KR840008385A - 충진재 존재하의 폴리디오가노실록산의 중합방법 - Google Patents
충진재 존재하의 폴리디오가노실록산의 중합방법 Download PDFInfo
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- KR840008385A KR840008385A KR1019840001283A KR840001283A KR840008385A KR 840008385 A KR840008385 A KR 840008385A KR 1019840001283 A KR1019840001283 A KR 1019840001283A KR 840001283 A KR840001283 A KR 840001283A KR 840008385 A KR840008385 A KR 840008385A
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- Prior art keywords
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- polydiorganosiloxane
- catalyst
- mixture
- weight
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- 238000000034 method Methods 0.000 title claims 14
- 239000000945 filler Substances 0.000 title claims 7
- 238000006116 polymerization reaction Methods 0.000 title claims 7
- -1 hydrocarbon radicals Chemical class 0.000 claims 10
- 239000003054 catalyst Substances 0.000 claims 9
- 239000000203 mixture Substances 0.000 claims 7
- 238000000354 decomposition reaction Methods 0.000 claims 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 4
- 125000004432 carbon atom Chemical group C* 0.000 claims 4
- 238000010438 heat treatment Methods 0.000 claims 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 4
- 125000005497 tetraalkylphosphonium group Chemical group 0.000 claims 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 4
- 229920002554 vinyl polymer Polymers 0.000 claims 4
- 239000004215 Carbon black (E152) Substances 0.000 claims 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 3
- 230000009849 deactivation Effects 0.000 claims 3
- 229930195733 hydrocarbon Natural products 0.000 claims 3
- 125000005496 phosphonium group Chemical group 0.000 claims 3
- 229920001296 polysiloxane Polymers 0.000 claims 3
- 150000004023 quaternary phosphonium compounds Chemical class 0.000 claims 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 2
- 125000001931 aliphatic group Chemical group 0.000 claims 2
- 229910052783 alkali metal Inorganic materials 0.000 claims 2
- 150000001340 alkali metals Chemical class 0.000 claims 2
- 150000007514 bases Chemical class 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 2
- 229910052697 platinum Inorganic materials 0.000 claims 2
- 229920005573 silicon-containing polymer Polymers 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 2
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 claims 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical group [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 claims 1
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims 1
- RMRFFCXPLWYOOY-UHFFFAOYSA-N allyl radical Chemical compound [CH2]C=C RMRFFCXPLWYOOY-UHFFFAOYSA-N 0.000 claims 1
- 125000004429 atom Chemical group 0.000 claims 1
- 238000009835 boiling Methods 0.000 claims 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical group BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims 1
- 229910052794 bromium Inorganic materials 0.000 claims 1
- 229910052793 cadmium Inorganic materials 0.000 claims 1
- 150000001661 cadmium Chemical class 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 125000001309 chloro group Chemical group Cl* 0.000 claims 1
- 239000008119 colloidal silica Substances 0.000 claims 1
- 238000006482 condensation reaction Methods 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 230000002779 inactivation Effects 0.000 claims 1
- 239000011630 iodine Chemical group 0.000 claims 1
- 229910052740 iodine Chemical group 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 229940049964 oleate Drugs 0.000 claims 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 1
- 229910052698 phosphorus Inorganic materials 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 claims 1
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 150000003254 radicals Chemical class 0.000 claims 1
- 239000012763 reinforcing filler Substances 0.000 claims 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 claims 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
내용 없음.
Description
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음
Claims (12)
- (A) 하기 일반식(I)의 폴리디오가노실록산 100중량부, 및 무기보강충진재 또는 무기중량충진재로 부터 선택된 충진재 1 내지 150중량부를 혼합시켜 혼합물을 제조하고; (B) 여기에, 언급된 폴리디오가노실록산의 축합반응을 야기시키에 충분한 양의 하기 일반식(II)의 촉매를 혼합시키고; (C) 혼합물을 촉매의 분해온도 이하로 가열하여 탈수시키고, 혼합물의 중합에 충분한 시간동안 습기를 제거시키고; (D) 이어서, 촉매를 비-활성화시켜, 생성된 실리콘 중합체의 분자량이 폴리디오가느실록산의 분자량보다 더 큰 안정한 실리콘 중합체-충진재 혼합물을 제조합을 특징으로 하여, 충진재의 존재하에 히드록실-말단폴리디오가노실록산을 중합하는 방법.상기식에서, R은 탄화수소라디칼, 할로겐화 탄화수소라디칼 또는 시아노알킬라디칼로부터 선택된 탄소수 1내지 18의 1가 라디칼이고, x는 3 내지 200이며, M은 알칼리금속, 테트라알킬포스포늄 또는 테트라알킬암모늄라디칼이고, Q는 알킬리금속, 테트라알킬포스포늄, 테트라알킬암모늄, 또는 수소라디칼이며, z는 1이상이다.
