Synthesis method of alkoxy-terminated polysiloxane and alkoxy-terminated polysiloxane
阅读说明：本技术 烷氧基封端聚硅氧烷的合成方法及烷氧基封端聚硅氧烷 (Synthesis method of alkoxy-terminated polysiloxane and alkoxy-terminated polysiloxane ) 是由 冯伦武 李胜杰 王成 冯琼华 肖俊平 于 2019-11-29 设计创作，主要内容包括：本发明公开了一种烷氧基封端聚硅氧烷的合成方法及烷氧基封端聚硅氧烷,涉及有机硅材料技术领域,本发明采用乙烯基硅油和烷氧基氢硅烷为原料,加入铂催化剂,温度60～120℃条件下,反应一段时间,制得烷氧基封端聚硅氧烷。该方案原料易得,反应过程中操作简单,反应条件较温和,对设备没有太高要求,无废液、废料产生,便于产业化。得到的产品烷氧基封端聚硅氧烷,无色透明,粘度稳定,适于制备各种储存期限与固化操作时间较长的室温硫化硅橡胶。(The invention discloses a synthesis method of alkoxy-terminated polysiloxane and the alkoxy-terminated polysiloxane, and relates to the technical field of organic silicon materials. The method has the advantages of easily obtained raw materials, simple operation in the reaction process, mild reaction conditions, no high requirement on equipment, no waste liquid and waste material generation and convenient industrialization. The obtained product alkoxy-terminated polysiloxane is colorless and transparent, has stable viscosity, and is suitable for preparing room temperature vulcanized silicone rubber with various storage lives and longer curing operation time.)
1. A method for synthesizing alkoxy-terminated polysiloxane, which is characterized by comprising the following steps:
taking 100 parts by mass of vinyl silicone oil and 1-4 parts by mass of alkoxy hydrogen silane as raw materials, adding 0.01-0.5 part by mass of platinum catalyst, and reacting at the temperature of 60-120 ℃ for 100-200 min;
after the reaction is finished, heating and pumping negative pressure to remove excessive alkoxy silane, wherein the temperature is 110-130 ℃ to prepare alkoxy terminated polysiloxane.
2. The method of claim 1, wherein: the viscosity of the vinyl silicone oil is 2000-80000 mPa.s.
3. The method of claim 1, wherein: the amount of the alkoxysilane to be used is preferably 4 parts by mass.
4. The method of claim 1, wherein: the platinum catalyst is isopropanol solution of chloroplatinic acid.
5. The method of claim 4, wherein: the amount of the isopropyl alcohol solution of chloroplatinic acid is preferably 0.4 part by mass.
6. The method of claim 1, wherein: the reaction temperature is preferably 80 ℃.
7. An alkoxy-terminated polysiloxane characterized by: the alkoxy end-capped polysiloxane comprises the following raw materials in parts by mass:
100 parts by mass of a vinyl silicone oil;
1 to 4 parts by mass of an alkoxy hydrosilane;
0.01 to 0.5 parts by mass of a platinum catalyst.
8. An alkoxy-terminated polysiloxane according to claim 7, wherein: the alkoxy-terminated polysiloxane is of the formula:
(CH3O)3SiCH2CH2Si(CH3)2O[(CH3)2SiO]n(CH3)2SiCH2CH2Si(OCH3)3。
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to a synthetic method of alkoxy-terminated polysiloxane and the alkoxy-terminated polysiloxane.
Background
The organosilicon room temperature vulcanized silica gel has been rapidly developed in recent decades due to its excellent properties, and has been widely applied to various fields of national economy. Among them, it has the advantages of convenient operation, no viscosity peak, no heat release in the curing process, excellent ageing resistance, energy saving and environmental protection, etc., and its development is very rapid.
