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Method for synthesizing ketocarbonyl-containing bis-hydroxypropyl terminated polysiloxane

A bishydroxypropyl sealing and polysiloxane technology, applied in the direction of polyurea/polyurethane coatings, coatings, etc., can solve the problems affecting the physical and mechanical properties of the coating film, poor mechanical properties, etc., to improve the physical and mechanical properties, improve Water resistance, the effect of improving the relative molecular mass

Inactive Publication Date: 2010-11-17
INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the introduction of polysiloxane segments into polyurethane molecules can significantly improve the water resistance of the coating film, the shortcomings of polysiloxane's poor mechanical properties also affect the physical and mechanical properties of the coating film.

Method used

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  • Method for synthesizing ketocarbonyl-containing bis-hydroxypropyl terminated polysiloxane
  • Method for synthesizing ketocarbonyl-containing bis-hydroxypropyl terminated polysiloxane

Examples

Experimental program
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Embodiment 1

[0027] Transesterification reaction (molar ratio triphenylphosphine: ethyl acetoacetate: allyl alcohol = 0.1:1:1.3)

[0028] In a 100mL three-necked flask, add 13.03g of ethyl acetoacetate, 7.54g of allyl alcohol, 2.62g of triphenylphosphine and 20mL of toluene, raise the temperature of the reaction system to 100°C, and continue the reaction at this temperature for 8 hours, stop reaction. The reaction solution was distilled under reduced pressure, and the fraction at 77°C / 1.13KPa was collected to obtain 10.82 g of allyl acetoacetate, with a yield of 76%.

[0029] Hydroxyl protection reaction (molar ratio of allyl alcohol: hexamethyldisilazane == 2: 1.1)

[0030] In a 100mL three-necked flask, slowly add 35.52g of hexamethyldisilazane to 23.23g of allyl alcohol dropwise at room temperature. After the dropwise addition, raise the temperature of the reaction system to 100°C and continue the reaction at this temperature After 6 hours, the reaction stopped. Atmospheric pressure ...

Embodiment 2

[0041] Ethyl acetoacetate is changed to methyl acetoacetate in the transesterification reaction of embodiment 1, and the ratio of the amount of methyl acetoacetate and allyl alcohol becomes 1: 1, and other reaction conditions are as described in embodiment 1, obtain Allyl acetoacetate, the yield was 72%.

Embodiment 3

[0043] The ratio of the amount of allyl alcohol and hexamethyldisilazane in the hydroxyl protection reaction of Example 1 is changed to 2: 1, and other reaction conditions are as described in Example 1 to obtain allyloxytrimethylsilane, The yield was 80%.

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Abstract

The invention discloses a method for synthesizing ketocarbonyl-containing bis-hydroxypropyl terminated polysiloxane. A target compound, namely the bis-hydroxypropyl terminated polysiloxane of which the side group contains ketocarbonyl, is prepared by taking methyl acetoacetate (or ethyl acetoacetate), allyl alcohol, hexamethyldisilazane, tetramethyldisilazane, tetramethylcyclotetrasiloxane and octamethylcyclotetrasiloxane as starting materials, and by performing ester interchange, hydroxyl protection, hydrosilylation, equilibrium polymerization and alcoholysis reaction. The purity of the product is over 98 percent.

Description

technical field [0001] The invention relates to a method for synthesizing polysiloxane, in particular to a method for synthesizing ketone carbonyl-containing dihydroxypropyl-terminated polysiloxane. Background technique [0002] Due to its environmental friendliness, water-based polyurethane has made great progress in the field of coating agents since its inception, but it also encountered a problem that restricts its application, that is, the existence of hydrophilic groups in the molecular chain segment makes the water-based polyurethane coating film poor in water resistance. . As we all know, polysiloxane has good water resistance. In order to improve the water resistance of waterborne polyurethane coating film, the method often used is to modify polyurethane with polysiloxane. Although the introduction of polysiloxane segments into polyurethane molecules can significantly improve the water resistance of the coating film, the disadvantage of polysiloxane's own poor mecha...

Claims

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Application Information

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IPC IPC(8): C08G77/14C08G77/06C08G18/61C09D175/04
Inventor 张萌岳晖邬元娟孙素芬刘峰
Owner INST OF QUALITY STANDARDS & TESTING TECH FOR AGRO PROD OF SHANDONG ACADEMY OF AGRI SCI
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