fact
Got blood? Of course you do. But do you have some blood to spare? If you're feeling generous The Children's Museum at the Paso Robles Volunteer Firehouse is playing host to a Blood Drive and Be the Match Bone Marrow Donor Registration April 26, 11 a.m. to 3 p.m. The museum is located at 623 13th St. in Paso Robles, and all donors will receive a free family play pass as well as refreshments provided by Umpqua Bank and Bonita McGonagill. The event is also a benefit for Madelyn Gonzalez, and donations can be made directly to her family via any Golden 1 Credit Union or by visiting comparing.com/medical-fundraiser/help-maddy-kick-cancer/136288. For questions about the event contact Jennifer Smith at 238-7432 or email firstname.lastname@example.com.
Contributor Ben Simon compiled this week's Strokes. Send your business and nonprofit news to email@example.com.
Santa Barbara supervisors move forward with North County Jail despite a nearly $15 million shortfall Community Notebook 5/26/16 - 6/2/16 Political Watch 5/26/16 Hobnobbing with Helen Can't-abis: Santa Maria issues injunction against a 'dispensary' operating in the city Groundwater basin laws raise concerns in Santa Barbara County Voter registration surges in the 24th District


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Starting this month, school students in my neighborhood will be gathering at the corner, waiting for their big yellow ride to school. Many parents look forward to this day and other parents dread the first day of school.
Yesterday, I had lunch with a couple who had just picked their son up from his first day of preschool. He proudly wore a paper animal on a string around his neck. For this family, days like this are always bittersweet. While they enjoy the things their son is learning, watching him explore his world from an ever changing viewpoint,they think about their daughter Vittoria and wonder what she would be doing right now. Would she be excited for her first day of school? Would she still love to read and draw? Vittoria, who would be 12 this month, died four years ago, waiting for a heart transplant.
Currently, there are 5 children between the ages of 6 and 17 on the Utah waiting list. But what will the new school year hold for these children? Some might be able to attend school. Others may be confined to a hospital while they wait. The reality is one or more of these children may not make the wait for transplant.
While we may not want to think about our own mortality, or that of our children, the reality is that there are some things that we need to consider; like purchasing life insurance, making out a will and organ, eye and tissue donation.
One more organ donor may have saved Vittoria's life. With that thought in mind as the kids go off to school, please discuss donation with your family and then say yes to donation on your driver license or go to www.yesutah.org. You might save the life of someone like Vittoria.
Dixie Madsen
Salt Lake City
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Aided by ISI & IM, Jaish-e-Mohammed planning a Pathankot-II: Military intelligence report
For the new exercise, JeM has opened at least three new 'offices' in Pakistan's Punjab and Khyber Pakhtunkhwa, the report says.
Mohamed A. El-Erian Says Fed is Talking up Rate Increase
A rally that sent global yields to a record low has slowed in the past few weeks as ...
Britain grants refugee status to ex-president of Maldives Mohamed Nasheed : Lawyer
Nasheed was allowed to go to Britain in January for medica...
Jaish-e-Mohammed terrorist from PoK caught, Aadhaar card recovered from him
The official said the operation spanned two months, with security forces keeping a track of Rehman's movement in Valley before finally arresting him.
Court extends police custody of Jaish-e-Mohammed members by 10 days
A Delhi court today extended by 10 days the police custody of three suspected members of terror outfit Jaish-e-Mohammed, arrested for allegedly planning an attack in Delhi.
Amal Clooney winning it for Mohamed Nasheed
Amal Clooney is representing former President Mohamed Nasheed, who was convicted last year on terrorism charges she calls "bogus."
Paris attacks suspect Mohamed Abrini arrested: Police
Paris attacks suspect Mohamed Abrini was arrested today, a police source said after a Belgian television station said he was detained in a Brussels district.
People here know our fight is against fascists: Mohammed Mohsin, AISF
Mohsin said, if elected, his priority would be to address the basic issues in the constituency like shortage of drinking water, unemployment and waste management.
Saudi prince Mohammed bin Salman makes bold challenges to kingdom's old ways
Whether the 31-year-old son of King Salman will achieve his goal of modernising the kingdom's economy is the subject of animated debate on social media, in office buildings and at coffee shops here.
Arrest of Jaish-e-Mohammed suspects confirm Project Karachi poses grave danger to India
They also confirm that Project Karachi - an ISI-backed scheme to train Indians for terrorist acts - continues to pose a grave danger to India.
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|Publication number
|Publication type
|Application number
|Publication date
|Jan 10, 1984
|Filing date
|Dec 9, 1982
|Priority date
|Dec 9, 1982
|Fee status
|Also published as
|Publication number
|Loyd B. Hutchinson
|Original Assignee
|The Dow Chemical Company
|Export Citation
|BiBTeX, EndNote, RefMan
|Referenced by (18), Classifications (8), Legal Events (4)
|External Links: USPTO, USPTO Assignment, Espacenet
The present invention relates to a process for the manufacture of amorphous chlorinated polyethylene. More particularly, the present invention relates to an anhydrous process for preparing amorphous chlorinated polyethylene.
Various processes for chlorinating olefin polymers in general and ethylene polymers in particular are known. The processes can generally be distinguished into three types, namely the chlorination of polyethylene "in solution", "in suspension" or "in bulk".
Chlorination of polyethylene in solution is known from U.S. Pat. No. 3,060,164.
