WO2019075851A1 - Procédé de mélange d'un caoutchouc de silicone liquide à l'aide de la polymérisation in situ - Google Patents

Procédé de mélange d'un caoutchouc de silicone liquide à l'aide de la polymérisation in situ Download PDF

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Publication number
WO2019075851A1
WO2019075851A1 PCT/CN2017/112846 CN2017112846W WO2019075851A1 WO 2019075851 A1 WO2019075851 A1 WO 2019075851A1 CN 2017112846 W CN2017112846 W CN 2017112846W WO 2019075851 A1 WO2019075851 A1 WO 2019075851A1
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WO
WIPO (PCT)
Prior art keywords
silicone rubber
silicate
polysiloxane
sio
temperature
Prior art date
Application number
PCT/CN2017/112846
Other languages
English (en)
Chinese (zh)
Inventor
谢朝辉
黄胜
杨家昌
张再成
吴长林
Original Assignee
惠州赛力珑新材料有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
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Application filed by 惠州赛力珑新材料有限公司 filed Critical 惠州赛力珑新材料有限公司
Publication of WO2019075851A1 publication Critical patent/WO2019075851A1/fr

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    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

Definitions

  • the invention relates to the technical field of liquid silicone rubber preparation, and in particular to a method for in-situ polymerization of liquid silicone rubber.
  • Silicone oil generally refers to linear polysiloxanes that remain liquid at room temperature.
  • silicone oil it is usually necessary to add silica to silicone oil and organically use silica with silazane.
  • the treatment improves the degree of dispersion of silica and silicone oil.
  • the specific surface area of silica is large and easy to agglomerate, it is still difficult to uniformly disperse in the silicone oil, and the dispersion of silica in the silicone oil will eventually affect. Mechanical properties of finished silicone rubber.
  • the present invention provides a method of in-situ polymerization of liquid silicone rubber.
  • the invention discloses a method for in situ polymerization and refining liquid silicone rubber, comprising the following steps:
  • the vacuum was applied and the temperature was raised to 120 to 150 ° C to remove low molecules, thereby preparing a liquid silicone rubber.
  • the silicate is methyl orthosilicate, orthosilicate or tetraethyl orthosilicate prepolymer.
  • the polysiloxane is a linear polysiloxane having a vinyl group at both ends or a side chain, and has a viscosity of 1,000 to 100,000 cSt.
  • SiO 2 mass fraction of the polysiloxane accounts according to an embodiment of the present invention, the introduction of silicate is 10 to 40%.
  • the silicone modifier is a silane coupling agent or a silazane
  • the mass of the silicone modifier is 15 to 50 of the mass of the SiO 2 introduced by the silicate. %.
  • the present invention can obtain the following technical effects:
  • the in-situ polymerization method for refining a liquid silicone rubber of the present application is obtained by uniformly dispersing and mixing a silicate having good compatibility with a silicone oil, and then performing hydrolysis, polycondensation and organication of the silicate, and uniformly dispersed by the silicone oil.
  • the method for refining liquid silicone rubber is to firstly mix silicate with polysiloxane, add water and silicone modifier, and generate SiO 2 by silicate hydrolysis to make SiO 2 and polysiloxane.
  • the alkane is uniformly dispersed, and the introduced SiO 2 accounts for 10 to 40% by mass of the polysiloxane.
  • the mechanical properties of the polysiloxane can be improved by appropriately introducing SiO 2 as a reinforcing agent and uniformly dispersing with the polysiloxane.
  • SiO 2 an organic agent to generate a silicone-modified SiO 2 SiO 2 while the organic modification, SiO 2 to improve the compatibility with the polysiloxane.
  • the quality of the added silicone modifier accounts for 15 to 50% of the mass of the SiO 2 produced by the hydrolysis of the silicate, and the compatibility of the SiO 2 and the polysiloxane is controlled by controlling the content of the silicone modifier to prevent the compatibility of the silicone modifier. If the degree of SiO 2 is too high or too low, the degree of organicization will affect the reinforcing effect, and the degree of organication will be too low, resulting in poor compatibility between SiO 2 and polysiloxane, resulting in a large viscosity.
  • the liquid silicone rubber compound will be refined in three embodiments below.
  • a silica gel compound will be produced by three comparative examples in accordance with the existing production methods mentioned in the background art.
  • the rubber materials prepared by the above three examples and the three comparative examples were vulcanized according to the same formula to prepare an added silicone rubber, and the viscosity of the added silicone rubber was measured and pressed into a film of the same size, and tested by a tensile tester.
  • the mechanical properties of the film were obtained as shown in Table 1 below.
  • the silicone rubber compound prepared in the three examples and the silica gel compound prepared in the three comparative examples were used to prepare the addition type silicone rubber, and the silicone rubber obtained by the method of the present application was prepared.
  • the mechanical properties of the compound are better.