- 제1항에 있어서, 칼륨 디오가노실란올레이트가 촉매인 경우에 언급된 알칼리금속수산화물은 수산화칼륨이며, 비활성화단계(D)가 약산으로 중화시키는 것으로 이루어지는 중합방법.
- 제2항에 있어서, 언급된 촉매가, 하기일반식(III)의 4급 포스포늄 화합물, 하기 일반식(IV)의 염기상화합물, 및 염기성 화합물을 용해시키에 충분한 양이상의 물을, 디오가노실리콘 화합물 또는 저분자량 디오가노실록산과 혼합시키고, 탈수시켜 제조된 것인 중합방법:상기식에서, R'는 지방족불포화가 없는 탄소수 1 내지 18의 1가 탄화수소라디칼이고, X는 염소, 브롬 및 요드이며, M은 알칼리금속이다.
- 제1항이 있어서, 언급된 촉매가, 하기 일반식(V)의 4급 포스포늄학합물을 디오가노실리콘 화합물 또는 저분자량 디오가노실록산과 혼합시키고 탈수시켜 제조된 4급 포스포늄 디오가노실란올레이트인 중합방법.상기식에서, R'는 지방족 불포화가 없는 탄소수 1 내지 18의 1가 탄화수소라디칼이고, R″는 수소 또는 탄소수 1 내지 6의 알킬라디칼이다.
- 제3항이 있어서, 언급된 촉매가 테트라알킬포스포늄디오가노실란올레이트이 며, 언급된 비활성화단계 (D)가, 4급 포스포늄 화합물의 분해가 완결될 때까지 이의 분해온도 이상의 온도로 가열시키는 것으로 이루어지는 중합방법.
- 제4항에 있어서, 언급된 비횔성화 단계(D)가, 4급 포스포늄 디오가노실란올레이트의 분해가 완결될 때까지 이의 분해온도 이상의 온도로 가열시키는 것으로 이루어지는 중합방법.
- 제2항에 있어서, 언급된 캄륨 디오가노실란올레이트가, 폴리디오가노실록산중에 실리콘원자 1,000 내지 10,000개당 1개의 칼륨원자를 제공하기에 충분한 양으로 존재하는 중합방법.
- 제5항에 있어서, 언급된 테트라알킬포스프늄 디오가노실란올레이트가, 폴리디오가노실록산중에 실리콘원자 1,000 내지 10,000개당 1개의 인원자를 제공하기에 충분한 양으로 존재하는 중합방법.
- 제6항에 있어서, 언급된 4급 포스포늄 디오가노실란올레이트가, 폴리디오가노실록산중에 실리콘원자 1,000 내지 10,000개당 1개의 인원자를 제공하기에 충분한 양으로 존재하는 중합방법.
- 제9항에 있어서, (B) 단계전에서, (A)단계의 혼합물을 조절된 시스템내에서 l00℃ 내지 일반식 (I)의 폴리디오가노실록산의 비점미만의 온도로 가열시켜 물을 제거하는 중합방법.
- 제8항에 있어서, 언급된 테트라알킬포스포늄디오가노실란올레이트가, 폴리디오가노실록산중에 실리콘원자 1,000내지 5,000개당 1개의 인원자를 제공하기에 충분한 양으로 존재하는 테트라-n-부틸포스포늄 디메틸실란올레이트이고, 언급된 충진재는 1내지 40중량부의 콜로이드성 실리카이며, 단계(C)의 가열온도는 100℃내지 130℃이며, 언급된 촉매는 혼합물을 (D)단계에서 테트라-n-부틸포스포늄 디오가노신란올레이트의 분해에 충분한 시간동안 160°내지 200℃의 온도로 가열하므로써 비활성화시키는 중합방법.