Chlorination of polyethylene in an aqueous suspension is known from U.S. Pat. No. 2,592,763.
U.S. Pat. No. 2,890,213 describes the chlorination of polyethylene in a fluidized bed, and British Pat. No. 834,905 describes the chlorination of free-flowing polyethylene, in each case in the absence of a liquid suspension agent or solvent, the so-called "chlorination in bulk."
The chlorinated polyethylenes obtained by these different chlorination methods show differences in properties, even if one starts from the same polyethylene material, and chlorinates to the same chlorine content. This appears to be connected principally with the more or less statistical distribution of the chlorine in and along the chlorinated polyethylene polymer chains, as is explained in French Pat. No. 1,316,044 and in British Pat. Nos. 843,209 and 950,374. Chlorinated polyethylenes with a non-statistical distribution of the chlorine atoms possess a much higher glass transition temperaure than do chlorinated polyethylenes having a statistical chlorine distribution, and are also much more rigid, hard and brittle.
A number of disadvantages attach to each of the aforementioned three methods, chlorination in solution, in suspension, or in bulk.
The process of chlorination in solution is expensive. The solubility of polyethylene in organic solvents which are inert to chlorine is relatively small, thus large quantities of solvent are needed. As a rule, expensive polyhalogen hydrocarbons must be used for this purpose. The chlorinated polyethylene product must also be later freed from solvent and removal of the last traces thereof is difficult. The separation itself is cumbersome and expensive.
At relatively low temperatures, the chlorination of polyethylene in suspension does not proceed in a statistical manner. A kind of block copolymer structure, having both chlorinated and non-chlorinated segments in the molecule, appears to be obtained, unless the chlorination is continued for very long times until high chlorine contents result. Although a variety of chlorinated polyethylene products may be produced by suspension chlorination, a number of disadvantages are inherent in a suspension chlorination process. First, effluent from the process is a relatively weak hydrochloric acid which must be substantially removed from the chlorinated polyethylene product. Removal generally requires use of a material such as caustic soda which results in an undesirable salt-containing effluent. Second, the chlorinated polyethylene products so produced must be dried before packaging. A third disadvantage is corrosion of processing equipment due to presence of aqueous mixture of chlorine and hydrochloric acid.
Usually, however, it is desired to obtain a soft and flexible chlorinated polyethylene with a crystallinity of less than about 2 percent. In other words, the chlorinated polyethylene should be fully or at least generally amorphous.
In French Pat. No. 1,316,044, a two-stage process has been described for obtaining generally statistical chlorination of polyethylene. In the two-stage process, the second stage is carried out at a rather high temperature, above the crystalline melting point of the polyethylene. "Crystalline melting point" as used herein means the temperature at which crystallinity disappears as evidenced by disappearance of double refraction, or characteristic X-ray diffraction lines. Preferably, the disappearance of crystallinity is measured by Differential Scanning Calorimetry.
Chlorination in suspension at a high temperature introduces the disadvantage that, at such high temperatures, and even under pressure, chlorine will dissolve to only a very small degree in the suspension agent (which is generally water). Subsequent processing of the product by centrifuging and drying is also expensive. Moreover, the by-product, hydrogen chloride, generally cannot be usefully recovered.
In British Pat. No. 843,209 the differences between chlorinated polyolefins with a statistical and a nonstatistical chlorine distribution are also discussed. Intermediate forms thereof are called hybrid polymers. The hybrid polymers are prepared according to British Pat. No. 843,209 by carrying out the chlorination partly in suspension and partly in solution. However, such a process is very cumbersome. The polyethylene chlorinated in suspension must first be separated from the suspension, and then subsequently dissolved. Only then can the second solution stage be carried out.
Chlorination in bulk, as described in U.S. Pat. No. 2,890,213 and British Pat. No. 834,905, can be carried out at rather high temperatures, with the chlorination reaction proceeding rather rapidly. However, a disadvantage of this method is that the chlorination generally proceeds too fast during the initial phase. Since chlorination is an exothermic reaction, when finely divided polyethylene is chlorinated without a solvent or suspension agent local overheating of the polymer occurs very easily. As a result, reaction speed is locally increased in those places. Local development of heat can in turn cause melting, agglomeration and lump formation, as well as decomposition and even burning of the polymer. These circumstances are also attended by the development of an extremely undesirable discoloration in the product.
Chlorinations partly at temperatures below the crystalline melting point and partly above the crystalline melting point are not only known from French Pat. No. 1,316,044 and British Pat. No. 843,209, but also from U.S. Pat. Nos. 2,398,803; 2,920,064; and British Pat. Nos. 1,073,504 and 1,036,360.
When chlorinating in bulk, it is also difficult to avoid sintering of the ethylene polymer particles to some degree. This forms agglomerates which, in turn, cannot be homogeneously chlorinated. The ethylene polymer also becomes discolored due to hot spots. To avoid such discoloration, it has been proposed that chlorination be carried out at low temperatures to minimize the occurrence of hot spots. The temperatures at which such chlorination is to be carried out, at 60° to 70° Centigrade (°C.), are considerably below the crystalline melting point. Low temperature chlorination must be continued until a certain minimum chlorine content is achieved. Only then can the reaction temperature be increased to a temperature above the crystalline melting point of the polyethylene. If the initial low temperature chlorination has been inadequate, further chlorination at the higher temperature will still lead to development of hot spots, agglomerations and attendant discoloration. However, chlorination at temperatures below the crystalline melting point of the polyethylene for an extended period of time generally results in production of large amounts of hard and brittle chlorinated polyethylene.
