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Method for preparing hydroxyl silicone oil by taking sodium acetate as acylating agent

A technology of hydroxy silicone oil and sodium acetate, applied in the field of preparing hydroxy silicone oil, can solve the problems of high cost, difficult market capacity sales, environmental pollution and the like

Inactive Publication Date: 2012-06-06
溧阳巨神科技材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN1821284A discloses a preparation method for synthesizing small molecule hydroxy silicone oil with potassium hydroxide. The hydroxy silicone oil siloxane chain link produced by this method is suitable as a silicone rubber structure control agent, but due to the need to consume a large amount of potassium hydroxide and Sulfuric acid (for neutralization), not only the cost is high, but also the discharged wastewater is difficult to treat
But this method can by-produce a large amount of sodium acetate (water liquid), though it can evaporate and crystallize into sodium acetate trihydrate or anhydrous sodium acetate, it is very difficult to sell because of the limited market capacity; and discharge will cause environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a four-necked reaction flask equipped with a stirrer, a thermometer, and a reflux condenser, under the protection of dry nitrogen, add 172.2 g (2.1 moles) of sodium acetate and 430 g of n-hexane; 129 g (1.0 mol) of dimethyldichlorosilane was injected. Under stirring, dimethyldichlorosilane was slowly added dropwise. After the drop was completed, the temperature was raised to 65-70°C and maintained for 1 hour. After the reaction is complete, filter off sodium chloride and unreacted sodium acetate while it is hot (about 50°C). The solvent is recovered from the filtrate by distillation, and what remains in the distillation bottle is dimethyldiacetoxysilane.

[0019] Get 158.4g (0.9 moles) of dimethyldiacetoxysilane and 296g (1.0 moles) of dimethylcyclosiloxane and add them in a four-necked flask equipped with a stirrer, a thermometer and a reflux condenser under the protection of dry nitrogen. Add 7.3g of zinc chloride (i.e. 1.6% of the total amount of reactants) unde...

Embodiment 2

[0021] The same device as in Example 1. In the formula of the first step, 430g of normal hexane is changed into 430g of benzene, all the other formulas are unchanged, and the reaction operations are all the same as in Example 1. In the second step, 176g (1.0 mole) of dimethyldiacetoxysilane and 296g (1.0 mole) of dimethylcyclosiloxane were taken, and other formulas and operating methods were the same as in Example 1. The final product obtained: viscosity 27.6mm2 / s, hydroxyl content 4.7%.

Embodiment 3

[0023] In a four-necked reaction flask equipped with a stirrer, a thermometer, and a reflux condenser, under the protection of dry nitrogen, add 172.2 g (2.1 moles) of sodium acetate and 430 g of n-hexane; 129 g (1.0 mol) of dimethyldichlorosilane was injected. Under stirring, dimethyldichlorosilane was slowly added dropwise. After the drop was completed, the temperature was raised to 65-70°C and maintained for 1 hour. After the reaction is complete, filter off sodium chloride and unreacted sodium acetate while it is hot (about 50°C). The solvent is recovered from the filtrate by distillation, and what remains in the distillation bottle is dimethyldiacetoxysilane.

[0024] Get 264g (1.5 moles) of dimethyldiacetoxysilane and 348g (1.0 moles) of tetramethyltetravinyl cyclotetrasiloxane and add them into the four-port agitator, thermometer, and reflux condenser under the protection of dry nitrogen. In the bottle, add 10.0 g of aluminum trichloride (i.e. 1.63% of the total amoun...

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PUM

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Abstract

The invention discloses a method for preparing hydroxyl silicone oil by taking sodium acetate as an acylating agent. In the method, dimethyldichlorosilane, cyclosiloxane and the sodium acetate are used as raw materials, and the solvent is a nonpolar solvent; the sodium acetate and the dimethyldichlorosilane react in an inert solvent to form dimethyldiacetoxysilane; and after a product sodium chloride is removed and the solvent is recovered by distillation, the dimethyldiacetoxysilane and the cyclosiloxane react in the presence of the catalysts to form alpha,omega-end acyloxy silicone oil. Thesodium acetate is easy to recycle and process, the dimethyldichlorosilane and the sodium acetate are easy to react, and a newly formed silicon chain link is a part of a hydroxyl silicone oil molecule, so that the method has low overall cost; and a by-product aqueous solution of sodium acetate is dehydrated to form anhydrous sodium acetate for recycling, so that the method fulfills the aims of environmental protection and comprehensive utilization.

Description

technical field [0001] The invention belongs to the field of organosilicon synthesis, in particular using sodium acetate as an acylating agent and recycling it to prepare hydroxyl silicone oil. Background technique [0002] The short-chain hydroxyl silicone oil with 4-10 silicone chain members is especially suitable as a structure control agent for high-temperature vulcanized silicone rubber. The simplest method for preparing short-chain hydroxy silicone oil is the hydrolysis of difunctional silanes (such as dimethyldichlorosilane, dimethyldialkoxysilane, etc.). However, the hydroxy silicone oil produced by this method, because of the (CH 3 ) 2 Si(OH) 2 Very active, part of it will polymerize into cyclosiloxane, and the other part will polymerize into hydroxy silicone oil with different molecular lengths. Sometimes the content of hydroxyl group is very high, and the content of hydroxyl group is very low if you are not careful. It has been proved in theory that hydroxy si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/16C08G77/06
Inventor 蒋志平杨浩平陈中民叶剑豪彭健陈益
Owner 溧阳巨神科技材料有限公司