Landscapes

  • 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

La présente invention concerne un procédé de mélange d'un caoutchouc de silicone liquide à l'aide de la polymérisation in situ. Le procédé de mélange d'un caoutchouc de silicone liquide à l'aide de la polymérisation in situ de la présente invention concerne la dispersion et le mélange uniformément d'un silicate ester qui présente une bonne compatibilité avec l'huile de silicone, puis la soumission du silicate ester à l'hydrolyse, la polycondensation et un traitement organique pour produire du SiO2 par hydrolyse du silicate ester, qui a été uniformément dispersé avec l'huile de silicone, de sorte que le SiO2 est uniformément dispersé dans l'huile de silicone, et également l'amélioration de la compatibilité du SiO2 avec l'huile de silicone par modification organique du SiO2, qui facilite l'amélioration des propriétés mécaniques du caoutchouc de silicone.
PCT/CN2017/112846 2017-10-16 2017-11-24 Procédé de mélange d'un caoutchouc de silicone liquide à l'aide de la polymérisation in situ WO2019075851A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201710959325.6 2017-10-16
CN201710959325.6A CN107698983A (zh) 2017-10-16 2017-10-16 一种原位聚合炼制液体硅橡胶的方法

Publications (1)

Publication Number Publication Date
WO2019075851A1 true WO2019075851A1 (fr) 2019-04-25

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Application Number Title Priority Date Filing Date
PCT/CN2017/112846 WO2019075851A1 (fr) 2017-10-16 2017-11-24 Procédé de mélange d'un caoutchouc de silicone liquide à l'aide de la polymérisation in situ

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Country Link
CN (1) CN107698983A (fr)
WO (1) WO2019075851A1 (fr)

Families Citing this family (1)

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Publication number Priority date Publication date Assignee Title
CN110670382B (zh) * 2019-09-28 2022-01-11 桐乡市鑫隆印染有限公司 一种厚型涤纶纺织品柔性化无水印染的方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1130053A2 (fr) * 2000-03-03 2001-09-05 The Goodyear Tire & Rubber Company Préparation d'un elastomère renforcé, composition elastomère et pneu comprenant cette composition
CN101165080A (zh) * 2006-10-16 2008-04-23 中国科学院化学研究所 用溶胶-凝胶法增强的室温硫化硅橡胶的方法
CN101796058A (zh) * 2007-07-13 2010-08-04 莫门蒂夫性能材料股份有限公司 使用官能化二氧化硅的可固化和固化的硅橡胶组合物及其制备方法

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CN100489036C (zh) * 2007-01-25 2009-05-20 四川大学 用于制备高强度透明室温固化硅橡胶的填充胶
JP5510148B2 (ja) * 2010-07-23 2014-06-04 信越化学工業株式会社 ミラブル型シリコーンゴム組成物の製造方法
CN102942721B (zh) * 2012-10-26 2014-10-15 武汉工程大学 纳米白炭黑增强丁苯橡胶复合材料的制备工艺

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1130053A2 (fr) * 2000-03-03 2001-09-05 The Goodyear Tire & Rubber Company Préparation d'un elastomère renforcé, composition elastomère et pneu comprenant cette composition
CN101165080A (zh) * 2006-10-16 2008-04-23 中国科学院化学研究所 用溶胶-凝胶法增强的室温硫化硅橡胶的方法
CN101796058A (zh) * 2007-07-13 2010-08-04 莫门蒂夫性能材料股份有限公司 使用官能化二氧化硅的可固化和固化的硅橡胶组合物及其制备方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DUAN, XIANJIAN ET AL.: "In-Situ Silica Reinforcing Rubber by Sol - Gel Method", CHINA SYNTHETIC RUBBER INDUSTRY, vol. 23, no. 3, 15 May 2000 (2000-05-15), pages 148 - 152, XP055594564, ISSN: 1000-1255 *
NING, YINGPEI: "Reinforcement Effect of Organic Siloxanes on the Silicon Networks", JOURNAL OF QINGDAO INSTITUTE OF CHEMICAL TECHNOLOGY, vol. 10, no. 2, 2 July 1989 (1989-07-02), pages 9 - 11, ISSN: 1672-6987 *

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