To eliminate such objections and disadvantages of the chlorination process in bulk, it has also been proposed to mix the ethylene polymer with inorganic salts, which are then to be washed out after the chlorination. Washing out and recovering, and/or discharging those salts, is, however, expensive, and renders this process economically unattactive.
An additional proposal to eliminate such disadvantages centers around selection of the polymer to be chlorinated. In U.S. Pat. No. 4,029,862, the olefin polymer to be chlorinated is characterized by having a flowability measured as angle of repose in the range of from about 24° to about 28°, a bulk density in the range of from about 25 to about 35 pounds per cubic foot and a surface area in the range of from about 2 to about 4 square meters per gram. The polymer is chlorinated to an extent of up to about 65 percent by weight chlorine using reaction temperatures not exceeding about 80° C. to provide a chlorine content of up to about 30 percent by weight and thereafter maintaining the reaction temperature from about 60° C. to about 100° C. In U.S. Pat. No. 4,197,386 an ethylene polymer starting material has the following combination of characteristics: (i) at most 5 mole percent of at least one α-alkene comonomer having from 3 to 8 carbon atoms, particularly propene or butene, (ii) having a density of 0.930-0.970, (iii) a melt index of at most about 5, (iv) a particle size distribution of between about 50 to 2000 microns, (v) a porosity of at most about 0.15 cubic centimeters per gram, (vi) a surface area determined in accordance with the method described in J. Am. Chem. Soc. 60 309 (1938) by Braunauer, Emmet and Teller of at most about 1 square meter per gram and (vii) a wax content of at most about 1 percent by weight.
In view of the foregoing, it is an object of the present invention to provide a process for preparing amorphous chlorinated polyethylenes which are generally soft and flexible yet free of discoloration.
It is also an object of the present invention to provide a non-crystalline, amorphous chlorinated polyethylene having satisfactory properties such as good flexibility and high elongation. Such chlorinated polyethylenes are suitable for use as impact modifiers in polyvinylchloride.
These and related objects are realized in an anhydrous free radical process for preparing amorphous chlorinated, solid, finely divided polyethylene particles; said process employing a free radical initiator, a flow of gaseous chlorine and agitation of the particles sufficient to expose generally all of said particles to the flow of gaseous chlorine, the process comprising a series of sequential steps:
(a) starting addition of gaseous chlorine to an agitated mass of porous, finely divided polyethylene particles, the particles being exposed to a free radical initiator, while said mass is at a temperature within a temperature range of from about 25° to about 50° Centigrade;
(b) continuing addition of gaseous chlorine to the agitated mass while continuing to expose the mass to a free radical initiator and while increasing the temperature of said mass over a temperature range of from about 50° Centigrade to about 105° Centigrade and maintaining the temperature within said temperature range until a level of chlorination of the agitated mass of from about 5 to about 15 percent by weight of said mass is attained;
(c) continuing addition of gaseous chlorine to the agitated mass while continuing to expose the mass to a free radical initiator and while further increasing the temperature of said mass to a temperature of from about 125° Centigrade to about 132° Centigrade, said temperature being increased at a rate which is sufficiently slow to preclude sintering of the agitated mass; and
(d) continuing addition of gaseous chlorine to the agitated mass while continuing to expose the mass to a free radical initiator and while further increasing the temperature of said mass to a temperature which is greater than about 130° Centigrade yet less than a temperature at which sintering of the agitated mass occurs and maintaining said temperature for a period of time sufficient to attain a predetermined level of chlorination and a predetermined level of relative crystallinity.
The amorphous chlorinated, solid, finely divided polyethylenes so prepared unexpectedly have very low blocking values. As used herein, the term "blocking" means the tendency of a powdered chlorinated polymer resin to clump, cake or agglomerate. The low blocking values are obtained without addition of conventional antiblock additives.
The term "olefin polymer" means polymers of olefins in which the backbone chain of the polymer macromolecule is substantially noncross-linked and nonbranched. The term "olefin polymers" includes polymers of the ethylene, propylene, butene-1 and higher 1-alkenes having 5 to 10 carbon atoms in which polymer the linear main chain has substituent ethylene mer units. As used herein, the term "olefin polymers" is also meant to include homopolymers, copolymers and interpolymers of 1-alkenes and mixtures and blends thereof. The molecular weights of olefin polymers used in the practice of this invention are comparable to those of olefin polymers produced in conventional Ziegler-Natta polymerization processes, e.g., from about 30,000 up to about 3 million or more.
For purposes of this invention, the term "polyethylene" is used to denote preferred olefin polymers and means homopolymers of ethylene and copolymers of ethylene and up to about 5 weight percent of aliphatic α-monoolefin or α-diolefin having from 2 to 18 carbon atoms. Illustratively, such α-olefins can include propylene, butene-1, pentene-1, 3-methylbutene-1, 4-methylpentene-1, hexene-1, octene-1, dodecene-1, octadecene-1, 1,7-octadiene and the like. Such polyethylenes have absolute densities in the range from about 0.90 to about 0.97 grams per cubic centimeter (g/cc), especially from about 0.935 to about 0.967 g/cc. Such polyethylenes also have melt indexes, as determined by the American Society for Testing Materials (ASTM) test D-1238-65T, Condition E (hereinafter ASTM D-1238-65T(E)) in the range of from about 0.01 to about 40 decigrams per minute, especially from about 0.1 to about 12 decigrams per minute and most especially from about 0.15 to about 3 decigrams per minute.
