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Method for preparing methyl phenyl ring siloxane mixture

A technology of methylphenyl cyclosiloxane and methylphenyl dialkoxysilane is applied in the field of preparation of methyl phenyl cyclosiloxane mixture, and can solve the problem of not providing methyl phenyl mixed ring body preparation methods, etc., to achieve the effects of high utilization of silicon atoms, energy saving, and saving of washing water.

Inactive Publication Date: 2009-08-12
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] The above-mentioned literature reports that organosilicon polymer materials containing methylphenylsiloxane chain members can be prepared from methylphenyldiethoxysilane, but does not provide a preparation method for methylphenyl mixed rings

Method used

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  • Method for preparing methyl phenyl ring siloxane mixture

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 521.8g of methylphenyldiethoxysilane with a purity greater than 99.8wt% and no trifunctional impurities, 5.2144g of LiOH·H 2 0 and 684g deionized water are added in the three-neck round-bottomed flask of 2000mL with mechanical stirring, temperature control sensor and packing separation column, the port on the packing separation column is connected with the distillation head, by adjusting the valve position on the distillation head discharge pipeline , the reflux ratio of the top material can be adjusted. Raise the temperature of the above-mentioned reaction mixture through an electric heating jacket, make methylphenyldiethoxysilane undergo hydrolysis and condensation reaction between 80~100°C, adjust the valve position on the discharge pipeline of the distillation head, and slowly receive the ethanol produced by the reaction- water mixture. After reacting for 6 hours, 633.5 g of ethanol-water mixture was received, and the refractive index of the overhead distillate was...

Embodiment 2

[0044]500g purity is greater than 99.8wt% and does not contain the methylphenyldiethoxysilane of trifunctionality impurity, the 208.6g alkaline aqueous solution and the 420g deionized water collected in the hydrolyzate oil-water separation process of embodiment 1 are added to In the 2000mL three-neck round bottom flask with mechanical stirring, temperature control sensor and packing separation column, the upper port of the packing separation column is connected to the distillation head, and the reflux ratio of the top material can be adjusted by adjusting the valve position on the discharge pipeline of the distillation head. Raise the temperature of the above-mentioned reaction mixture through an electric heating jacket, make methylphenyldiethoxysilane undergo hydrolysis and condensation reaction between 80~100°C, adjust the valve position on the discharge pipeline of the distillation head, and slowly receive the ethanol produced by the reaction- water mixture. After reacting ...

Embodiment 3 and Embodiment 4

[0047] Except changing the kind and consumption of hydrolysis condensation catalyst, cracking catalyst, temperature of reaction and the reaction time, all the other conditions are with embodiment 1, carry out experiment according to the procedure identical with embodiment 1, gained result is shown in the table below.

[0048] The following table is embodiment 3 and 4 raw material proportioning, reaction conditions and reaction result

[0049]

[0050] By the same method as in Example 1, the methylphenyl mixed ring body prepared in Example 4 is used to replace the methylphenyl mixed ring body in Example 1 to prepare methylphenylethylene with a phenyl molar fraction of 20%. Base raw rubber, analyzed by GPC, relative to polystyrene, its molecular weight is 5.79×10 5 g / mol; Take 2g of methyl phenyl vinyl raw rubber sample, put it in 25mL of toluene solution, stir at room temperature, after 1h, the sample is completely dissolved in toluene.

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Abstract

The invention discloses a preparation method of a methyl phenyl cyclosiloxane mixture, in particular a preparation method of a methyl phenyl cyclosiloxane mixture which does not contain trifunctional impurity. In the invention, methyl phenyl dialkoxy silane and a catalyst react; when a refraction index nD of a received alcohol-water mixture generated by the reaction is close to 1.3325, the reaction is stopped; standing and layering are carried out; and then, cracking reaction is carried out on an oil layer and the catalyst so as to obtain the target product. The invention has the advantages of simple production process, washing water saving, low cracking temperature and energy saving. A mixed ring body can be used as a basic polymer for a methyl phenyl high-temperature glue which has high phenyl content, high viscosity, high molecular weight, no cross binding and flat gravitational flow. The methyl phenyl mixed ring body can also be used for preparing high-temperature resistant and radiation resistant materials needed by high-temperature organosilicone heat-conducting silicon oil and a nuclear power facility and also be used for preparing power-type LED organosilicone sealing materials.

Description

technical field [0001] The invention relates to a preparation method of a methylphenyl cyclosiloxane mixture, in particular to a preparation method of a methylphenyl cyclosiloxane mixture free of trifunctional impurities. Background technique [0002] Methylphenylcyclosiloxane mixture is composed of methylphenylcyclotrisiloxane, methylphenylcyclotetrasiloxane, methylphenylcyclopentasiloxane and other homologues and their isomers For example, methylphenylcyclotrisiloxane has two cis and trans geometric isomers, and methylphenylcyclotetrasiloxane has one cis and three trans geometric isomers There are four geometric isomers in methylphenyl cyclopentasiloxane. [0003] Methylphenyl cyclosiloxane mixture (referred to as methylphenyl mixed ring, the same below) is an important raw material in the silicone industry, and is widely used in the synthesis of methylphenyl silicone oil and methylphenyl silicone resin And methyl phenyl silicone rubber raw rubber, so as to endow the mat...

Claims

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Application Information

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IPC IPC(8): C07F7/21B01J27/02B01J23/04
Inventor 伍川杨雄发董红金晶胡从达徐晓秋彭家建蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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