KR100660366B1 - 실리카 제조 방법, 특정 구멍-크기 및/또는 입자-크기분포를 가지는 실리카 및, 특히 강화 중합체에 있어서의이들의 용도 - Google Patents
실리카 제조 방법, 특정 구멍-크기 및/또는 입자-크기분포를 가지는 실리카 및, 특히 강화 중합체에 있어서의이들의 용도 Download PDFInfo
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- KR100660366B1 KR100660366B1 KR1020047002164A KR20047002164A KR100660366B1 KR 100660366 B1 KR100660366 B1 KR 100660366B1 KR 1020047002164 A KR1020047002164 A KR 1020047002164A KR 20047002164 A KR20047002164 A KR 20047002164A KR 100660366 B1 KR100660366 B1 KR 100660366B1
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Abstract
Description
Claims (58)
- 실리케이트와 산화제의 반응에 의해 실리카 현탁액을 수득한 후, 이 현탁액을 분리 및 건조시키는 것을 포함하는 유형의 실리카 제조 방법에 있어서, 실리케이트와 산화제의 반응을 하기의 연속 단계에 따라 수행하는 것을 특징으로 하는 방법:(ⅰ) pH 가 2 내지 5 인 저장 수용액 (aqueous stock) 을 형성하는 단계;(ⅱ) 반응 혼합물의 pH 를 2 내지 5 로 유지하는 방식으로, 상기 저장액에 실리케이트 및 산화제를 동시에 첨가하는 단계;(ⅲ) 산화제의 첨가를 중지시킨 반면, 7 내지 10 의 반응 혼합물의 pH 값을 수득할 때까지, 반응 혼합물에 실리케이트를 계속 첨가하는 단계;(ⅳ) 반응 혼합물의 pH 를 7 내지 10 으로 유지하는 방식으로, 반응 혼합물에 실리케이트 및 산화제를 동시에 첨가하는 단계; 및(ⅴ) 실리케이트의 첨가를 중지시킨 반면, 6 미만의 반응 혼합물의 pH 값을 수득할 때까지, 반응 혼합물에 산화제를 계속 첨가하는 단계.
- 제 1 항에 있어서, 숙성 단계를 단계 (ⅲ) 및 단계 (ⅳ) 사이에 수행하는 것을 특징으로 하는 방법.
- 제 1 항 또는 제 2 항에 있어서, 숙성 단계를 단계 (ⅴ) 후에 수행하는 것을 특징으로 하는 방법.
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- 제 1 항 또는 제 2 항에 있어서, 실리케이트와 산화제의 전체 반응을 70 내지 95℃ 에서 수행하는 것을 특징으로 하는 방법.
- 제 1 항 또는 제 2 항에 있어서, 실리케이트와 산화제의 전체 반응을 70 내지 95℃의 일정한 온도에서 수행하는 것을 특징으로 하는 방법.
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- 제 1 항 또는 제 2 항에 있어서, 스프레이 건조에 의해 건조를 수행하는 것을 특징으로 하는 방법.
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- 하기를 보유하는 것을 특징으로 하는 실리카:- 40 내지 525 ㎡/g 의 CTAB 비표면적 (SCTAB);- 45 내지 550 ㎡/g 의 BET 비표면적 (SBET);- 초음파 분해 후 XDC 입자 크기 분석에 의해 측정한, 0.91 이상의 물체 크기 분포 폭 Ld ((d84 - d16)/d50), 및- 비 V(d5 - d50)/V(d5 - d100) 이 0.66 이상인 구멍 부피 분포.
- 제 17 항에 있어서, 물체 크기 분포 폭 Ld 가 0.94 이상인 것을 특징으로 하는 실리카.
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- 제 17 항 또는 제 18 항에 있어서, 하기를 보유하는 것을 특징으로 하는 실리카:- 초음파 분해 후 XDC 입자 크기 분석에 의해 측정한, 1.04 이상의 물체 크기 분포 폭 Ld ((d84 - d16)/d50), 및- 비 V(d5 - d50)/V(d5 - d100) 이 0.71 이상인 구멍 부피 분포.
- 제 17 항 또는 제 18 항에 있어서, 파동 형태의 초음파 분해로 칭하는 시험에서 600 와트 (watt) 탐침의 100% 전력으로 측정한, α로 나타내는 분해 속도가 0.0035 ㎛-1ㆍ분-1 이상인 것을 특징으로 하는 실리카.
- 하기를 보유하는 것을 특징으로 하는 실리카:- 40 내지 525 ㎡/g 의 CTAB 비표면적 (SCTAB);- 45 내지 550 ㎡/g 의 BET 비표면적 (SBET); 및- 0.70 초과의 구멍 분포 폭 ldp.
