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Long-chain alkyl phenyl modified hydrogen containing silicone oil releasing agent preparation method

A long-chain alkylphenyl and release agent technology, applied in the direction of silicon organic compounds, can solve the problems of complex process, long cycle, high cost, etc., and achieve the effects of small steric hindrance, high conversion rate, and high efficiency

Inactive Publication Date: 2015-04-08
仪征市新源新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention proposes a method for preparing a long-chain alkylphenyl modified hydrogen-containing silicone oil release agent. The synthesis process involved in this application is the addition of styrene and alpha olefins to tetramethyltetrahydrocyclotetrasiloxane , and then under the action of octamethylcyclotetrasiloxane and hexamethyldisiloxane, ring-opening polymerization of long-chain alkylphenyl modified hydrogen-containing silicone oil release agent, this technology overcomes the synthesis process of the prior art Existing problems and deficiencies such as complex process, low efficiency, high cost and long cycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Under nitrogen protection, 20 parts by mass of tetramethyltetrahydrocyclotetrasiloxane and 0.140 parts by mass of catalyst were added to the reactor, and when the temperature was raised to 120°C, 17.36 parts by mass of styrene was uniformly added dropwise within 30 minutes. After the addition of styrene, the reaction time was maintained at 120°C for 3 hours, and then 18.70 parts by mass of octene and 0.112 parts by mass of isopropanol solution of chloroplatinic acid were added dropwise at the same time, and the dropping time was controlled at 30 minutes. Continue the reaction at 120°C for 6 h, lower the temperature to 50°C, add 2% activated clay for adsorption, filter with suction, and remove low-volatile substances at a temperature lower than 0.01 MPa to obtain tetramethylalkylphenylcyclotetrasilicon Oxygen intermediates. 56.06 parts by mass of the tetramethylalkylphenylcyclotetrasiloxane intermediate product, 66.83 parts by mass of octamethylcyclotetrasiloxane, 13...

Embodiment example 2

[0017] Under nitrogen protection, 20 parts by mass of tetramethyltetrahydrocyclotetrasiloxane and 0.146 parts by mass of catalyst were added to the reactor, and when the temperature was raised to 120°C, 17.36 parts by mass of styrene was uniformly added dropwise within 30 minutes. After the addition of styrene, the reaction time was maintained at 120°C for 3 hours, and then 21.04 parts by mass of nonene and 0.117 parts by mass of isopropanol solution of chloroplatinic acid were added dropwise at the same time, and the dropping time was controlled at 30 minutes. Continue the reaction at 120°C for 6 h, lower the temperature to 50°C, add 2% activated clay for adsorption, filter with suction, and remove low-volatile substances at a temperature lower than 0.01 MPa to obtain tetramethylalkylphenylcyclotetrasilicon Oxygen intermediates. 58.40 mass parts of tetramethylalkylphenyl cyclotetrasiloxane intermediate product, 64.35 mass parts of octamethylcyclotetrasiloxane, 13.52 mass ...

Embodiment example 3

[0019] Under nitrogen protection, 20 parts by mass of tetramethyltetrahydrocyclotetrasiloxane and 0.152 parts by mass of catalyst were added to the reactor, and when the temperature was raised to 120°C, 17.36 parts by mass of styrene was uniformly added dropwise within 30 minutes. After the addition of styrene, the reaction time was maintained at 120°C for 3 h, and then 23.33 parts by mass of decene and 0.121 parts by mass of isopropanol solution of chloroplatinic acid were added dropwise at the same time, and the dropping time was controlled at 30 min. Afterwards, the reaction was continued at 120°C for 6 h, the temperature was lowered to 50°C, 2% activated clay was added for adsorption, and the low volatile substances were removed by suction filtration at a temperature lower than 0.01 MPa to obtain tetramethylalkylphenylcyclotetra Siloxane intermediates. 60.69 mass parts of tetramethylalkylphenyl cyclotetrasiloxane intermediate product, 59.40 mass parts of octamethylcyclotet...

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PUM

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Abstract

The invention discloses a long-chain alkyl phenyl modified hydrogen containing silicone oil releasing agent preparation method. The method includes the steps of subjecting tetramethyl tetra-hydrogen cyclotetrasiloxane and a catalyst of chloroplatinic acid to reaction, dropping styrene for reaction for some time, dropping long-chain alpha-olefin and a chloroplatinic acid isopropyl propanol solution to obtain an intermediate product of tetramethyl alkyl phenyl cyclotetrasiloxane, subjecting the obtained intermediate product of tetramethyl alkyl phenyl cyclotetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and an acid catalyst to full reaction, fully cooling the obtained liquid, slowly adding calcium hydroxide to adjusting the PH value to 6-7, filtering out solids produced in neutralization with a vacuum pump, adding anhydrous magnesium sulfate to adsorb water produced in neutralization, and filtering to obtain a long-chain alkyl phenyl modified hydrogen containing silicone oil releasing agent. The long-chain alkyl phenyl modified hydrogen containing silicone oil releasing agent prepared through the preparation method has the advantages of being simple in process, high in efficiency, low in cost, short in cycle and the like.

Description

technical field [0001] The invention relates to a preparation method of a long-chain alkylphenyl modified hydrogen-containing silicone oil release agent. Background technique [0002] As a mold release agent, long-chain alkylphenyl modified silicone oil has the advantages of chemical resistance and heat resistance, so it is widely used in resin molds. [0003] Existing technical route: Using conventional macromolecular hydrogen-containing silicone oil in the market as raw material, hydrogen-containing silicone oil with a suitable molecular weight is obtained through telomerization, and long-chain olefins and styrene are added to hydrogen-containing silicone oil to synthesize the target product. [0004] The disadvantages of this route are: [0005] 1. The hydrogen-containing silicone oil used in this method is obtained by telomerization of macromolecular hydrogen-containing silicone oil. The molecular weight distribution obtained after telomerization of the hydrogen-contain...

Claims

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Application Information

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IPC IPC(8): C08G77/06B29C33/64C07F7/21
Inventor 季永新李俊姜金梅
Owner 仪征市新源新材料科技有限公司
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