A commonly used alkoxy-terminated polysiloxane resin synthesis method is to use hydroxyl-terminated polysiloxane and alkoxy silane as raw materials to synthesize alkoxy-terminated 107 resin by using organic tin or amine catalysts and the like, and the synthesized resin has unstable resin storage due to the factors of catalyst residues for catalyzing alkoxy hydrolysis and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for synthesizing alkoxy-terminated polysiloxane and alkoxy-terminated polysiloxane, which solve the problem that the resin synthesized by the prior method is unstable in storage due to the factors such as catalyst residue and the like.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows: a method of synthesizing an alkoxy-terminated polysiloxane comprising the steps of:
taking 100 parts by mass of vinyl silicone oil and 1-4 parts by mass of alkoxy hydrogen silane as raw materials, adding 0.01-0.5 part by mass of platinum catalyst, and reacting at the temperature of 60-120 ℃ for 100-200 min;
after the reaction is finished, heating and pumping negative pressure to remove excessive alkoxy silane, wherein the temperature is 110-130 ℃ to prepare alkoxy terminated polysiloxane.
On the basis of the technical scheme, the viscosity of the vinyl silicone oil is 2000-80000 mPa.s.
Based on the above technical solution, the amount of the alkoxysilane to be used is preferably 4 parts by mass.
On the basis of the technical scheme, the platinum catalyst is an isopropanol solution of chloroplatinic acid.
Based on the above technical solution, the amount of the isopropyl alcohol solution of chloroplatinic acid is preferably 0.4 parts by mass.
On the basis of the technical scheme, the reaction temperature is preferably 80 ℃.
The invention also provides alkoxy-terminated polysiloxane, which comprises the following raw materials in parts by weight:
100 parts by mass of a vinyl silicone oil;
1 to 4 parts by mass of an alkoxy hydrosilane;
0.01 to 0.5 parts by mass of a platinum catalyst.
On the basis of the technical scheme, the chemical formula of the alkoxy-terminated polysiloxane is as follows:
(CH3O)3SiCH2CH2Si(CH3)2O[(CH3)2SiO]n(CH3)2SiCH2CH2Si(OCH3)3。
compared with the prior art, the invention has the advantages that:
the synthesis method of the alkoxy-terminated polysiloxane provided by the invention has the advantages of easily available raw materials, simple operation in the reaction process, mild reaction conditions, no high requirement on equipment, no waste liquid and waste material generation, and convenience for industrialization. The obtained product alkoxy-terminated polysiloxane is colorless and transparent, has stable viscosity, and is suitable for preparing room temperature vulcanized silicone rubber with various storage lives and longer curing operation time.
The alkoxy-terminated polysiloxane prepared by the scheme solves the problems of high viscosity peak and storage stability, and the correspondingly obtained silica gel has excellent high-temperature and high-humidity resistance, and particularly the silicon rubber of the alkoxy-terminated polysiloxane has excellent thixotropy.
Detailed Description
The embodiment of the invention provides a method for synthesizing alkoxy-terminated polysiloxane, which comprises the following steps:
taking 100 parts by mass of vinyl silicone oil and 1-4 parts by mass of alkoxy hydrogen silane as raw materials, adding 0.01-0.5 part by mass of platinum catalyst, and reacting at the temperature of 60-120 ℃ for 100-200 min;
after the reaction is finished, heating and pumping negative pressure to remove excessive alkoxy silane, wherein the temperature is 110-130 ℃ to prepare alkoxy terminated polysiloxane.
The chemical reaction equation is as follows:
CH2＝CH-Si(CH3)2O[(CH3)2SiO]n(CH3)2Si-CH＝CH2+HSi(OCH3)3→(CH3O)3SiCH2CH2Si(CH3)2O[(CH3)2SiO]n(CH3)2SiCH2CH2Si(OCH3)3。
the viscosity of the vinyl silicone oil is 2000-80000 mPa.s.
The platinum catalyst is isopropanol solution of chloroplatinic acid.
The reaction temperature is preferably 80 ℃.
The embodiment of the invention also provides alkoxy-terminated polysiloxane, which comprises the following raw materials in parts by weight:
100 parts by mass of a vinyl silicone oil;
1 to 4 parts by mass of an alkoxy hydrosilane;
0.01 to 0.5 parts by mass of a platinum catalyst.
The alkoxy-terminated polysiloxane is of the formula:
(CH3O)3SiCH2CH2Si(CH3)2O[(CH3)2SiO]n(CH3)2SiCH2CH2Si(OCH3)3。
the present invention will be described in further detail with reference to examples.
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