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Application of phosphazene compound in preparation of methyl silicone oil and preparation method of methyl silicone oil

A technology of phosphazene compound and methyl silicone oil, which is applied in the application of phosphazene compound in the preparation of methyl silicone oil, the field of preparation of methyl silicone oil, can solve the problems of cumbersome production process, high energy consumption, and no catalyst residue.

Inactive Publication Date: 2020-10-23
上海抚佳精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Therefore, the technical problem to be solved by the present invention is to overcome the fact that the methyl silicone oil synthesized by the acid method or the alkali method in the prior art cannot take into account the two aspects of no catalyst residue and no low molecular weight impurities, and both have cumbersome production processes and energy consumption. Higher defects, thereby providing a kind of phosphazene compound in the preparation method of the application of methyl silicone oil and methyl silicone oil

Method used

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  • Application of phosphazene compound in preparation of methyl silicone oil and preparation method of methyl silicone oil
  • Application of phosphazene compound in preparation of methyl silicone oil and preparation method of methyl silicone oil
  • Application of phosphazene compound in preparation of methyl silicone oil and preparation method of methyl silicone oil

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Embodiment 1

[0042] The present embodiment relates to a kind of preparation method of methyl silicone oil, comprises the following steps:

[0043] Under nitrogen protection, 93.20g octamethylcyclotetrasiloxane, 6.80g hexamethyldisiloxane and 0.02g phosphazene compound P 8 Add OH into the reactor, react at 40°C for 1 hour, and control the stirring speed at 550r / min. After the reaction, the reaction system is adsorbed by silica gel to remove the phosphazene compound to obtain the final product.

[0044]The reaction yield is 95%, and the product is colorless and transparent, and the GPC (gel permeation chromatography) detects Mw=2390g / mol, and the GPC detection result is as follows: figure 1 shown.

[0045] After CPR (trace alkaline substance) detection, the alkali content in the final product was 0 ppm, which confirmed that there was no phosphazene compound residue in the final product.

Embodiment 2

[0047] The present embodiment relates to a kind of preparation method of methyl silicone oil, comprises the following steps:

[0048] Under nitrogen protection, 128.80g octamethylcyclotetrasiloxane, 9.70g 1,1,3,3-tetramethyldisiloxane and 0.14g phosphazene compound P 8 Add OH into the reactor, react at 35°C for 2h, and control the stirring speed at 500r / min. After the reaction, add 2-3 drops of glacial acetic acid to quench the catalyst, extract the reaction system with methanol and remove the phosphazene compound to obtain the final product.

[0049] The reaction yield is 94%, and the product is colorless and transparent. It is detected by GPC with Mw=1945g / mol. The GPC detection curve is shown in figure 2 .

[0050] After CPR detection, the alkali content in the final product was 0 ppm, which confirmed that there was no phosphazene compound residue in the final product.

Embodiment 3

[0052] The present embodiment relates to a kind of preparation method of methyl silicone oil, comprises the following steps:

[0053] Under nitrogen protection, 211.85g hexamethylcyclotrisiloxane, 57.23g methyl hydrogen silicone oil (hydrogen content is 1.59%), 30.91g hexamethyldisiloxane and 0.06g phosphazene compound P 8 Add OH into the reactor, react at 30°C for 5h, and control the stirring speed at 600r / min. After the reaction was finished, 2 g of glacial acetic acid was added to neutralize the phosphazene compound to inactivate it to obtain the final product.

[0054] The reaction yield is 96%, and the product is colorless and transparent. It is detected by GPC that Mw=1450g / mol. The GPC detection curve is shown in image 3 .

[0055] After CPR detection, the alkali content in the final product was 0 ppm, which confirmed that there was no phosphazene compound residue in the final product.

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Abstract

The invention relates to the field of methyl silicone oil preparation. The invention particularly relates to application of a phosphazene compound in preparation of methyl silicone oil and a preparation method of the methyl silicone oil. The preparation method of the methyl silicone oil comprises the following steps: adding a cyclosiloxane monomer, linear siloxane, an end-capping reagent and the phosphazene compound into a reactor, carrying out a ring-opening polymerization reaction under the protection of an inert atmosphere, and removing the phosphazene compound in the obtained product afterthe reaction is finished, thereby obtaining the methyl silicone oil. The preparation method is simple and effective, the energy consumption is low, and the catalytic activity of the used phosphazenecompound is high; when the phosphonitrile compound is used for catalyzing the ring-opening polymerization reaction of cyclosiloxane, a formed product is closer to a target product, side reactions arefew in the reaction process, and the phosphonitrile compound is easy to remove from a system, so that the obtained methyl silicone oil is controllable in molecular weight, regular in structure, high in purity and free of small molecular impurities and catalyst residues.

Description

technical field [0001] The invention relates to the field of methyl silicone oil preparation, in particular to an application of a phosphazene compound in the preparation of methyl silicone oil and a preparation method of methyl silicone oil. Background technique [0002] Polysiloxane is a kind of polymer with repeated Si-O bonds as the main chain, and organic groups are directly connected to silicon atoms. Silicone oil refers to a linear polysiloxane product that maintains a liquid state at room temperature. Silicone oil has Good surface activity, heat resistance, weather resistance and aging resistance, and it is colorless, odorless and physiologically inert. After further modification and cross-linking, the product can be used as a foam stabilizer, defoamer, wetting agent, conditioner, etc. , has a wide range of applications in polyurethane foam, pesticides, cosmetics, coatings, textile printing and dyeing, oil exploration, building materials and other fields. [0003] S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/30C08G77/26C08G77/06
CPCC08G77/06C08G77/26C08G77/30
Inventor 郭奕孟静夏凉李玉博
Owner 上海抚佳精细化工有限公司