- 제 24 항에 있어서, 초음파 분해 후 XDC 입자 크기 분석에 의해 측정한, 물체 크기 분포 폭 Ld ((d84 - d16)/d50) 가 0.91 이상인 것을 특징으로 하는 실리카.
- 제 24 항 또는 제 25 항에 있어서, 파동 형태의 초음파 분해로 칭하는 시험에서 600 와트 탐침의 100% 전력으로 측정한, α로 나타내는 분해 속도가 0.0035 ㎛-1ㆍ분-1 이상인 것을 특징으로 하는 실리카.
- 하기를 보유하는 것을 특징으로 하는 실리카:- 40 내지 525 ㎡/g 의 CTAB 비표면적 (SCTAB);- 45 내지 550 ㎡/g 의 BET 비표면적 (SBET);- 초음파 분해 후 XDC 입자 크기 분석에 의해 측정한, 0.95 이상의, 500 ㎚ 미만인 물체의 크기 분포 폭 L'd ((d84 - d16)/d50); 및- 비 V(d5 - d50)/V(d5 - d100) 이 0.71 이상인 구멍 부피 분포.
- 제 20 항에 있어서, 비 V(d5 - d50)/V(d5 - d100) 이 0.73 이상인 것을 특징으로 하는 실리카.
- 하기를 보유하는 것을 특징으로 하는 실리카:- 40 내지 525 ㎡/g 의 CTAB 비표면적 (SCTAB);- 45 내지 550 ㎡/g 의 BET 비표면적 (SBET);- 초음파 분해 후 XDC 입자 크기 분석에 의해 측정한, 0.90 이상의, 500 ㎚ 미만인 물체의 크기 분포 폭 L'd ((d84 - d16)/d50); 및- 비 V(d5 - d50)/V(d5 - d100) 이 0.74 이상인 구멍 부피 분포.
- 제 20 항에 있어서, 물체 크기 분포 폭 Ld 가 1.04 이상이고, 500 ㎚ 미만인 물체의 크기 분포 폭 L'd 가 0.95 이상인 것을 특징으로 하는 실리카.
- 제 29 항 또는 제 31 항에 있어서, 파동 형태의 초음파 분해로 칭하는 시험에서 600 와트 탐침의 100% 전력으로 측정한, α로 나타내는 분해 속도가 0.0035 ㎛-1ㆍ분-1 이상인 것을 특징으로 하는 실리카.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, (시어즈 (Sears) 수 ×1000) / (BET 비표면적 (SBET)) 비가 60 미만인 것을 특징으로 하는 실리카.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, 초음파 분해 후 XDC 입자 크기 분석에 의해 측정한 입자 크기 분포의 형태가 하기의 조건을 만족시키도록 하는 물체 크기를 가지는 것을 특징으로 하는 실리카: XDC 형태 (㎚) ≥ (5320 / SCTAB (㎡/g)) + 8.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, 직경이 3.7 내지 80 ㎚ 인 구멍에 의해 형성된 구멍 부피 (V80) 가 1.35 ㎤/g 이상인 것을 특징으로 하는 실리카.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, 하기를 보유하는 것을 특징으로 하는 실리카:- 60 내지 330 ㎡/g 의 CTAB 비표면적 (SCTAB);- 70 내지 350 ㎡/g 의 BET 비표면적 (SBET).
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, CTAB 비표면적 (SCTAB) 이 90 내지 230 ㎡/g 인 것을 특징으로 하는 실리카.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, BET 비표면적 (SBET) 이 110 내지 270 ㎡/g 인 것을 특징으로 하는 실리카.
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- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, 평균 크기가 80 ㎛ 이상인, 거의 구형 비드 (bead) 의 형태인 것을 특징으로 하는 실리카.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, 평균 크기가 15 ㎛ 이상인 분말 형태인 것을 특징으로 하는 실리카.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 있어서, 평균 크기가 1 ㎜ 이상인 과립 형태인 것을 특징으로 하는 실리카.
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- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항의 실리카를 중합체용 강화 필러로서 사용하는 방법.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 따른 실리카를 천연 고무 조성물 중 강화 필러로서 사용하는 방법.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 따른 실리카를 구두 밑창에서의 강화 필러로서 사용하는 방법.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 따른 실리카를 고성능 부품용 중합체 조성물 중 강화 필러로서 사용하는 방법.
- 제 17 항, 제 24 항, 제 29 항 또는 제 31 항 중 어느 한 항에 따른 실리카를 촉매 지지체로서, 활성 물질용 흡수제로서, 점도-개질, 질감조절 또는 굳기방지제로서, 전지 격리판용 성분으로서, 또는 덴트리피스용 또는 종이용 첨가제로서 사용하는 방법.
