A water-repellent finishing solution for textiles based on fluorine-containing polyurethane, its preparation method and application

A technology of water-repellent finishing liquid and fluorine-containing alkyl polyurethane, which is applied in the fields of textiles and papermaking, fiber treatment, and liquid-repellent fibers, etc. , Introducing fluoroalkyl and other issues to achieve excellent water repellency, high fluorine content, and mild reaction conditions

Active Publication Date: 2019-07-09
NANTONG TEXTILE & SILK IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the lack of fluoroalkylated monomers for the synthesis of polymeric diols, it is difficult to obtain side-group fluoropolymer diols; there are many ideas for polyurethane fluoroalkylation through diisocyanate fluoroalkylation Problems, such as diisocyanate due to its small molecular weight, it is difficult to introduce a lot of fluoroalkyl groups on polyurethane macromolecules even if they are fluoroalkylated

Method used

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  • A water-repellent finishing solution for textiles based on fluorine-containing polyurethane, its preparation method and application
  • A water-repellent finishing solution for textiles based on fluorine-containing polyurethane, its preparation method and application
  • A water-repellent finishing solution for textiles based on fluorine-containing polyurethane, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Synthesis of fluorine-containing alkyl epoxy monomer

[0035] a. Synthesis of nonafluorooxetane

[0036] 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, washed 3 times with water to obtain a 4-nonafluorobutyl-3-iodobutyl acetate solution, which was added to a 1000mL three-necked flask, and 305g of a mass concentration was added dropwise to a 20% sodium hydroxide solution. Insulate and react at 15°C for 3h. After the reaction, the layers were separated. The organic layer was washed three times with water, dried and distilled unde...

Embodiment 2

[0058] (1) Synthesis of fluorine-containing alkyl epoxy monomer

[0059] a. Synthesis of nonafluorooxetane

[0060] In a 1000mL three-necked flask equipped with a thermometer, ice-water bath and magnetic stirrer protection, add 16.8g of enbutyl acetate, 27.2g of sodium bicarbonate (NaHCO 3 ), 55.6g sodium dithionite, 225g N,N-dimethylformamide, 200g water, add 55.8g perfluorobutyl iodide dropwise, react at -13°C for 3h, slowly rise to room temperature, and keep warm for 4h. After the reaction was completed, extraction was performed three times with 160 g of toluene. The extracts were combined, washed 3 times with water to obtain a 4-nonafluorobutyl-3-iodobutyl acetate solution, which was added to a 1000mL three-necked flask, and 312g of a mass concentration was added dropwise to a 15% sodium hydroxide solution. Insulate and react at 12°C for 4h. After the reaction, the layers were separated. The organic layer was washed three times with water, dried and distilled under red...

Embodiment 3

[0082] (1) Synthesis of fluorine-containing alkyl epoxy monomer

[0083] a. Tridecafluorooxetane Synthesis

[0084]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, washed 3 times with water to obtain a 4-tridecafluorohexyl-3-iodobutyl acetate solution, which was directly added to a 1000mL three-necked flask, and 511g of a mass concentration of 10% sodium hydroxide solution was added dropwise , kept at 15°C for 6h. After the reaction, the layers were separated. The organic layer was washed three times with water, dried and distilled under reduced pressure...

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Abstract

Disclosed in the present invention is a textile water-repellent finishing liquid based on fluorine-containing polyurethane, a preparation method therefor, and a use thereof. The preparation method comprises: adding a non-ionic surfactant and a cationic surfactant into a de-ionized water, slowly adding dropwise a fluoroalkyl-containing polyurethane solution, and further stirring at a high speed to obtain a uniform finishing liquid; and carrying out an addition polymerization reaction on the fluoroalkyl-containing polyurethane with fluoroalkyl-containing copolyether glycol and diisocyanate in the presence of a fluorine-containing solubilizing agent. Due to the structure of a fluoroalkyl lateral-group type polyether block, the fluorine-containing polyurethane has high fluorine content, and thus surface energy is low. The polyurethane is emulsified to prepare the finishing liquid which is used for finishing the textile and has a water contact angle of greater than 139.5 degrees; and the finishing liquid has excellent water-repellent function.

Description

technical field [0001] The invention relates to a polyurethane finishing solution, in particular to a textile water-repellent finishing solution based on fluorine-containing polyurethane, a preparation method and application thereof, and belongs to the field of polyurethane polymers and textile finishing auxiliaries. Background technique [0002] The surface free energy of polymer solids (γ c ) is related to the elements of its surface composition. The introduction of fluorine atoms significantly reduces the surface free energy, and the more fluorine atoms are substituted, the more obvious the effect of reducing the surface free energy is. If fluorine atoms are introduced into the surface of fabric fibers, so that when the concentration of fluorine atoms on the surface of the fabric reaches a certain level, the critical surface tension of the fibers will be greatly reduced, and when the critical surface tension is reduced to the point where water and oil cannot spread by th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/66C08G18/50C08G18/10C08G18/32D06M15/576D06M101/06
CPCC08G18/10C08G18/5015D06M15/576D06M2101/06D06M2200/12
Inventor 李战雄陈蕾遇娜刘群
Owner NANTONG TEXTILE & SILK IND TECH RES INST
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