The olefin polymers employed in the practice of this invention are in the form of normally extrudable, free flowing powder having a bulk density in the range of from about 18 to about 35 pounds per cubic foot, especially from about 20 to about 25 pounds per cubic foot. The particles of such powder are generally free flowing, porous particles having individual sizes suitably within the range of from about 40 to about 600 microns, beneficially from about 100 to about 400 microns, and desirably from about 100 to about 200 microns. The powder suitably has a generally uniform, narrow particle size distribution in the range of from about 100 to about 200 microns. It is generally recognized that excessive fines are carried out of a fluidized bed reactor by a fluidizing medium. The particle sizes must, however, not be so large as to result in an undesirably low level of chlorination.
The olefin polymer powders used in the present invention are beneficially made under conditions characteristic of Ziegler polymerization in the presence of a catalyst prepared from an organomagnesium component which does not generally reduce titanium tetrachloride at a temperature of 25° C. The catalyst is prepared in accordance with U.S. Pat. No. 4,244,838, the teachings of which are incorporated herein by reference thereto. A process for preparing olefin polymer powders which employs the catalyst is taught in U.S. Pat. No. 4,246,383, the teachings of which are incorporated herein by reference thereto.
It is understood, however, that other processes capable of producing olefin polymer powders in general, and polyethylene powders in particular, having the aforementioned properties are also suitably employed in the practice of this invention.
For purposes of the present invention, the chlorination of such olefin polymer powders may be effected in various ways. It is possible, for example, to agitate the granular polymer by means of stirring devices while exposing it to the action of a current of chlorine, in the substantial absence of oxygen, wherein the chlorine has preferably been preheated. Various apparatus which are equipped with efficient agitating means may be employed to accomplish such agitation and exposure to chlorine. Illustrative apparatus include reactors having paddle agitators or other agitation means, and rotating cylinders which may be provided with internal mixing baffles other agitation means. The apparatus may be vertically or horizontally disposed, or may be inclined from the horizontal to facilitate a continuous internal passage of solid material therethrough during operation. As an alternative, the material may be thoroughly exposed to the halogen atmosphere and effectively agitated by conducting the reaction according to well-known fluid bed techniques. When using fluid bed techniques, a current of halogen atmosphere is passed through a finely divided and free-flowing layer (fluidized bed) of the material to be halogenated. The passage or forcing of the halogen atmosphere through the fluidized bed is done at a rate sufficient to accomplish a thorough agitation and exposure of the material being halogenated. Any apparatus in which a free-flowing mass of polymer may be thoroughly subjected to a halogen atmosphere at a desired temperature or over a desired temperature range may be suitably employed for conducting the reaction according to the present invention. Fluorine and vaporized bromine, or mixtures of these may advantageously be used in conjunction with gaseous chlorine to constitute the halogen atmosphere of the present invention. Beneficially the halogen atmosphere of the present invention predominantly comprises gaseous chlorine. In certain instances it may be desirable for the halogen atmosphere to contain inert gases and vapors as diluents or carriers. Inclusion of an inert gas may permit a better control over the reaction. In some instances it may also be advantageous to have only portions of the halogen atmosphere diluted when a continuous process is being employed or to have it diluted only during particular intervals in a batch reaction. In this manner, it is possible in the course of a particular halogenation reaction to adjust reaction conditions to suit the changing reactivity, at various halogen contents, of the olefin polymer powder being halogenated.
Any compatible gas or vapor which, under the reaction conditions, is inert to both the halogen atmosphere and the olefin polymer powder being halogenated may be used as a diluent for the halogen atmosphere. Helium and the inert gases, nitrogen, hydrogen halides; and perchloro, perfluoro, or fluoro-chloro hydrocarbons are examples of suitable diluents. Recycling of the hydrogen halide formed during the reaction will also provide a suitable means for diluting the halogen atmosphere. It may sometimes be desirable to externally cool the hydrogen halide formed during the reaction when it is being recycled as a diluent. This may furnish an effective means for controlling the temperature of the reaction within a desired range.
The polymer and the halogen atmosphere are beneficially anhydrous, or dry in the physio-chemical sense. If anhydrous conditions are not maintained, any water which is present will be vaporized and converted to steam. The steam will add pressure to the reactor and will contribute to corrosion problems. Accordingly, reactor design and construction would have to be changed if water were present. In addition, initiation of the chlorination reaction, which will be detailed hereinafter, would be altered if water were present.
Temperatures suitable for halogenation of the olefin polymer powder will vary within limits depending upon a variety of factors and conditions. Temperatures will generally be governed by the mutual reactivity of the particular olefin polymer powder and halogen atmosphere which are being employed and by the extent of halogenation desired. The reactivity of the halogen atmosphere depends directly on the particular halogen or halogens contained therein and, upon effective concentration of said halogen or halogens. The reactivity of the polymer being halogenated is initially fixed by the character of the parent material but may change in the course of a given reaction with a changing halogen content in such polymer. The particle size or shape of the polymer being halogenated may also influence the reaction. Particles having greater surface areas, particularly smaller sized particles or those with crenulated or otherwise irregular configurations, are generally more conducive to a halogenation reaction. The rate of reaction at any given temperature is also largely dependent upon the rate of diffusion of the halogen from the halogen atmosphere into the polymer being halogenated and upon the capacity of the polymer at such temperature to absorb the particular halogen which is involved.