- 제 55 항에 있어서, 커플링제인 모노에톡시디메틸실릴프로필 테트라술피드의 존재 하에서 이루어지는 방법.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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FR01/11001 | 2001-08-13 | ||
FR0111001 | 2001-08-13 | ||
PCT/FR2002/002872 WO2003016215A1 (fr) | 2001-08-13 | 2002-08-13 | Procede de preparation de silices, silices a distribution granulometrique et/ou repartition poreuse particulieres et leurs utilisations, notamment pour le renforcement de polymeres |
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KR20040030070A KR20040030070A (ko) | 2004-04-08 |
KR100660366B1 true KR100660366B1 (ko) | 2006-12-21 |
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KR1020047002164A KR100660366B1 (ko) | 2001-08-13 | 2002-08-13 | 실리카 제조 방법, 특정 구멍-크기 및/또는 입자-크기분포를 가지는 실리카 및, 특히 강화 중합체에 있어서의이들의 용도 |
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US (3) | US20050032965A1 (ko) |
EP (3) | EP1419106B1 (ko) |
JP (1) | JP4515761B2 (ko) |
KR (1) | KR100660366B1 (ko) |
CN (2) | CN100430317C (ko) |
AU (1) | AU2002341047B8 (ko) |
BR (1) | BR0211703B1 (ko) |
CA (2) | CA2729228C (ko) |
DK (1) | DK1419106T3 (ko) |
ES (1) | ES2610590T3 (ko) |
MX (1) | MXPA04001133A (ko) |
PT (1) | PT1419106T (ko) |
RU (1) | RU2270167C2 (ko) |
TW (1) | TWI247725B (ko) |
WO (1) | WO2003016215A1 (ko) |
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US20240158615A1 (en) | 2022-11-02 | 2024-05-16 | The Goodyear Tire & Rubber Company | Precipitated silica pretreated with a coupling agent and polyethylene glycol for a rubber composition |
WO2024104971A1 (en) | 2022-11-14 | 2024-05-23 | Rhodia Operations | Modified precipitated silica, its manufacture and use |
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CN1016911B (zh) * | 1990-10-22 | 1992-06-03 | 同济大学 | 高介电常数低介电损耗膜 |
FR2678259B1 (fr) * | 1991-06-26 | 1993-11-05 | Rhone Poulenc Chimie | Nouvelles silices precipitees sous forme de granules ou de poudres, procedes de synthese et utilisation au renforcement des elastomeres. |
EP0670813B1 (fr) * | 1993-09-29 | 2003-03-12 | Rhodia Chimie | Silice precipitee |
FR2732328B1 (fr) * | 1995-03-29 | 1997-06-20 | Rhone Poulenc Chimie | Nouveau procede de preparation de silice precipitee, nouvelles silices precipitees contenant de l'aluminium et leur utilisation au renforcement des elastomeres |
IN188702B (ko) * | 1995-06-01 | 2002-10-26 | Degussa | |
FR2749576B1 (fr) * | 1996-06-06 | 1998-09-04 | Rhone Poulenc Chimie | Procede de preparation de silice susceptible d'etre utilisee dans les compositions dentifrices |
FR2763581B1 (fr) * | 1997-05-26 | 1999-07-23 | Rhodia Chimie Sa | Silice precipitee utilisable comme charge renforcante pour elastomeres |
DE19740440A1 (de) * | 1997-09-15 | 1999-03-18 | Degussa | Leicht dispergierbare Fällungskieselsäure |
EP1034135B1 (fr) | 1997-11-28 | 2005-11-16 | Compagnie Générale des Etablissements MICHELIN-MICHELIN & CIE | Charge alumineuse renforcante et composition de caoutchouc comportant une telle charge |
JP2001525436A (ja) | 1997-11-28 | 2001-12-11 | コンパニー ゼネラール デ エタブリッスマン ミシュラン−ミシュラン エ コムパニー | アルミナ層で被覆されたカーボンブラックで補強したタイヤ用ゴム組成物 |
EP1114093B1 (fr) | 1999-05-28 | 2004-10-13 | Société de Technologie Michelin | Composition de caoutchouc pour pneumatique, a base d'elastomere dienique et d'un oxyde de titane renfor ant |
JP5022548B2 (ja) | 1999-05-28 | 2012-09-12 | ソシエテ ド テクノロジー ミシュラン | ジエンエラストマー及び強化酸化チタンに基づくタイヤ用ゴム組成物 |
HUP0204138A3 (en) * | 1999-07-28 | 2004-08-30 | Grace Gmbh & Co Kg | Preciptated silica, a process to make it, and its use |
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- 2002-08-13 US US10/486,573 patent/US20050032965A1/en not_active Abandoned
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR101426175B1 (ko) * | 2009-09-03 | 2014-08-01 | 로디아 오퍼레이션스 | 침강 실리카의 신규 제조 방법 |
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