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Silicon oil preparation method

A technology of silicone oil and high hydrogen-containing silicone oil, which is applied in the field of silicone oil production, can solve the problems of side reactions, long reaction time, and complicated procedures in the polymerization process, and achieve the effects of simple operation, avoiding side reactions, and improving product quality

Inactive Publication Date: 2013-09-04
JIANGSU OSIC PERFORMANCE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 3) There are side reactions during the polymerization process;
[0007] 4) The reaction time is relatively long and the energy consumption is high;
[0008] 5) The process is complicated and the yield is low (90-92%)

Method used

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  • Silicon oil preparation method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] At 30°C, add 25 parts of D4 (I), 2 parts of hexamethyldisiloxane according to (II) and 5 parts of hydrogen-containing silicone oil (III) into mixing kettle 1 in proportion, and pre-mix for 30 minutes. During the mixing process Heat the raw material to 40-80°C, pass the metering pump 2 at a rate of 1-20m 3 / h flow rate to transfer the pre-mixed raw materials to the catalytic bed 3, the pressure of the pre-mixture passing through the resin catalytic bed 3 is kept at 1MPa, and the contact time is kept at 6h. (IV).

Embodiment 2

[0034] At 20°C, add 40 parts of D4 (I) and 2 parts of tetramethyldisiloxane (V) into the mixing kettle 1 in proportion, and pre-mix for 30 minutes. During the mixing process, the raw materials are heated to 40-80°C. Metering pump 2 is 1~20m 3 / h flow rate transfers the pre-mixed raw material to the catalytic bed 3, the pre-mixture is kept at 0.85MPa by the resin catalytic bed pressure, and the contact time is maintained at 8h, and the product obtained by the reaction is collected by the collection tank 4, which is terminal hydrogen silicone oil ( VI).

Embodiment 3

[0036] At 45°C, add 20 parts of D4 (I) and 5 parts of heptamethyltrisiloxane (VII) into mixing kettle 1 in proportion, and pre-mix for 30 minutes. During the mixing process, the raw materials are heated to 40-80°C, and the metering pump 2 is used for 1-20m 3 The premixed raw material is transferred to the catalytic bed 3 at a flow rate of / h. The pressure of the premixed resin catalytic bed is kept at 1.2MPa, and the contact time is kept at 4h. (VIII).

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Abstract

The invention discloses a silicon oil preparation method. The method comprises the following steps: adding reaction raw materials comprising octamethylcyclotetrasiloxane, hexamethyldisiloxane and polymethylhydrosiloxane, or octamethylcyclotetrasiloxane and tetramethyldisiloxane, or octamethylcyclotetrasiloxane and heptamethyltrisiloxane to a mixing kettle, uniformly mixing, carrying out preheating treatment, metering through a catalysis bed filled with an acidic anion resin catalyst, and reacting to obtain silicon oil. A fluidized bed is utilized to substitute a production technology grating an organosilicon copolymer intermediate through a general catalyst continuous process. The monomer residual quantity is reduced to below 5%, a too wide problem of the polymer molecule weight is solved, and the polymer molecule weight distribution index is less than 1.1. The reaction time is shortened, and the generation of side reactions is effectively avoided. The method has the characteristics of product quality improvement, simple operation, low energy consumption and the like.

Description

technical field [0001] The invention relates to the technical field of silicone oil production, in particular to a method for continuously preparing hydrogen-terminated silicone oil and hydrogen-containing silicone oil. Background technique [0002] At present, the domestic production of grafted silicone copolymer intermediates is mainly based on the batch method. In this method, after the monomer is heated up (80 ° C ~ 100 ° C), the catalyst (usually protons such as sulfuric acid) is directly added to the kettle. acid), after long-term polymerization (15-20h), the production is completed through neutralization (alkali neutralization, generally using sodium bicarbonate), cooling, desalination, and filtration. [0003] The above method has the following disadvantages: [0004] 1) The residual amount of monomer and catalyst impurities is high, generally greater than 8%; [0005] 2) Polymer molecular weight distribution Broad molecular weight distribution Index>1.2; [00...

Claims

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Application Information

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IPC IPC(8): C08G77/44C08G77/12C08G77/06
Inventor 郭毅吴斌周宇宇
Owner JIANGSU OSIC PERFORMANCE MATERIALS CO LTD
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