Method for synthesizing dihydroxyl-terminated polysiloxane

The technology of a dihydroxyalkyl polysiloxane and a synthesis method is applied in the field of synthesis of double-terminal dihydroxyalkyl polysiloxanes, which can solve problems such as high cost, unfavorable application fields, and decreased yield of final products, and achieve improved Production efficiency, short total reaction time, and production cost reduction effects

Inactive Publication Date: 2012-06-20
邬元娟
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the reaction process, the yield of the final product decreases due to the side reaction between the hydroxyl group and the Si-H group. Therefore, in order to avoid the side reaction, the conventional method is to protect the hydroxyl group first, and then remove the protecting group after the reaction is completed. remove
[0003] Although hydroxyl protection can effectively suppress side reactions and provide product yield, the cost of using hexamethyldisilazane or trimethylchlorosilane as hydroxyl protecting agent is higher; in addition, the protection and deprotection of hydroxyl increase the Reaction steps, so that the total reaction time to synthesize the final product also increases
These shortcomings also increase the industrialization cost of hydroxyhydrocarbyl polysiloxane, which is not conducive to expanding the application field

Method used

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  • Method for synthesizing dihydroxyl-terminated polysiloxane
  • Method for synthesizing dihydroxyl-terminated polysiloxane
  • Method for synthesizing dihydroxyl-terminated polysiloxane

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Hydrosilylation reaction (molar ratio of allyl glycidyl ether: tetramethyldisiloxane: chloroplatinic acid = 2.4: 1: 3.1 × 10 -4 ) In a 100ml four-necked bottle, add allyl glycidyl ether 27.38g, 10mL toluene and 40μL chloroplatinic acid 3.1×10 -5 mol of isopropanol solution, after passing nitrogen gas for 20 minutes, the temperature of the reaction system was raised to 100° C., and 13.41 g of tetramethyldisiloxane was added dropwise at this temperature, and the reaction was terminated after 8 hours of reaction. Vacuum distillation collected at 198-202°C (0.67KPa) to obtain 32.44g of 1,3-diepoxy-terminated disiloxane with a yield of 89.6%.

[0024] The product was characterized by infrared spectroscopy, as shown in the attached figure 1 The infrared spectrum shown. It can be seen from the map that the 1108cm -1 The stretching vibration absorption peak of the C-O-C bond appeared at 3051cm -1 The stretching vibration absorption peak of the C-H bond on the epoxy bond app...

Embodiment 2

[0031] Allyl glycidyl ether in the hydrosilylation reaction of Example 1 was replaced by 1,2-epoxy-8-nonene, 1,2-epoxy-8-nonene and tetramethyldisiloxane The ratio of the amount of alkane substance becomes 2.6: 1, and other reaction conditions are as described in embodiment 1, obtain the 1 of structure different from embodiment 1, the 3-diepoxy-terminated disiloxane, yield is 84% .

Embodiment 3

[0033] In the equilibrium reaction of embodiment 1, 1,3-bis(hydroxyethyl) hydroxyalkyl terminated disiloxane and D 4 The ratio of the amount of the substance becomes 1:9, and other reaction conditions are as described in Example 1, and the target compound double-terminal containing dihydroxyhydrocarbyl polysiloxane having an average molecular weight different from Example 1 of 3200 is obtained, and the yield 87%.

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Abstract

The invention discloses a method for synthesizing dihydroxyl-terminated polysiloxane. The method synthesizes the target dihydroxyl-terminated polysiloxane compound by using unsaturated epoxy compound, tetramethyldisiloxane, methylaminoethanol and octamethylcyclotetrasiloxane as starting materials and by hydrosilylation, epoxy-opening and equilibrium polymerization. The hexamethyldisilazane or trimethylchlorosilane are not needed as a hydroxyl protector, so the production cost is reduced; and hydroxyl protection and deprotection are avoided in a preparation process, so reaction steps are reduced, the total reaction time for synthesizing the final product is short and the production efficiency is increased.

Description

technical field [0001] The invention relates to a method for synthesizing polysiloxane containing two hydroxyl groups at both ends. Background technique [0002] Due to the presence of chemically active hydroxyalkyl functional groups, more and more hydroxyalkyl polysiloxanes are used to react with isocyanate groups or carboxyl groups to modify certain synthetic resins (such as polyurethane and polyester). properties to improve various properties of materials. However, most hydroxyhydrocarbyl polysiloxanes are generally prepared by reacting unsaturated hydroxyl compounds with Si-H groups. During the reaction process, the yield of the final product decreases due to the side reaction between the hydroxyl group and the Si-H group. Therefore, in order to avoid the side reaction, the conventional method is to protect the hydroxyl group first, and then remove the protecting group after the reaction is completed. remove. [0003] Although hydroxyl protection can effectively suppr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/26C08G77/16C08G77/06
Inventor 邬元娟张萌郭栋梁方丽萍董崭王峰恩
Owner 邬元娟
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