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A kind of environment-friendly preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane

A technology of tetravinyltetramethylcyclotetrasiloxane and pentamethylcyclotrisiloxane, which is applied in the field of synthesis of organosilicon compounds to achieve the effects of high efficiency, inhibition of formation, and improvement of ring-forming selectivity

Active Publication Date: 2019-03-15
新元化学(山东)股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention solves the environmental protection problems caused by the use of chlorosilanes in the prior art and avoids the use of chlorosilanes; on the other hand, the present invention improves the yield and selectivity of products through process control and the effect of auxiliary catalysts; at the same time, the present invention It also has the advantages of low cost, simple operation, high efficiency, and good safety.

Method used

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  • A kind of environment-friendly preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane
  • A kind of environment-friendly preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment 1, a kind of preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane comprises steps:

[0045] (1) In a 2L four-necked flask equipped with mechanical stirring, a constant pressure dropping funnel, a thermometer and a distillation tower, add 592g (2mol) of octamethylcyclotetrasiloxane (D 4 ) and 344g (1mol) tetravinyltetramethylcyclotetrasiloxane (D 4 Vi ), mix evenly, then add 4.68g of solid potassium hydroxide and 56.16g of triphenylphosphine to it, and stir to form a suspension; turn on the heating, slowly heat up, and the material in the kettle gradually becomes viscous, accompanied by white solid suspension When the temperature rises to 95-100°C, the system gradually changes from viscous to thin, and a sufficient pre-cracking reaction is carried out, and the reaction time is 1.5h; then,

[0046] (2) Add 4.68g of solid potassium hydroxide to the kettle, raise the temperature to 145°C, and carry out co-cleavage reaction, the reaction time is 0...

Embodiment 2

[0054] Embodiment 2, a kind of preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane, comprising steps:

[0055] (1) Add 592g (2mol) octamethylcyclotetrasiloxane (D 4 ) and 344g (1mol) tetravinyltetramethylcyclotetrasiloxane (D 4 Vi ), mix evenly, then add 4.68g of solid potassium hydroxide and 74.88g of triphenylphosphine to it, and stir to form a suspension; turn on the heating, slowly heat up, and the material in the kettle gradually becomes viscous, accompanied by white solid suspension When the temperature rises to 100°C, the system gradually changes from viscous to thin, and it is maintained for 1-2 hours to carry out a sufficient pre-cracking reaction; then,

[0056] (2) Add 5.62g of solid potassium hydroxide to the kettle, raise the temperature to 143-147°C, maintain for 40min, and carry out co-cleavage reaction;

[0057] (3) Adopt a water jet vacuum pump to change the system from a normal pressure state to a negative pressure state, and keep the press...

Embodiment 3

[0063] Embodiment 3, a kind of preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane, comprising steps:

[0064] (1) Add 592g (2mol) octamethylcyclotetrasiloxane (D 4 ) and 344g (1mol) tetravinyltetramethylcyclotetrasiloxane (D 4 Vi ), mix evenly, then add 5.62g of solid potassium hydroxide and 84.24g of triphenylphosphine to it, and stir to form a suspension; turn on the heating, slowly heat up, and the material in the kettle gradually becomes viscous, accompanied by white solid suspension When the temperature rises to 90-110°C, the system gradually changes from viscous to thin, and maintains for 1-2h to carry out a sufficient pre-cracking reaction; then,

[0065] (2) Add 5.62g of solid potassium hydroxide to the kettle, raise the temperature to 140-150°C, maintain for 0.5h, and carry out co-cleavage reaction;

[0066] (3) Adopt water jet vacuum pump, system is changed into negative pressure state by normal pressure state, pressure maintains-0.092MPa continue...

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Abstract

The invention relates to an environment-friendly preparation method of 2-vinyl-2, 4, 4, 6, 6-pentamethyl cyclotrisiloxane. The method includes: carrying out precracking reaction on octamethylcyclotetrasiloxane (D4) and tetravinyl tetramethylcyclotetrasiloxane (D4<Vi>) in a mole ratio of 2:1 in the presence of a co-cracking catalyst and an auxiliary catalyst; then replenishing the co-cracking catalyst and carrying out co-cracking reaction at 140-150DEG C; changing the ordinary pressure into negative pressure, and collecting co-cracking fraction, adding D4 and D4<Vi> dropwise simultaneously while recovering the fraction, and maintaining the total drop adding amount equal to the total recovery amount; and aggregating the fraction and performing rectification, thus obtaining the target product. The method provided by the invention improves the yield and selectivity of cyclotrisiloxane, inhibits the generation of cyclotetrasiloxane, also avoids implosion and crosslinking of the reaction raw materials, and has the characteristics of simple operation, low cost, high efficiency, environmental protection and safety, etc.

Description

technical field [0001] The invention relates to an environment-friendly preparation method of 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane, which belongs to the field of synthesis of organosilicon compounds. Background technique [0002] Cyclosiloxane is a very important intermediate raw material in the silicone industry, and is widely used in the synthesis of silicone oil, silicone resin and silicone rubber. The organosilicon material prepared with it has excellent electrical properties, physiological inertness, corrosion resistance, high and low temperature resistance, aging resistance and other properties, which are incomparable and replaceable by other organic polymer materials. It has been widely used in ships, light industry textiles, construction, machinery, medicine, transportation, etc., and has increasingly become an important and indispensable new polymer material in the national economy. [0003] 2-vinyl-2,4,4,6,6-pentamethylcyclotrisiloxane is a special organo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 解乐福于鹏飞王天宇侯志伟夏子祥于佳平
Owner 新元化学(山东)股份有限公司
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