It has been found that amorphous halogenated olefin polymers, specifically amorphous chlorinated polyethylenes, are prepared by a process which involves at least four steps. In a first step, using chlorinated polyethylene by way of example, addition of gaseous chlorine to an agitated mass of porous, finely divided polyethylene particles, the particles being in admixture with an initiator, is started while said mass is at a temperature within a temperature range of from about 25° to about 50° C. It has been found that delaying addition of chlorine until the agitated mass of polyethylene particles has been heated to a temperature greater than about 50° C. produces undesirable results. One of the undesirable results is that the polymer particles cannot be maintained in a fluidized or agitated state. Loss of the fluidized state is evidenced by a caking up of the polymer powder. It has been found that little, if any, halogenation actually takes place during the first step. As hereinabove noted, however, the first step is critical. In a second step, addition of gaseous chlorine to the agitated mass is continued while the temperature of said mass is increased over a temperature range of from about 50° C. to about 105° C. The temperature of the agitated mass is maintained within the temperature range until a level of chlorination of the agitated mass of from about five to about fifteen percent by weight of said mass is attained. It has been found that, with a level of chlorination of less than about five percent by weight, the agitated mass of polyethylene particles tends to agglomerate as chlorination at higher temperatures is attempted. It has also been found that with a level of chlorination of greater than about fifteen percent by weight of said mass in the second step, an undesirably stiff chlorinated polyethylene product results once chlorination is completed. A nominal melting point for polyethylene is 130° C. It has been found that as the polymer is chlorinated, the melting point decreases to a minimum of about 106° C. at a level of chlorination of about 12 percent by weight of chlorinated polymer. As the level of chlorination is increased above about 12 percent by weight of chlorinated polymer, the melting point begins to increase above the minimum. As one exceeds the melting point, sufficient melting of at least surface portions of polymer particles occurs to cause the polymer particles to begin to agglomerate. As a maximum level of chlorination of about fifteen percent by weight of the agitated mass occurs during the second step, the temperature of said mass during the second step should not exceed about 105° C. In a third step, addition of gaseous chlorine to the agitated mass is continued while the temperature of said mass is further increased to a temperature of from about 125° C. to about 132° C. The temperature of said mass is increased at a particular rate which is sufficiently fast to be economical yet sufficiently slow to generally retain a porous particulate structure and to generally prevent sintering of the partially chlorinated polyethylene particles. It has been found that a rate of heating which is too rapid generally results in a chlorinated polyethylene product which is not amorphous after chlorination is terminated. The term "amorphous" as used herein describes a chlorinated polymer having a percent relative crystallinity suitably less than about two percent, beneficially less than about 0.5 percent, desirably less than about 0.3 percent. A rate of heating which is too rapid may also result in agglomeration of the partially chlorinated polyethylene particles. An agglomerated or sintered mass of partially chlorinated polyethylene particles is of no practical use. In light of the foregoing, a suitable rate of heating is from about 0.15° to about 0.36° Centigrade per minute. Beneficially, the rate of heating is from about 0.20° to about 0.36° Centigrade per minute. Desirably, the rate of heating is from about 0.25° to about 0.32° Centigrade per minute. In a fourth step, chlorination of the polyethylene particles is completed. Addition of gaseous chlorine to the agitated mass is continued while the temperature of said mass is further increased to a temperature greater than about 130° C. but less than a temperature at which the particles begin to agglomerate. The temperature must be sufficiently high to produce an amorphous polymer as defined herein by destroying generally all residual crystallinity. The temperature must also be sufficiently low to preclude formation of large lumps or agglomerates of particles. The presence of agglomerates renders a product generally unsuitable for commercial use. It has been found that temperature of up to about 145° C. may be used for the fourth step without detriment. Persons skilled in the art will recognize that temperatures sufficiently in excess of 145° C. will cause the particles to coalesce into one or more large lumps.
Halogen levels of from about 20 to about 50 percent by weight of halogenated polymer may be obtained in accordance with the present invention. Beneficially amorphous chlorinated polyethylenes having a chlorine content, based on chlorinated polymer weight, of from about 25 to about 45 weight percent are obtained. Desirably such chlorinated polyethylenes have a chlorine content of from about 30 to about 42 weight percent. Persons skilled in the art will recognize that chlorinated polyethylene having a chlorine content of 60 weight percent or more will tend to be a glassy material rather than a rubbery material.
Although the rate of halogenation increases with temperature, care should be taken to avoid higher temperatures which may sinter, fuse or char the polymer. When this occurs it becomes more difficult to keep the finely divided polymer in a proper state of agitation and it may cause non-uniformity in the product. In addition, the halogenation reaction is seriously impeded with a sintered polymer because exposed particle surface area is markedly reduced by sintering.
The halogenation reaction of the present invention may be conducted under any suitable pressure. Beneficially, it is carried out at atmospheric pressure. The reaction may, however, be carried out at superatmospheric pressure in order to hasten the rate of reaction. Satisfactory results may also be obtained when the reaction is being conducted under atmospheric pressure by employing a halogen atmosphere which contains amounts of the halogen in excess of stoichiometric requirements. When the reaction is conducted under superatmospheric pressure, care should be exercised to adequately vent by-product materials which are formed in order to maintain an effective halogen level in the halogen atmosphere.
