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Preparation method of copolyether containing fluoroalkyl

A technology of fluorine-containing alkyl copolyether and alkyl copolyether, which is applied in the field of fine chemical synthesis technology and polymer materials, and can solve problems such as inability to prevent water and oil, low fluorine content of fluorine-containing groups, and insufficient surface energy. problems, to achieve good appearance, easy surface properties, and good comprehensive mechanical properties

Active Publication Date: 2018-10-26
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Or use perfluoroether small molecule diols such as hexafluoropentanediol polyether as raw materials, which are used to prepare fluorine-containing polyurethanes so that polyether segments enter polyurethanes with soft segments, and the product has good flexibility; however, these fluorine-containing polyurethanes Due to the low fluorine content of the fluorine-containing groups used, the surface energy provided is not low enough to perform the function of water and oil repellency

Method used

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  • Preparation method of copolyether containing fluoroalkyl
  • Preparation method of copolyether containing fluoroalkyl
  • Preparation method of copolyether containing fluoroalkyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) One-pot preparation of fluorine-containing alkyl epoxy monomers

[0055] a. Synthesis of nonafluorooxetane

[0056] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.5g of enbutyl acetate, 26.6g of sodium bicarbonate (NaHCO 3 ), 55.0g sodium dithionite, 220g N,N-dimethylformamide, 210g water, 55.4g perfluorobutyl iodide was added dropwise, reacted at -15°C for 3h, slowly raised to room temperature, and kept for 2h. After the reaction was completed, extraction was performed three times with 150 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.

[0057] The above-mentioned fluorine-containing alkyl iodide butyl acetate solution was directly added into a 1000 mL three-neck flask, 305 g of sodium hydroxide solution with a mass concent...

Embodiment 2

[0073] (1) One-pot preparation of fluorine-containing alkyl epoxy monomers

[0074] a. Synthesis of nonafluorooxetane

[0075] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 15.9g of butyl acetate, 27.1g of sodium bicarbonate, 55.3g of sodium dithionite, 218g of N,N-dimethylformamide, 209g of water, 54.9g of perfluorobutyl iodide was added dropwise, reacted at -12°C for 3h, slowly raised to room temperature, and kept for 3h. After the reaction was finished, extract with 165g trifluorotoluene in 3 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.

[0076] The above-mentioned fluorine-containing alkyl iodide butyl acetate solution was directly added into a 1000mL three-neck flask, and 310g of sodium hydroxide solution with a mass concentration of 20%...

Embodiment 3

[0091] (1) One-pot preparation of fluorine-containing alkyl epoxy monomers

[0092] a. Tridecafluorooxetane Synthesis

[0093] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.8g of butyl acetate, 27.9g of sodium bicarbonate, 54.8g of sodium dithionite, 235g of N,N-dimethylformamide, 230g of water, 72.6g of perfluorohexyl iodide was added dropwise, reacted at -14°C for 5h, slowly raised to room temperature, and kept for 6h. After the reaction was finished, extract with 188g trifluorotoluene three times. The extracts were combined and washed three times with water to obtain a solution of 4-tridecafluorohexyl-3-iodobutyl acetate, which was directly put into the next step of cyclization reaction without any treatment.

[0094] The above-mentioned fluorine-containing alkyl iodide butyl acetate solution was directly added into a 1000mL three-necked flask, and 511g of sodium hydroxide solution with a mass concentrat...

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Abstract

The invention relates to a preparation method of fluoroalkyl-containing copolyether. The preparation method comprises the following steps: taking perfluoroalkyl iodide and allyl acetate and butenyl acetate to be subjected to single electron transfer reaction and cyclization reaction respectively to prepare two epoxy monomers including fluoroalkyl-containing ethylene oxide and fluoroalkyl-containing trimethylene oxide; then carrying out ring-opening copolymerization on the two monomers under the catalysis of Lewis acid to obtain the fluoroalkyl-containing copolyether. A side group of the fluoroalkyl-containing copolyether provided by the invention is fluoroalkyl and good hydrophobicity can be provided. Alternative structure characteristics of two different chain sections of the copolyetherprovide good molecular flexibility and a product is not easy to crystallize and has a low melting point; meanwhile, a trimethylene oxide chain section exists so that the copolyether has good hydrophobicity. Synthesis reaction of the copolyether has moderate conditions and a technology is simple; the copolyether can be synthesized by conventional equipment so that the preparation method is suitablefor industrialized production.

Description

[0001] The present invention belongs to a divisional application with the invention name of a fluorine-containing alkyl copolyether and its preparation method, application number 201611173219.7, and application date of December 18, 2016, and belongs to the preparation method part. technical field [0002] The invention relates to a preparation method of fluorine-containing alkyl copolyether, belonging to the fields of fine chemical synthesis technology and polymer materials. Background technique [0003] Polyurethane has superior mechanical properties, good adhesive properties, and excellent weather resistance, electrical properties and other advantages. Because of this, polyurethane has been widely used in adhesives, paint inks, coatings, plastics and elastomers, and fibers. Polyurethane is generally formed by the addition polymerization of polymer polyols and diisocyanates. According to the different types of polymer polyols and diisocyanates, polyurethane varieties with r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/22C08G18/50C09D175/08C09D5/16C07C41/02C07C43/11
CPCC07C41/02C08G18/5015C08G65/226C09D5/1662C09D175/08C07C43/11
Inventor 李战雄王蕾童德进王海朋
Owner SUZHOU UNIV
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