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A kind of fluorine-containing polyether diol and preparation method thereof

一种含氟聚醚、二元醇的技术，应用在含氟聚醚二元醇及其制备领域，能够解决影响聚醚链增长、很难制取高分子量聚醚等问题，达到疏水性强、良好分子链柔顺性、反应条件温和的效果

Active Publication Date: 2019-01-22
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This shows that when 1,2-propylene oxide is used to synthesize polyether, it is easy to generate unsaturated monohydroxyl ether by-products, which will affect the chain growth of polyether, so it is difficult to prepare high molecular weight polyether with basic catalysts

Method used

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  • A kind of fluorine-containing polyether diol and preparation method thereof
  • A kind of fluorine-containing polyether diol and preparation method thereof
  • A kind of fluorine-containing polyether diol and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044](1) Synthesis of nonafluorooxetane

[0045] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.1g of butyl acetate, 26.2g of sodium bicarbonate, 55.8g of sodium dithionite, 227g of N,N-dimethylformamide, 202g of water, 55.3g of perfluorobutyl iodide was added dropwise, reacted at -13°C for 3h, slowly raised to room temperature, and kept for 2h. After the reaction was completed, extraction was performed three times with 180 g of toluene. The extracts were combined and washed three times with water to obtain a solution of 4-nonafluorobutyl-3-iodobutyl acetate, which was directly put into the next step of cyclization reaction without treatment.

[0046] The above-mentioned fluorine-containing alkyl iodide butyl acetate solution was directly added into a 1000mL three-necked flask, and 310g of sodium hydroxide solution with a mass concentration of 20% was added dropwise, and kept at 12°C for 3 hours. After the ...

Embodiment 2

[0054] (1) Synthesis of nonafluorooxetane

[0055] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.0g butyl acetate, 26.6g sodium bicarbonate, 55.5g sodium dithionite, 231g N,N-dimethylformamide, 208g of water, 55.9g of perfluorobutyl iodide was added dropwise, reacted at -14°C for 3h, slowly raised to room temperature, and kept for 4h. After the reaction was finished, extract with 200 g trifluorotoluene three times. The extracts were combined and washed three times with water to obtain a solution of 4-nonafluorobutyl-3-iodobutyl acetate, which was directly put into the next step of cyclization reaction without treatment.

[0056] The above-mentioned fluorine-containing alkyl iodide butyl acetate solution was directly added into a 1000mL three-necked flask, and 385g of sodium hydroxide solution with a mass concentration of 15% was added dropwise, and kept at 12°C for 3 hours. After the reaction, the layers we...

Embodiment 3

[0062] In a 3000mL three-neck flask equipped with a thermometer, a mechanical stirrer and a constant pressure dropping funnel, add under nitrogen protection, add 565g of dichloromethane and 6.2g of 1,4-butanediol, cool to 1°C in an ice-water bath, and slowly Add 5.5 gBF 3 .Et 2 O, the temperature rises by about 6°C. After 1 hour of reaction, add 292g of 3-(1H,1H-nonafluoropentyl)oxetane and 185g of 3,3-dimethyloxetane dropwise composed of mixed monomers. The control is added for 2 hours. After the addition, the temperature was raised to 30°C, and the reaction was continued for 36h. Stop responding. Adding 102g mass concentration is 2.5% NaHCO 3 Aqueous solution, stirred and reacted for 3 hours, extracted 3 times with 1500g dichloromethane, combined the organic layers, added a desiccant anhydrous magnesium sulfate and dried for 1 hour, filtered to remove the desiccant, and evaporated the filtrate to obtain 412.2g of the product, with a yield of 86.4 %.

[0063] The numbe...

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Abstract

The invention relates to a fluorine-containing polyether diol and a preparation method thereof. The perfluoroalkyl iodide is used as a starting material, and a single-electron addition reaction is carried out with vinyl butyl acetate, and then the fluorine-containing polyether diol is prepared through a cyclization reaction. Fluoroalkyl oxetane; when fluorine-containing alkyl oxetane is copolymerized with dimethyl oxetane, since the polymerization reactivity of the two epoxy monomers is close, the fluoroalkyl group can be obtained in Polyether products with very uniform distribution on the main chain of polyether macromolecules; polyether diols with different fluorine contents are obtained by adjusting the proportion of comonomers, which is conducive to the preparation of fluorine-containing polymer products with various properties; by adding non-fluorine-containing oxygen heterocycles Cyclobutane monomer copolymerization reduces the production cost of fluorine-containing polyether products. When the side group type fluorine-containing alkyl polyether glycol provided by the present invention is used for preparing polymer materials, the side chain fluoroalkyl group can provide strong hydrophobicity; meanwhile, the preparation process of the provided fluorine-containing polyether glycol is simple and convenient , the reaction conditions are mild, the production only needs conventional equipment, and it is suitable for industrial production.

Description

technical field [0001] The invention relates to a fluorine-containing polyether diol and a preparation method thereof, belonging to the fields of fine chemical synthesis and polymer materials. Background technique [0002] Polyether polyol is the key raw material for the synthesis of polyurethane, which is prepared by ring-opening polymerization of epoxy compounds. Commonly used epoxy compounds are ethylene oxide, propylene oxide, oxetane and tetrahydrofuran. A homopolyether synthesized from an epoxy compound monomer is called a homopolyether, and a copolyether can be obtained by copolymerizing two epoxy compounds. [0003] Polyoxyethylene (also known as polyoxyethylene ether) is obtained by polymerizing ethylene oxide as a raw material in the presence of water and an alkali catalyst. In the presence of a basic catalyst, propylene oxide is polymerized to produce polyoxypropylene, and the terminal hydroxyl group of the product is a secondary hydroxyl group, and its reactivi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/22C08G18/50
CPCC08G18/5015C08G65/226C08G65/2639
Inventor 李战雄戴礼
Owner SUZHOU UNIV
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