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Preparation method of polyether modified silicone oil used for producing antistatic agent

A technology of polyether modified silicone oil and antistatic agent, which is applied in the direction of chemical instruments and methods, and other chemical processes, and can solve the problems of easy residual catalyst, yellowish product color, and affecting product performance, and achieve high purity and specific surface area. Large, well-performing effects

Inactive Publication Date: 2017-10-24
义乌市诠铈新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Polyether modified silicone oil can not only be used as defoamer and leveling agent in industrial fields, but also widely used in daily life, such as fabric finishing agent, cosmetics, etc. Most of the existing polyether modified silicone oil production processes use Simple filtration, activated carbon adsorption and other methods for product purification, the products produced are prone to residual impurities such as catalysts and raw materials, which makes them unsuitable for daily life such as daily chemicals and fabric finishing, and affects product performance. At the same time, it may cause product color Therefore, it is necessary to develop an easy-to-use high-efficiency adsorbent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1. Preparation of Adsorbent

[0017] In a 1000L high-speed stirred tank, add 100Kg of agarose hydrophobic interaction medium, 0.5Kg of tert-butyl 3-oxoazetidine-1-carboxylate, (R)-(+)-3-aminotetrahydrofuran p-toluenesulfonic acid Salt 0.5Kg, (1-(2-(trimethylsilyl) ethoxymethyl))-1H-imidazole-2-methanamine hydrochloride 1Kg, N,N-dimethylformamide 350Kg, at 80 The reaction is carried out at ℃ for 10 hours, and the product is separated and dried to obtain the adsorbent product of the present invention.

[0018] 2. Preparation of polyether modified silicone oil

[0019] In parts by weight, react 100 parts of polyether, 130 parts of hydrogen-containing silicone oil, 2 parts of chloroplatinic acid, and 18 parts of isopropanol in a nitrogen atmosphere at a temperature of 95°C for 4 hours. The product is filtered and separated to obtain polyether modified Pass the crude product of polyether-modified silicone oil into the chromatographic column equipped with the adsorbent prod...

Embodiment 2

[0021] 1. Preparation of Adsorbent

[0022] In a 1000L high-speed stirred tank, add 100Kg of agarose hydrophobic interaction medium, 0.1Kg of tert-butyl 3-oxoazetidin-1-carboxylate, (R)-(+)-3-aminotetrahydrofuran p-toluenesulfonic acid Salt 0.1Kg, (1-(2-(trimethylsilyl)ethoxymethyl))-1H-imidazole-2-methanamine hydrochloride 0.5Kg, N,N-dimethylformamide 200Kg, then React at a temperature of 60° C. for 6 hours, and the product is separated and dried to obtain the adsorbent product of the present invention.

[0023] 2. Preparation of polyether modified silicone oil

[0024] In parts by weight, react 100 parts of polyether, 80 parts of hydrogen-containing silicone oil, 1 part of chloroplatinic acid, and 10 parts of isopropanol in a nitrogen atmosphere at a temperature of 80°C for 2 hours. The product is filtered and separated to obtain a polyether modified For the crude product of silicone oil, pass the crude product of polyether-modified silicone oil into the chromatographic co...

Embodiment 3

[0026] 1. Preparation of Adsorbent

[0027] In a 1000L high-speed stirred tank, add 100Kg of agarose hydrophobic interaction medium, 1Kg of tert-butyl 3-oxoazetidin-1-carboxylate, (R)-(+)-3-aminotetrahydrofuran p-toluenesulfonate 1Kg, (1-(2-(trimethylsilyl)ethoxymethyl))-1H-imidazole-2-methanamine hydrochloride 2Kg, N,N-dimethylformamide 500Kg, then 100℃ After reacting at high temperature for 15 hours, the product was separated and dried to obtain the adsorbent product of the present invention.

[0028] 2. Preparation of polyether modified silicone oil

[0029] In parts by weight, react 100 parts of polyether, 180 parts of hydrogen-containing silicone oil, 5 parts of chloroplatinic acid, and 30 parts of isopropanol in a nitrogen atmosphere at a temperature of 110°C for 4 hours. The product is filtered and separated to obtain polyether modified Pass the crude product of polyether-modified silicone oil into the chromatographic column equipped with the adsorbent produced in ste...

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Abstract

The invention provides a preparation method of polyether modified silicone oil used for producing an antistatic agent. The preparation method comprises the steps of: 1) preparing raw materials including, by weight, 100 parts of polyether, 80-180 parts of hydrogen-containing silicone oil, 1-5 parts of chloroplatinic acid, and 10-30 parts of isopropyl alcohol; 2) in a nitrogen gas environment, performing a reaction at 80-110 DEG C for 2-6 h; 3) filtering and separating a product to produce a crude product of the polyether modified silicone oil; and 4) treating the crude product of the polyether modified silicone oil on a chromatographic column packed with a high-effective adsorbent at the flowing rate of 0.5 BV, thus producing the high-purity polyether modified silicone oil product.

Description

technical field [0001] The invention relates to a preparation method of polyether modified silicone oil, in particular to a preparation method of polyether modified silicone oil for antistatic agent. Background technique [0002] Polyether modified silicone oil is a silicone nonionic surfactant with unique properties. It has good lubricity, lower surface tension, better softness and antistatic properties, and good leveling properties, which can improve the intermolecular stress of the resin, overcome the shortcomings of these resins, and obtain new It has good demulsibility and is suitable for oil-water separation in some specific occasions. Compared with polydimethylsiloxane, this product can be miscible with water in any proportion, and it is also compatible with polar organic solvents such as alcohol , DMF, ether, ester, etc. are mutually soluble, and are partially or completely soluble in non-polar solvents such as toluene and alkanes. It is easy to use and has a wide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C08G77/34B01J20/22B01J20/30
CPCB01J20/22C08G77/34C08G77/46
Inventor 王艺霖曹东立
Owner 义乌市诠铈新材料有限公司