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Method of synthetizing small molecule hydroxyl silicone oil through using continuation method

A technology of molecular hydroxy silicone oil and continuous method, which is applied in the field of synthesizing small molecule hydroxy silicone oil, can solve the problem of acetic acid taste in the product, and achieve the effects of high product yield, good repeatability, and good storage stability

Active Publication Date: 2012-07-11
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many ways to prepare small-molecule hydroxy silicone oil. At present, the most used in industrial production is the reaction of D4 (DMC) and acetic anhydride, but the product has the smell of acetic acid.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] A continuous method for synthesizing small-molecule hydroxy silicone oil. Add 1,000 grams of hexamethylcyclotrisiloxane, 1,400 grams of acetone, and 120 grams of water into a 3,000-ml four-necked bottle with stirring, raise the temperature and keep it at 50°C, dissolve and mix After uniformity, adopt a peristaltic pump to continuously pass through a fixed bed of 100 grams of D001 strong acid ion exchange resin and a fixed bed of 100 grams of KY-23 strong acid ion exchange resin, each fixed bed reaction temperature is 50 ° C, and the residence time is controlled at 50 seconds. The crude product of small molecule hydroxy silicone oil was obtained, and the crude product was desolvated by normal pressure, and then the low components were removed under reduced pressure to obtain a small molecule hydroxy silicone oil with a viscosity of 22CS, a hydroxyl content of 9%, and a yield of 94.6%.

[0010] Stability is reflected in the appearance of the product as a colorless transpar...

Embodiment 2

[0012] A continuous method for synthesizing small-molecule hydroxysilicone oil. Add 1,000 grams of hexamethylcyclotrisiloxane, 1,400 grams of acetone, and 120 grams of water into a 3,000-ml four-necked bottle with stirring, raise the temperature and keep it at 40°C, dissolve and mix After uniformity, adopt peristaltic pump to pass through continuously the fixed bed that is added with 100 grams of 732 ion exchange resins and the fixed bed of 100 grams of KY-2 ion exchange resins, each fixed bed reaction temperature is 40 ℃, residence time is controlled at 30 seconds, obtains small The crude product of molecular hydroxy silicone oil, the crude product is often desolvated by pressure, and then the low components are removed under reduced pressure to obtain small molecular hydroxy silicone oil with a viscosity of 24CS, a hydroxyl content of 8%, and a yield of 90.1%.

[0013] Stability is reflected in the fact that after 6 months of storage, the appearance of the product is a colorl...

Embodiment 3

[0015] A continuous method for synthesizing small-molecule hydroxy silicone oil. Add 1,000 grams of hexamethylcyclotrisiloxane, 1,400 grams of acetone, and 120 grams of water into a 3,000-ml four-necked bottle with stirring, raise the temperature and keep it at 60°C, dissolve and mix After uniformity, use a peristaltic pump to continuously pass through 2 fixed beds with 100 grams of D001 strong acid ion exchange resin and 100 grams of KY-2 ion exchange resin. The reaction temperature of each fixed bed is 60 ° C, and the residence time is controlled at 70 Seconds, the crude product of small molecule hydroxy silicone oil was obtained. The crude product was desolvated by normal pressure and then the low components were removed under reduced pressure to obtain small molecule hydroxy silicone oil with a viscosity of 20CS, a hydroxyl content of 9%, and a yield of 93.9%.

[0016] Stability is reflected in the fact that after 6 months of storage, the appearance of the product is a colo...

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PUM

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Abstract

The invention relates to a method of synthetizing small molecule hydroxyl silicone oil through using a continuation method. The method comprises the steps as follows: adding the1,000 g of hexamethyl cyclotrisiloxane, 1,400 g of acetone and 120 g of water into a 3,000 ml four-mouth bottle with the stirring function, heating and keeping the temperature to 40 DEG C to 60 DEG C, melting and mixing uniformly; adopting a peristaltic pump to continuously pass through two fixed beds added with 100 g of strongly acidic styrene cation exchange resin, wherein the strongly acidic styrene cation exchange resin comprises a macroporous type and a gel type, and has the following grades: 732, D001, KY-2 and KY-23; obtaining a small molecule hydroxyl silicone oil crude product after the each fixed bed reaction temperature is 40 DEG C to 60 DEG C and the retention time is controlled to 30-70 seconds; and obtaining small molecule hydroxyl silicone oil after the crude product is subject to normal pressure desolvation, decompression and removal of low component. The method has the advantages of continuation production, high reproducibility and high product yield; and moreover, the product is colorless transparent liquid from the appearance, the viscosity is 15-30 mm2 / s, and the hydroxyl content is in the range of 6-10%.

Description

technical field [0001] The invention relates to a method for synthesizing small molecule hydroxy silicone oil, in particular to a method for continuously synthesizing small molecule hydroxy silicone oil. Background technique [0002] Small molecule hydroxy silicone oil is a substance with active hydroxyl groups, and is an ideal structure control agent for silicone rubber. There are many ways to prepare small-molecule hydroxy silicone oil. At present, the most used method in industrial production is the reaction of D4 (DMC) and acetic anhydride, but the product has the smell of acetic acid. Contents of the invention [0003] The invention provides a method for continuously synthesizing small-molecule hydroxy silicone oil, using the by-product D obtained in the production of organosilicon methyl cyclosiloxane 3 Use it as raw material to make hydroxy silicone oil, digest the by-products, increase the added value of the by-products, the yield is high, and the products can be ...

Claims

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Application Information

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IPC IPC(8): C08G77/16C08G77/06
Inventor 肖赣湘孙秀珍廖桂根贺志江
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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