The halogenation reaction of the present invention is suitably carried out in the presence of a free radical initiator. The free radical initiator is suitably selected from the group consisting of chemical free radical forming initiators, free radical forming radiation and a combination of free radical forming radiation and one or more chemical free radical forming initiators.
Free radical forming radiation must have a wavelength sufficient to activate the halogen. In general, suitable results are obtained by employing ultraviolet radiation having a wavelength in the range of from about 3000 to about 4500 Angstroms (Å). Beneficial results have been obtained by using ultraviolet radiation having a wavelength of from about 3350 to about 3650 Å.
Suitable chemical free radical forming initiators are: peroxides and hydroperoxides, for instance benzoylperoxide, diisopropylperoxydicarbonate, benzoylhydroperoxide, cumenehydroperoxide, lauroylperoxide, and the like, azo compounds in particular those with a nitrile group at a carbon atom which is adjacent to an azonitrogen atom, like dimethyl and diethyl, α,α'-azodiisobutyronitrile and α,α'-azobis(α,ε-dimethylvaleronitrile). Other known initiators can be used in the process according to the invention.
The following example illustrates the invention but should not be considered as limiting its scope. All parts and percentages are by weight unless otherwise indicated.
General Procedure
A. Ethylene Polymer
In each of the following examples, polyethylene powders having melt index values I2, as determined by ASTM D 1238, Condition E, of 0.1, 0.4, or 11.4 decigrams per minute were, unless otherwise specified, prepared in accordance with U.S. Pat. No. 4,246,383 cited hereinabove. The melt index value I2 of the powder used in each example is set forth in a table which summarizes the examples.
B. Chlorination Apparatus
A 4 inch by 36 inch vertically arranged Pyrex® glass tube, having a 12 inch portion of the inside thereof adjacent one end (hereinafter the "bottom end") covered with a 1/16 inch sheet of a fluorinated ethylene-propylene fluorocarbon polymer commercially available from E. I. duPont de Nemours and Co. under the trade designation Teflon™, served as a reactor vessel. A truncated hollow right cylinder conical insert made of polytetrafluoroethylene was fitted into the bottom end of the tube. The conical insert had a large opening and a small opening. The large opening had a diameter of about 4 inches. The large opening was positioned so that it was remote from rather than proximate to the bottom end of the tube. The small opening had a diameter of about 1.3 inches and was positioned so that it was proximate to the bottom end of the tube. Adjacent to the conical insert and arranged so as to cover the bottom end of the tube was a screen assembly. The screen assembly had four layers arranged as follows: (a) a 200 mesh screen of polytetrafluoroethylene; (b) a woven mat made of glass fibers, commercially available from Owens-Corning Fiberglas Corporation under the trade designation Fiberglas™; (c) a 400 mesh stainless steel screen; and (d) a 20 mesh stainless steel screen. Layer (a) was placed next to the conical insert. A metal funnel, having the larger opening adjacent layer (d) of the screen assembly was connected to the bottom end of the tube. The stem or smaller opening of the funnel was connected to a gas supply line which in turn was connected to an overpressure relief valve set at 50 pounds per square inch, a gaseous chlorine supply line and a gaseous nitrogen supply line. By a suitable arrangement of check valves and blocking valves, a ratio of gaseous chlorine to gaseous nitrogen could be established. The gaseous nitrogen supply line had incorporated therein an electrical heater for the gaseous nitrogen. A set point controller was used to maintain the temperature of the nitrogen at a manually selected temperature. One thermocouple was placed inside the tube near the screen assembly to measure powder temperature. A second thermocouple was placed inside the metal funnel to measure inlet temperature of the nitrogen gas or nitrogen/halogen gas mixture. A cap connected to a scrubber was fitted with a second end of the tube (hereinafter referred to as the "top end").
C. Procedure
A sample of the ethylene polymer powder to be chlorinated was placed into the reactor vessel. The powder was then made free of oxygen by passing a dry and pure gaseous nitrogen stream through the reactor vessel until the powder was heated to temperature of about 40° C. Heating of the reactor vessel and the polymer powder contained therein was accomplished by heating the nitrogen stream. The flow of nitrogen gas, regulated at 2.0 cfm, was sufficient to fluidize the polymer powder. Gaseous chlorine was added to the gaseous nitrogen during heating of the polymer powder from a temperature of about 25° C. to about 50° C. The polymer powder temperature at which gaseous chlorine was introduced into the reactor vessel is hereinafter set forth in the table. A nitrogen to chlorine ratio of 10:1 was used unless otherwise specified. The final temperature is hereinafter specified unless chlorination was terminated prior to reaching the final temperature. After chlorination was completed, ambient temperature gaseous nitrogen was passed through the polymer powder until the polymer powder was at a safe handling temperature of less than about 80° C. The powder was then removed from the reactor.
D. Polymer Property Tests
Melt Index - I2 - Melt index in decigrams/minute as determined respectively by ASTM Test No. D-1238-64T, Condition E.
Crystallinity - percent relative crystallinity.
