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Synthesis method of hydroxyl terminated polyether for cultural relic adhesive

A technology of hydroxyl-terminated polyether and synthesis method, applied in the direction of polyurea/polyurethane coatings, coatings, etc., can solve the problems of difficult catalyst recovery, environmental pollution, toxic substances, etc., and achieves rich raw materials, good effects, and easy production and preparation. Effect

Inactive Publication Date: 2019-02-15
郑州博物馆 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In view of the above situation, in order to overcome the defects of the prior art, the object of the present invention is to provide a synthetic method for hydroxyl-terminated polyether used in cultural relic adhesives, which can effectively solve the problem of toxic substances, Environmental pollution, difficulty in catalyst recovery and high cost

Method used

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  • Synthesis method of hydroxyl terminated polyether for cultural relic adhesive
  • Synthesis method of hydroxyl terminated polyether for cultural relic adhesive

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Experimental program
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Effect test

Embodiment 1

[0008] Embodiment 1: A method for synthesizing a hydroxyl-terminated polyether used as an adhesive for cultural relics according to the present invention. Specifically, 5 g of loaded anhydrous aluminum chloride catalyst is weighed and added to a three-necked flask, and then 20 ml of dihydrogen chloride is added to the flask. Chloromethane solvent, place the three-necked flask in a low-temperature liquid circulation pump, when the temperature drops below 5°C, add 40ml of cyclohexane epoxy into the three-necked flask dropwise, after the addition is complete, add 1g of chain extender to the three-necked flask Glycerol, the reaction temperature is 10°C, react for 3 hours, add 20ml of distilled water into the three-necked flask, stop the reaction, wash, and distill under reduced pressure to obtain the homopolyether of hydroxyl-terminated polyether.

Embodiment 2

[0009] Embodiment 2: A method for synthesizing a hydroxyl-terminated polyether used as an adhesive for cultural relics according to the present invention, specifically, take 8g of loaded anhydrous aluminum chloride catalyst, add it to a three-necked flask, and then add 25ml dihydrogen chloride to the flask. Chloromethane solvent, place the three-necked flask in the low-temperature liquid circulation pump, when the temperature drops below 5°C, add 50ml of the mixed solution of epoxycyclohexane and tetrahydrofuran in a molar ratio of 1:1 into the three-necked flask dropwise, After the dropwise addition, add 2g of chain extender glycerol to the three-necked flask, and react at 15°C for 8 hours. Add 20ml of distilled water to the three-necked flask to terminate the reaction, wash, and distill under reduced pressure to obtain the ring of hydroxyl-terminated polyether. Oxycyclohexane-tetrahydrofuran copolyether.

Embodiment 3

[0010] Embodiment 3: A method for synthesizing a hydroxyl-terminated polyether used as an adhesive for cultural relics according to the present invention. Specifically, 10 g of loaded anhydrous aluminum chloride catalyst is weighed and added to a three-necked flask, and then 30 ml of dihydrogen chloride is added to the flask. Chloromethane solvent, place the three-necked flask in a low-temperature liquid circulation pump, and when the temperature drops below 5°C, add 60ml of a mixed solution of epoxycyclohexane and epichlorohydrin at a molar ratio of 1:1 to the three-necked flask dropwise. In the flask, after the dropwise addition, add 4g of chain extender glycerin into the three-necked flask, react at 20°C, react for 12h, add 20ml of distilled water into the three-necked flask, terminate the reaction, wash, and distill under reduced pressure to obtain hydroxyl-terminated poly Ether epoxy cyclohexane - epichlorohydrin copolyether.

[0011] Taking epichlorohydrin as an example,...

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Abstract

The invention aims to provide a synthesis method of hydroxyl terminated polyether for a cultural relic adhesive. Hydroxyl terminated polyether containing the cyclohexane ring is synthesized by catalysis from supported anhydrous aluminium chloride as a catalyst and glycerin as a promoter and a chain extender. The method is simple, environmentally friendly, safe and good in effect, the raw materialsare abundant, production and preparation are easy, the problems of production of toxic and harmful substances, environmental pollution and high cost of an existing polyether polyol synthesis processcan be effectively solved, and the method is innovative in polyether polyol synthesis and has great economic and social benefits.

Description

technical field [0001] The invention relates to chemical industry, in particular to a method for synthesizing a hydroxyl-terminated polyether used for adhesives for cultural relics, which is catalyzed by supported anhydrous aluminum chloride and contains a cyclohexane ring. Background technique [0002] Polyether polyol is an important fine chemical product, which is mainly used in the production of polyurethane coatings, elastomers, cultural relic adhesives and other products. At present, in the synthesis process of polyether polyol, the ring-opening catalyst of epoxycyclohexane Boron trifluoride ether is mostly boron trifluoride ether, and boron trifluoride ether has strong toxicity and hazards, causing harm to personnel and polluting the environment. Boron trifluoride ether is a liquid catalyst, which is difficult to recycle, not recyclable, and high in cost. Therefore, improvement and innovation in its preparation method is imperative. Contents of the invention [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C09D175/08
CPCC08G65/2609C08G65/2654C09D175/08
Inventor 金姗姗李华李振兴邵帅李建文
Owner 郑州博物馆
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