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Diffluent side-chain fluorine-containing polyether diol prepared from perfluorinated ethylene oxide and multicomponent cyclic ether through copolymerization

A technology of copolyether diol and ethylene oxide, which is applied in the field of soluble side chain fluorine-containing polyether diol and its preparation, can solve the problems of rising use cost, waste of effective resources, harsh solvents, etc., and reduce processing cost , expand the use of space, and reduce pollution

Active Publication Date: 2017-08-08
孔庆刚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned various side chain fluorine-containing homopolymerization, binary copolymerization or ring-opening multi-component fluorine-containing copolymers of cyclic ether monomers all have two deficiencies in varying degrees: (1) the prepared side chain Fluorine-containing polyether polyols have certain difficulties in controlling the fluorine content; (2) the prepared side-chain fluorine-containing polyether polyols are not easily dissolved in non-toxic or low-toxic solvents that are common in industry and cheap
These two factors have led to: 1) expensive fluorine elements cannot be used to their full potential, resulting in a waste of effective resources; Difficult to dissolve and harsh on the required solvents, which leads to increased use costs and pollution to the processing environment

Method used

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  • Diffluent side-chain fluorine-containing polyether diol prepared from perfluorinated ethylene oxide and multicomponent cyclic ether through copolymerization
  • Diffluent side-chain fluorine-containing polyether diol prepared from perfluorinated ethylene oxide and multicomponent cyclic ether through copolymerization
  • Diffluent side-chain fluorine-containing polyether diol prepared from perfluorinated ethylene oxide and multicomponent cyclic ether through copolymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Dissolve 0.05 moles of 2-(heptafluorotetradecyl)oxirane and 0.95 moles of 2-methylphenyl glycidyl ether in 100 mL of dichloromethane to form a dichloromethane solution of a three-membered cyclic ether .

[0037]Then, add 5 moles of oxetane, 50 mL of dichloromethane, 0.15 moles of 98% concentrated sulfuric acid and 0.18 moles of ethylene glycol into a 1000 mL kettle, cool down to -10 ° C, stir for 20 minutes and maintain this temperature, drop Add 0.05 moles of 2-(heptafluorotetradecyl)oxirane and 0.95 moles of 2-methylphenyl glycidyl ether in dichloromethane solution, and control the dripping within 2 hours. Maintain at -10°C and react for 10 hours. Add 20ml of deionized water to terminate the reaction, distill off the solvent, and neutralize to neutral with sodium bicarbonate solution. Add 200 mL of deionized water, stir and wash with water for 20 minutes, let stand to separate layers, remove the solvent from the oil phase by rotary evaporator, and obtain crude polye...

Embodiment 2

[0039] Dissolve 0.1 mol of 2-(heptadecafluorononyl)oxirane and 0.5 mol of benzyl glycidyl ether in 200 mL of ether to form an ether solution.

[0040] In a 1000mL kettle equipped with a stirrer, after replacing the air in the kettle with pure nitrogen, cool down to -5°C and add 100mL of ether as a solvent, add 1.8 moles of oxetane, 0.072 moles of perchloric acid and 0.12 moles of butane alcohol. The ether solution formed by dissolving 0.1 moles of 2-(heptadecafluorononyl)oxirane and 0.5 moles of benzyl glycidyl ether and 200 mL of diethyl ether was added dropwise, and the controlled dropping was completed within 3 hours. Keep at -5°C, react for 8 hours, add 30ml of deionized water to terminate the reaction, distill off the solvent, and neutralize to neutral with sodium carbonate solution. Add 200 mL of deionized water to wash for 20 minutes, let stand to separate, and wash the oil phase with distilled water again, let stand to separate. The oil phase was then vacuum-dried at...

Embodiment 3

[0042] Dissolve 0.15 mol of 2-perfluoropentyl oxirane and 0.3 mol of benzyl glycidyl ether together in 250 mL of acetone to form a three-membered cyclic ether in acetone.

[0043] In a 1000 mL kettle equipped with a stirrer, after replacing the air in the kettle with pure nitrogen, cool down to -0°C and add 100 mL of acetone as a solvent, add 0.45 moles of tetrahydrofuran, 0.0225 moles of perchloric acid and 0.027 moles of butanediol. The above-mentioned acetone solution formed by dissolving 0.15 moles of 2-perfluoropentyl oxirane and 0.3 moles of benzyl glycidyl ether in 250 mL of acetone was added dropwise, and the controlled dropping was completed within 3 hours. Keep at 0°C, react for 10 hours, add 50ml of deionized water to terminate the reaction, distill off the solvent, and neutralize to neutral with ammonium carbonate aqueous solution. Add 200 mL of deionized water to wash for 20 minutes, let stand to separate, and wash the oil phase with distilled water again, let sta...

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Abstract

The invention discloses diffluent side-chain fluorine-containing polyether diol prepared from perfluorinated ethylene oxide and multicomponent cyclic ether through copolymerization. The diffluent side-chain fluorine-containing polyether diol is prepared from perfluoroalkyl substituted ethylene oxide, substituted epoxy propane and oxetane or tetrahydrofuran through copolymerization reaction. The side-chain fluorine-containing copolyether diol with different fluorine contents can be synthesized through changing the raw material proportion; the fluorine raw materials are sufficiently utilized; meanwhile, substituted epoxy propane with different substituent groups can be selected according to the subsequent reaction purposes of the side-chain fluorine-containing polyether diol; the defects of serious phase splitting and processing inconvenience in the organic fluorine compound processing process are overcome; then, the side-chain fluorine-containing polyether diol can be easily dissolved into low-price non-toxicity and low-toxicity solvents in general use in industry; the processing cost can be reduced to a great degree; the processing environment pollution is reduced. Generally, the side-chain fluorine-containing polyether diol provided by the invention is very convenient in various kinds of subsequent use; the use space of the polyether diol is expanded to a great degree.

Description

technical field [0001] The invention belongs to the technical field of intermediates of polymer materials, and specifically relates to an easily soluble side chain fluorine-containing polyether diol copolymerized by perfluorinated ethylene oxide and polycyclic ethers and a preparation method thereof. Background technique [0002] Since the element fluorine has an electronegativity of 4.0 and the atomic radius is the smallest of all elements in the periodic table except hydrogen, the carbon-fluorine bond in the fluoropolymer has a shorter bond length and a larger bond energy. This makes fluoropolymers have good chemical and thermal stability. For polymers containing perfluorinated side chains, the fluorine atoms are closely arranged along the carbon-carbon bonds of the side chains, and many perfluorinated side chains migrate to the gas-solid interface of the main chain due to incompatibility with the main chain, effectively protecting the main chain It is not directly affect...

Claims

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Application Information

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IPC IPC(8): C08G65/22C08G65/18C08G65/20
CPCC08G65/18C08G65/20C08G65/226
Inventor 孔庆刚王静施博文
Owner 孔庆刚
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