TABLE I__________________________________________________________________________ Rate TempPoly- Total Increaseethylene Reaction in StageExampleMelt Cl2 Start Time Stage 3 Max temps °C. % %No. Index Temp. °C. Hrs/min °C./min 2 3 4 Cl2 Cryst Remarks__________________________________________________________________________**1 0.4 65/49 7/0 0.3 97 130 130 33.9 <0.1 some black specks, no lumps, see Note 1**2 0.4 25 5/45 0.33 99 131 131 37.5 <0.1**3 0.1 26 5/15 0.3 100 128 129 35.1 <0.5**4 0.4 40 5/20 0.36 101 130 131 36.5 <0.1**5 0.1 33 4/58 0.25 96 129 129 39.5 <0.36 0.4 41 1/30 -- 75 -- 98 13.8 * no lumps7 0.4 71 0/38 -- 75 -- 98 * * fluidization lost8 0.4 44 1/30 -- 86 -- 75 * * N2 contaminated w/120 ppm O29 0.4 40 5/10 0.43 99 129 129 * ˜5 no specks or lumps10 0.4 33 5/35 0.7 99 132 130 ˜35 ˜10 fast third stage**11 0.1 40 3/18 0.3 99 132 132 34.3 ˜2**12 0.1 42 4/0 0.25 101 129 129 37.3 ˜1**13 0.1 37 4/10 0.29 96 126 127 36.9 ˜2 temp profile14 11.4 42 3/14 0.43 93 128 146 * * one big lump15 11.4 31 2/0 * 105 -- 105 * * trouble con- trolling temperature and fluid- ization16 0.1 33 * * 96 -- 110 * * See Note 217 11.4 37 4/45 0.30 90 120 136 35.4 0.12__________________________________________________________________________ *not measured **the invention Note 1 The flow of gaseous chlorine was started at 65° C. The powder caked up and fluidization was lost. After the caked powder was cooled to a temperature of about 49° C., it returned to a freeflowing powder state. The flow of gaseous chloride was then restarted Note 2 The purpose of this example was to evaluate the effect of blocking ultraviolet light from the reactor. This was done by wrapping the reactor vessel in aluminum foil. Chlorination ceased while the reactor was wrappe in aluminum foil. Upon removal of the foil, chlorination started. Rewrapping the reactor in foil caused cessation of chlorination.
A review of the preceding examples 1-17 is instructive because it shows the necessity (a) of maintaining a generally oxygen-free atmosphere (Example 8), (b) of starting addition of chlorine gas at a temperature of less than 50° C. (Example 7), (c) of maintaining a proper rate of temperature increase in stage 3 (Example 10) and (d) of the presence of ultraviolet light to catalyze the chlorination reaction (Example 16). Similar results are obtained with other olefin polymer powders and with other halogens or halogen mixtures in accordance with the present invention.
Blocking Test
In the blocking test, an attempt is made to form a tablet or cake by compressing a 50 gram quantity of powdered chlorinated polyethylene resin in a mold. The tablet, if formed, is then pressed with a sharp edge of a wedge until the tablet is ruptured. A measure of the relative force required to rupture the tablet provides an indicator of the tendency of a resin to block.
Results of Blocking Test
A portion of the polymer prepared in Example 1 was placed into the mold and compressed. The tablet so formed returned to granular form on removal from the mold. Accordingly, the polymer of the present invention had a relative blocking value of zero. A slurry chlorinated polyethylene (36 percent by weight chlorine) compounded with conventional antiblock additives had a relative blocking value of about 25. The same polymer without antiblock additives had a relative blocking value in excess of ten times that of the polymer compounded with antiblock additives. This relatively simple test clearly demonstrates that a reduced blocking tendency is available from the process of the present invention. Similar beneficial results are obtained with other chlorinated polyethylene resins prepared in accordance with the present invention.
|Citing Patent
|Filing date
|Publication date
|May 14, 1984
|Jun 3, 1986
|Union Carbide Corporation
|Preparation of elastomeric, chlorinated ethylene polymers
|Dec 17, 1984
|Jul 22, 1986
|Basf Aktiengesellschaft
|Chlorination of polymers
|Jul 7, 1986
|Nov 10, 1987
|The Dow Chemical Company
|Process for preparing a porous polymer article
|May 5, 1986
|Nov 17, 1987
|The Dow Chemical Company
|Low viscosity, semicrystalline chlorinated polyethylene resins and articles formed therefrom
|Mar 2, 1987
|May 24, 1988
|Kanegafuchi Kagaku Kogyo Kabushiki Kaisha
|Polyolefin particles and process for preparing the same
|Jul 24, 1987
|Jun 14, 1988
|The Dow Chemical Company
|Low viscosity, semicrystalline chlorinated polyethylene resins and articles formed therefrom
|Mar 30, 1987
|Dec 27, 1988
|Agency Of Industrial Science And Technology
|Method for graft polymerization of acetylene compound on a shaped polymer article
|Sep 28, 1987
|May 8, 1990
|The Dow Chemical Company
|Oxidation of halogenated polymers
|Nov 22, 1988
|Jul 31, 1990
|The Dow Chemical Company
|Oxidation of halogenated polymers and anticaking halogenated polymers
|Apr 30, 1990
|Nov 26, 1991
|Kang Hee Dong
|Process for the chlorination of polyolefins
|Nov 17, 1997
|Jul 27, 1999
|Bp Chemicals Limited
|Apparatus and process for polymerising olefin in gas phase
|Feb 12, 1996
|Jul 27, 1999
|Bp Chemicals Limited
|Apparatus and process for polymerising olefin in gas phase
|Mar 31, 1998
|Sep 26, 2000
|The B. F. Goodrich Company
|Blocky chlorinated polyolefins, process for making and use as impact modifier compatibilizer for PVC or CPVC
|Aug 4, 1999
|Mar 20, 2001
|The B. F. Goodrich Company