- 제1항에 있어서, 분자당 2개 이상의 비닐 또는 알릴 라디칼을 함유하는 폴리디오가노실록산이 0.01 내지 2.0%의 비닐 또는 알릴라디칼을 가지며; 언급된 경화제가, 폴리디오가노실록산중에 비닐 또는 알릴라디칼 당 1개이상의 실리콘-결합된 수소원자를 제공하기에 충분한 양의 오가노하이드로겐실록산[이것은 분자당 평균 2개 이상의 실리콘-결합된 수소원자를 가지며, R″′HSiO, R″′2SiO, R″′2HSiO0.5, R″′2SiO0.5및 SiO2유니트(여기서, R″′는 메틸, 에틸, 비닐, 페닐, 3,3,3-트리플루오로프로필 또는 2-시아노에틸이다)로 이루어진다], 및 실리콘 중합체-충진재혼합물중에 실리콘중합체 1,000,000중량부당 1중량부 이상의 플라티늄을 제공하기에 충분한 양의 플라티늄 촉매로 이루어진 것인 중합방법.※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/474,919 US4433096A (en) | 1983-03-14 | 1983-03-14 | Polymerization of polydiorganosiloxane in the presence of filler |
US474,919 | 1983-03-14 |
Publications (2)
Publication Number | Publication Date |
---|---|
KR840008385A true KR840008385A (ko) | 1984-12-14 |
KR910008342B1 KR910008342B1 (ko) | 1991-10-12 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
KR1019840001283A KR910008342B1 (ko) | 1983-03-14 | 1984-03-14 | 충진재 존재하의 폴리디오가노실록산의 중합방법 |
Country Status (10)
Country | Link |
---|---|
US (1) | US4433096A (ko) |
EP (1) | EP0119093B1 (ko) |
JP (1) | JPS59176326A (ko) |
KR (1) | KR910008342B1 (ko) |
AU (1) | AU565080B2 (ko) |
BR (1) | BR8401140A (ko) |
CA (1) | CA1246275A (ko) |
DE (1) | DE3483485D1 (ko) |
NZ (1) | NZ207214A (ko) |
ZA (1) | ZA841242B (ko) |
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US2490357A (en) * | 1946-04-24 | 1949-12-06 | Corning Glass Works | Polymerization of siloxanes |
US2727876A (en) * | 1952-03-06 | 1955-12-20 | Du Pont | Composition and process |
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US3477988A (en) * | 1967-04-05 | 1969-11-11 | Union Carbide Corp | Preparation of organopolysiloxanes by siloxane rearrangement |
GB1220686A (en) * | 1967-05-26 | 1971-01-27 | Midland Silicones Ltd | Organopolysiloxane compositions |
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US4008261A (en) * | 1975-01-02 | 1977-02-15 | Dow Corning Corporation | Method of preparing phosphonium siloxanes and products thereof |
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US4268452A (en) * | 1980-03-10 | 1981-05-19 | Toray Silicone Company, Ltd. | Noncurable sealing materials |
-
1983
- 1983-03-14 US US06/474,919 patent/US4433096A/en not_active Expired - Lifetime
-
1984
- 1984-02-08 CA CA000447036A patent/CA1246275A/en not_active Expired
- 1984-02-20 NZ NZ207214A patent/NZ207214A/en unknown
- 1984-02-21 ZA ZA841242A patent/ZA841242B/xx unknown
- 1984-03-13 DE DE8484301687T patent/DE3483485D1/de not_active Expired - Fee Related
- 1984-03-13 BR BR8401140A patent/BR8401140A/pt not_active IP Right Cessation
- 1984-03-13 EP EP84301687A patent/EP0119093B1/en not_active Expired - Lifetime
- 1984-03-13 AU AU25566/84A patent/AU565080B2/en not_active Ceased
- 1984-03-14 KR KR1019840001283A patent/KR910008342B1/ko not_active IP Right Cessation
- 1984-03-14 JP JP59048948A patent/JPS59176326A/ja active Granted
Also Published As
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---|---|
JPS635418B2 (ko) | 1988-02-03 |
NZ207214A (en) | 1987-03-31 |
EP0119093A3 (en) | 1986-03-05 |
AU2556684A (en) | 1984-09-20 |
EP0119093B1 (en) | 1990-10-31 |
AU565080B2 (en) | 1987-09-03 |
DE3483485D1 (de) | 1990-12-06 |
EP0119093A2 (en) | 1984-09-19 |
KR910008342B1 (ko) | 1991-10-12 |
US4433096A (en) | 1984-02-21 |
CA1246275A (en) | 1988-12-06 |
JPS59176326A (ja) | 1984-10-05 |
BR8401140A (pt) | 1984-10-23 |
ZA841242B (en) | 1985-04-24 |
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