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Hydroxyl terminated polyepichlorohydrin and preparation method thereof

A technology of hydroxyl-terminated polyepichlorohydrin and epichlorohydrin is applied in the field of hydroxyl-terminated polyepichlorohydrin and its preparation, and can solve the problems of poor heat resistance of polyurethane and the like

Active Publication Date: 2015-09-09
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of poor heat resistance of the existing polyurethane with hydroxyl-terminated polyepichlorohydrin as the matrix resin, and to provide a kind of hydroxyl-terminated polyepichlorohydrin and its preparation method

Method used

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  • Hydroxyl terminated polyepichlorohydrin and preparation method thereof
  • Hydroxyl terminated polyepichlorohydrin and preparation method thereof
  • Hydroxyl terminated polyepichlorohydrin and preparation method thereof

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preparation example Construction

[0026] The present invention also provides a kind of preparation method of hydroxyl-terminated polyepichlorohydrin, comprising as follows:

[0027] Mix heptasilsesquioxane trisilanol, boron trifluoride ether solution and solvent, the solvent is not particularly limited, preferably dichloromethane, and then drop the mixture of epichlorohydrin and dichloroethane Solution, to obtain a mixture, the preferred dropping temperature is 18-23°C, the obtained mixture is reacted at 40-45°C for 1.5-3.5h, and the product obtained is preferably washed with saturated sodium bicarbonate until neutral, and after extraction and vacuum distillation A hydroxyl-terminated polyepichlorohydrin is obtained.

[0028] The mass ratio of the mixed solution of described heptasilsesquioxane trisilanol, boron trifluoride ether solution and epichlorohydrin and ethylene dichloride is preferably (20-30):(10-20): (35-65). The volume ratio of epichlorohydrin and dichloroethane in the mixed solution of epichlor...

Embodiment 1

[0039] Weigh 3.3g of catalyst lithium hydroxide monohydrate and 1.27g of deionized water into a 500ml three-necked flask, add 165ml of a mixed solvent of acetone and methanol, and slowly add 31.1g of isobutyltrimethoxysilane dropwise under nitrogen protection; Then heat up to reflux 65°C, stir for 14 hours, stop heating, cool down to room temperature, add 150ml of concentrated hydrochloric acid (1mol / L) to acidify, stir for 2 hours; Washed three times and dried at 35°C for 48h to obtain white solid T7-POSS.

[0040] Add 30g of T7-POSS, 10g of boron trifluoride ether solution and dichloroethane into the reaction kettle and stir evenly, then add dropwise 35g of a mixed solution of epichlorohydrin and dichloroethane, and the reaction temperature is controlled At 18-23°C, after all the mixed solutions are added dropwise, the temperature is raised to 40°C to continue the reaction for 1.5 hours, and the resulting solution is washed repeatedly with saturated sodium bicarbonate until ...

Embodiment 2

[0043] Weigh 5.3g of catalyst lithium hydroxide monohydrate and 3.27g of deionized water into a 500ml three-necked flask, add 165ml of acetone and methanol mixed solvent, and slowly add 21.5g of cyclohexyltrimethoxysilane dropwise under the protection of nitrogen; Heat up to reflux 65°C, stir and react for 14 hours, stop heating, lower to room temperature, add 100ml of concentrated hydrochloric acid (1mol / L) to acidify, stir and react for 2 hours; after stopping stirring, filter with suction, wash the product with water until neutral, and then wash with acetonitrile Three times, and dried at 35°C for 48h, a white solid T7-POSS was obtained.

[0044]Add 20g of T7-POSS, 20g of boron trifluoride ether solution and dichloroethane into the reaction kettle and stir evenly, then add dropwise 45g of a mixed solution of epichlorohydrin and dichloroethane, and the reaction temperature is controlled At 18-23°C, after all the mixed solution has been added dropwise, the temperature is rais...

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Abstract

The invention provides hydroxyl terminated polyepichlorohydrin and a preparation method thereof, which belongs to the polyepichlorohydrin and its preparation method fields. A problem that heat resistance of polyurethane which takes hydroxyl terminated polyepichlorohydrin as a matrix resin is poor can be solved. A structural formula of the hydroxyl terminated polyepichlorohydrin is shown in a formula (1), and the invention also provides the preparation method of hydroxyl terminated polyepichlorohydrin. According to the invention, chloropropylene oxide takes hepta-polysilsesquioxane trimethylsilanolate, because that a main chain contains a silsesquioxane structure, heat resistance of polyurethane which takes hydroxyl terminated polyepichlorohydrin as the matrix resin can be greatly increased.

Description

technical field [0001] The invention belongs to the field of polyepichlorohydrin and its preparation method, and in particular relates to a hydroxyl-terminated polyepichlorohydrin and its preparation method. Background technique [0002] Hydroxyl-terminated epichlorohydrin is obtained by ring-opening polymerization of epichlorohydrin. The polyurethane elastomer and adhesive produced by the reaction with isocyanate compounds have excellent flame retardant properties, and there are a large number of methylene chloride groups on the molecular chain. Its chlorine content is as high as 38%. It has very good corrosion resistance and can adapt to the highly corrosive marine environment. It can be used to manufacture flame-retardant, seawater-resistant, oil-resistant polyurethane adhesives, coatings and potting materials. [0003] Most of the currently synthesized hydroxyl-terminated polyepichlorohydrins use small molecular polyols (such as ethylene glycol, glycerol) as chain extend...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G18/50
Inventor 郑春柏杨天博柳美华魏巍尹园张依帆邓鹏飏
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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