|Blocky chlorinated polyolefins, process for making and use as impact modifier compatibilizer for PVC or CPVC
|Sep 29, 1999
|Aug 21, 2001
|Pmd Holdings Corporation
|Block chlorinated polyolefins for use as impact modifier enhancers for PVC or CPVC
|May 4, 1990
|Nov 8, 1990
|Kang Hee Dong
|Chlorinating mixt. of finely divided polyolefin - and anti-coagulating agent in presence of free radical accelerator, avoiding liq. or gaseous media
|Jul 22, 1987
|Jan 26, 1989
|The Dow Chemical Company
|Low viscosity, semicrystalline chlorinated polyethylene resins and articles formed therefrom
|Mar 18, 1999
|Oct 7, 1999
|The B.F. Goodrich Company
|Blocky chlorinated polyolefins, process for making and use as impact modifier compatibilizer for pvc or cpvc
|U.S. Classification
|522/131, 525/333.8, 525/334.1, 522/133, 525/356
|International Classification
|Cooperative Classification
|European Classification
|Oct 14, 1983
Owner name: DOW CHEMICAL COMPANY THE
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:HUTCHINSON, LOYD B.;REEL/FRAME:004177/0679
Effective date: 19821207
Owner name: DOW CHEMICAL COMPANY THE, STATELESS
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:HUTCHINSON, LOYD B.;REEL/FRAME:004177/0679
Effective date: 19821207
|Apr 9, 1987
|Fee payment
Year of fee payment: 4
|May 3, 1991
|Fee payment
Year of fee payment: 8
|Apr 11, 1995
|Fee payment
Year of fee payment: 12


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Multilayer circuit board and method of manufacturing the same
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United States Patent #6701613
In a method of manufacturing a multilayer circuit board, cable patterns in a plurality of cable layers can be precisely formed, and the cable layer are formed with higher density, with higher reliability. The multilayer circuit board comprises: a plurality of cable layers, each of which includes electric conductive sections; a plurality of first insulating layers, each of which encloses the electric conductive sections in each cable layer and fills spaces between the electric conductive sections; and post vias electrically connecting the electric conductive sections in one cable layer to those in another cable layer. Height of the electric conductive sections in each cable layer are equal to that of the first insulating layer enclosing those electric conductive sections.
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Koji Uehara named to All-Star team in place of Masahiro Tanaka
|07.09.14 at 8:59 pm ET
With Yankees starter Masahiro Tanaka unavailable to pitch in the All-Star Game due to elbow inflammation, Red Sox closer Koji Uehara has been added to the American League roster for the showcase. Uehara is making the All-Star team for the first time.
Here is the Red Sox press release announcing Uehara's addition:
Red Sox right-handed pitcher Koji Uehara was added to the active American League roster for Major League Baseball's 85th All-Star Game, which will take place on Tuesday, July 15 at Target Field in Minneapolis, MN. He replaces right-handed pitcher Masahiro Tanaka of the New York Yankees, who was placed on the disabled list today.
Major League Baseball and Red Sox Manager John Farrell, who is guiding the American League All-Star team, made the announcement.
This is the first major league All-Star selection for Uehara, 39, who was an All-Star for the Yomiuri Giants of Nippon Professional Baseball eight times (1999-2005, 2007).
The Red Sox' closer is 4-2 with 18 saves this season. He owns a 1.30 ERA (6 ER/41.2 IP) and 52 strikeouts compared just six walks and 25 hits allowed. Entering today, he ranked among AL relievers in save percentage (2nd, 94.7), WHIP (2nd, 0.74), ERA (3rd, 1.30), strikeout/walk ratio (3rd, 8.7), wins (T-3rd), saves (5th), walk rate (6th, 1.3 BB/9.0 IP), and strikeouts (T-6th, 52).
In the 2013 regular season, Uehara notched 21 saves and went 4-1 with a 1.09 ERA (9 ER/74.1 IP). With only 33 hits and seven walks allowed, he posted the best single-season WHIP in major league history among pitchers with at least 40.0 innings (0.57). He also became the first major leaguer ever with at least 100 strikeouts (101) and fewer than 10 walks allowed (9) in a season, and set an AL record for scoreless appearances with 44.
Uehara recorded saves in all seven chances during the Red Sox' postseason run to the 2013 World Series Championship and was named MVP of the American League Championship Series.
Only five other first-time MLB All-Stars have been older than Uehara: Satchel Paige (46 in 1952), Tim Wakefield (42 in 2009), Arthur Rhodes (40 in 2010), Jamie Moyer (40 in 2003), and Connie Marrero (40 in 1951).
In 113 appearances since joining the Red Sox in 2013, Uehara is 8-3 with 39 saves, a 1.16 ERA, with 153 strikeouts and just 15 walks in 116.0 innings.
Over parts of six seasons in the big leagues with the Orioles (2009-11), Rangers (2011-12), and Red Sox (2013-14), Uehara has gone 13-12 with 53 saves and a 2.28 ERA (83 ER/327.2 IP) in 270 outings, including 12 starts. With just 44 walks allowed and 384 career strikeouts, he owns the best strikeout-to-walk ratio in major league history among pitchers with at least 100.0 lifetime innings.
Among those representing the Red Sox, Uehara will join teammate Jon Lester, as well as Farrell and his coaching staff, at the Midsummer Classic.
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