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Fluorine-containing epoxide resin reactive diluent and preparation thereof

An epoxy resin reactive diluent and fluorine-containing alcohol technology, applied in the diluent field, can solve the problems of excessive epichlorohydrin recovery process, incomplete penetration, poor flame retardancy, etc., improve comprehensive performance, and facilitate closed-loop , the effect of improving characteristics

Inactive Publication Date: 2009-01-28
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the general reactive diluent can basically meet the requirements of reducing the viscosity of epoxy resin and improving the processability, but there are certain problems when used under high-demand conditions, such as poor weather resistance, incomplete penetration, and low temperature resistance. , poor flame retardancy and other disadvantages
It has been reported that tetrafluoropropanol directly synthesizes glycidyl ether and its preparation method: the molar ratio of epichlorohydrin / tetrafluoropropanol is 6:1; the molar ratio of sodium hydroxide / tetrafluoropropanol is 1.05: 1; The reaction temperature is 70 degrees, and the reaction time is 5 hours, but there are problems such as excessive epichlorohydrin recovery process and low epoxy value

Method used

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  • Fluorine-containing epoxide resin reactive diluent and preparation thereof
  • Fluorine-containing epoxide resin reactive diluent and preparation thereof
  • Fluorine-containing epoxide resin reactive diluent and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In a 5000ml three-necked flask equipped with an oil bath heating device, a stirrer, a thermometer, and a condenser, add 3000g of tetrafluoropropanol, start stirring, raise the temperature of the oil bath to 110°C, collect the transparent fraction above 100°C, and seal it for future use .

[0047] In a 2000ml four-neck flask equipped with a water bath heating device, a stirrer, a thermometer, a condenser, and a balance funnel, add 200g of tetrafluoropropanol and 2g of boron trifluoride ether. The temperature of the system was controlled at 60° C., and 200 g of 1-chloro-2,3-propylene oxide was added dropwise through a balance funnel for etherification reaction, and the reaction time was 4 hours. During the dropping process, constantly observe the temperature change of the system, and take appropriate cooling measures. Add 85g of flake NaOH in portions through the feeding port, and the separation time is 20 minutes. The reaction time is 6h, and the temperature is 30°C. ...

Embodiment 2

[0050] In a 5000ml three-necked flask equipped with an oil bath heating device, a stirrer, a thermometer, and a condenser, add 3000g of tetrafluoropropanol, start stirring, raise the temperature of the oil bath to 110°C, collect the transparent fraction above 100°C, and seal it for future use .

[0051] In a 2000ml four-necked flask equipped with a water bath heating device, a stirrer, a thermometer, a condenser, and a balance funnel, add 200g of tetrafluoropropanol and boron trifluoride ether SnCl 4 2g. The temperature of the system was controlled at 100° C., and 225 g of 1-chloro-2,3-propylene oxide was added dropwise through a balance funnel for etherification reaction, and the reaction time was 2 hours. During the dropping process, constantly observe the temperature change of the system, and take appropriate cooling measures. Then add 85 g of flaky KOH in portions through the feeding port, with an interval of 20 minutes. The reaction time is 2h, and the temperature is 2...

Embodiment 3

[0054] In a 5000ml three-necked flask equipped with an oil bath heating device, a stirrer, a thermometer, and a condenser, add 3000g of tetrafluoropropanol, start stirring, raise the temperature of the oil bath to 110°C, collect the transparent fraction above 100°C, and seal it for future use .

[0055] In a 2000ml four-neck flask equipped with a water bath heating device, a stirrer, a thermometer, a condenser, and a balance funnel, add 200g of tetrafluoropropanol and 1g of boron trifluoride ether. The temperature of the system was controlled at 30° C., and 200 g of 1-chloro-2,3-propylene oxide was added dropwise through a balance funnel for etherification reaction, and the reaction time was 8 hours. During the dropping process, constantly observe the temperature change of the system, and take appropriate cooling measures. Then add 100 g of flaky NaOH in portions through the feeding port, with an interval of 20 minutes. The reaction time is 2h, and the temperature is 50°C. ...

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Abstract

The invention provides a novel reactive diluent of a fluoro-epoxy resin and a preparation method thereof. In the invention, fluoro-alcohol and epihalohydrin are adopted as the materials; Lewis acid is used as a catalyst for carrying out a ring-opening etherification; then alkaline matter is added for carrying out a ring-closing reaction; after the post-treatment techniques of washing, filtering and solvent removing, etc., the novel reactive diluent of the fluoro-epoxy resin is obtained. The diluent provided by the invention has no thrill taste; the diluting effect is better than common reactive diluents; in addition, the reactive diluent can effectively improve the defects of poor weatherability, incomplete penetration, poor fire resistance and being incapable of resisting high temperature; the reactive diluent has the advantages of innocuity, non-corrosiveness, convenient operation, and safe use, etc.

Description

technical field [0001] The invention relates to a diluent, in particular to a novel reactive diluent for fluorine-containing epoxy resin and a preparation method thereof. Background technique [0002] Epoxy resin reactive diluent is mainly used to improve and adjust the flow characteristics of epoxy resin, strengthen the construction and operability, the main species are alcohol glycidyl ethers, for example, n-butyl glycidyl ether 501, phenyl glycidyl ether 690 , Mixed cresol glycidyl ether X-52, ethylene glycol diglycidyl ether, etc. At present, the general reactive diluent can basically meet the requirements of reducing the viscosity of epoxy resin and improving the processability, but there are certain problems when used under high-demand conditions, such as poor weather resistance, incomplete penetration, and low temperature resistance. , poor flame retardancy and other shortcomings. It has been reported that tetrafluoropropanol directly synthesizes glycidyl ether and ...

Claims

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Application Information

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IPC IPC(8): C07D301/27C07D303/22C08G59/18
Inventor 刘守贵宋尚林
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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