Method for preparing inertia high-boiling silicone oil from organic silicone high-boiling residues

A technology of high-boiling silicone oil and high-boiling substances, which is applied in the field of high-boiling silicone oil preparation, can solve the problems of uncontrollable viscosity of high-boiling silicone oil products, inability to achieve complete replacement, and increase in the viscosity of silicone oil, so as to solve environmental protection and safety issues. Simple processing method and high production efficiency

Inactive Publication Date: 2016-12-07
浙江中天东方氟硅材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process uses methanol and chlorine groups in high-boiling substances to carry out alkoxy substitution, but in general, complete substitution cannot be achieved, and alkoxy groups are unstable, resulting in uncontrollable viscosity of high-boiling silicone oil products and low product quality , poor stability
[0010] Alcoholyze

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Utilize organosilicon high boiling matter to prepare inert high boiling silicone oil, the specific steps are:

[0070] A. Hydrolysis

[0071] At normal temperature, add 1000g cracking waste high boiling point, 50g methyl methacrylate, 30g trimethyl monochlorosilane in the stirred hydrolysis kettle, and then drop 365g water into the hydrolysis kettle, along with the dripping of water gradually A hydrolysis reaction occurs, the temperature of the hydrolysis reaction is 25±5°C, the dripping time is 1.5 hours, and the stirring is continued for 5 minutes after the dripping is completed, then the stirring is stopped, the stratification is allowed to stand, the aqueous phase is discarded, and the organic phase is washed twice with water;

[0072] B. Hydrosilylation

[0073] Transfer the washed organic phase into an addition reactor, then add 0.39 g of chloroplatinic acid-isopropanol solution with a mass concentration of 1% as a catalyst, raise the temperature to 60-70° C., an...

Embodiment 2

[0081] Utilize organosilicon high boilers to prepare inert high boiling silicone oil Inert high boiling silicone oil, the specific steps are:

[0082] A. Hydrolysis

[0083] At normal temperature, add 1000g of rectification waste high boiling point, 400g of mechanically used delowering fraction, 38g of trimethylchlorosilane into the stirred hydrolysis kettle, and then drop 375g of water into the hydrolysis kettle, and gradually A hydrolysis reaction occurs, the temperature of the hydrolysis reaction is normal temperature, the dripping time is 1h, and the stirring is continued for 10min after the dripping is completed, then the stirring is stopped, the stratification is allowed to stand, the acidic aqueous phase is discarded, and the organic phase is washed twice with water;

[0084] B. Hydrosilylation

[0085] Transfer the washed organic phase into an addition reactor, then add 0.48 g of chloroplatinic acid-isopropanol solution with a mass concentration of 1% as a catalyst, f...

Embodiment 3

[0093] Utilize organosilicon high boilers to prepare inert high boiling silicone oil Inert high boiling silicone oil, the specific steps are:

[0094] A. Hydrolysis

[0095] At normal temperature, add 1000g of cracking waste high boiling, 390g of n-dodecene, 43g of trimethyl monochlorosilane into the stirring hydrolysis kettle, then drop 388g of water into the hydrolysis kettle, and gradually hydrolyze with the dripping of water Reaction, hydrolysis reaction temperature is 30°C ~ 40°C, dripping time is 2h, continue to stir for 5min after dripping, then stop stirring, let stand to separate layers, discard the acidic aqueous phase, and wash the organic phase with water twice;

[0096] B. Hydrosilylation

[0097] Transfer the washed organic phase into an addition reactor, then add 0.50 g of chloroplatinic acid-isopropanol solution with a mass concentration of 1% as a catalyst, raise the temperature to 60-70° C., and carry out the addition reaction under stirring for 6 hours;

...

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Abstract

The invention discloses a method for preparing inertia high-boiling silicone oil from organic silicone high-boiling residues. With organic silicone high-boiling residues as the reaction raw material, the method includes the four steps of hydrolysis, hydrosilylation, neutralization, and devolatiligation and decoloration. The organic silicone high-boiling residues as the raw material are rectified high-boiling residues or decomposed high-boiling residues. The rectified high-boiling residues are high-boiling residues obtained by separating dimethyldichlorosilance out of the organic silicone high-boiling residues in advance through rectification. The decomposed high-boiling residues are high-boiling residues obtained by decomposing the organic silicone high-boiling residues in advance through a decomposing device and separating out monosilane. The decomposed high-boiling residues or rectified high-boiling residues which are difficult to process and use are used as the raw material, and the inertia high-boiling silicone oil which is controllable in viscosity, low in activity and high in stability is prepared through hydrolysis, addition and other reaction. The method is controllable in reaction process, simple in post-processing method, conventional in reaction device, high in production efficiency, stable in product quality and suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for preparing high-boiling silicone oil, in particular to a method for preparing inert high-boiling silicone oil by using organosilicon high-boiling matter. Background technique [0002] Organosilicon high boilers are a yellow, pungent and highly corrosive high-boiling chlorosilane mixture produced during the synthesis of methylchlorosilane monomers. Silicon-silicon bonds, silicon-carbon-silicon, silicon -Oxygen-silicon bonds, and also contain insoluble Cu, Zn, Al and a small amount of fine silicon powder left over from the synthesis reaction. The density of silicone high boiler is about 1.13g / cm 3 , the boiling range is 80-215°C. [0003] With the rapid development of the world's organosilicon industry, the output of methylchlorosilane is increasing, resulting in a large amount of organosilicon high boilers; in the process of synthesizing methylchlorosilane by direct method, every ton of crude monomer synthesized, ...

Claims

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Application Information

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IPC IPC(8): C08G77/18C08G77/06C08G77/04C08G77/32
CPCC08G77/18C08G77/04C08G77/06C08G77/32
Inventor 邵向东席先锋杨庆红曾鸿王鑫
Owner 浙江中天东方氟硅材料股份有限公司
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