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Preparation method of fluoride-free waterproof agent

A fluorine-free water repellent and co-solvent technology, applied in liquid repellent fibers, fiber treatment, textiles and papermaking, etc., can solve problems such as incompleteness, lack of crystal plane structure, loss of waterproof performance, etc., and achieve high commercial value , Excellent durability and water resistance, environmental friendly effect

Active Publication Date: 2022-05-27
DYMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Ordinary fluorine-free waterproofing agents containing long-chain alkyl groups, because of the lack or incomplete crystal structure, will cause a certain loss of waterproof performance. When the critical surface tension is close to water, milk and other liquids, these liquids will damage the fabric. moisten

Method used

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  • Preparation method of fluoride-free waterproof agent
  • Preparation method of fluoride-free waterproof agent
  • Preparation method of fluoride-free waterproof agent

Examples

Experimental program
Comparison scheme
Effect test

Synthetic example 1

[0034] [Synthesis of (Z)-2-stearyl-2,3-dichloroacrylate (C18ClA)]

[0035] Put 105 g of deionized water into a four-necked bottle, start stirring, and then put 28.75 g (0.719 mol) of sodium hydroxide into it. When the temperature dropped to 40°C, 25 g (0.148 mol) of furochloric acid was added in batches, and the temperature was controlled at about 40-45°C to react for 3 hours. The reaction solution was cooled to 22 ° C, 37.5 mL of concentrated hydrochloric acid (36%) was added dropwise to the reaction solution, and the temperature during the dropwise addition was controlled below 30 ° C. After the dropwise addition, a large amount of solid was precipitated. After filtering, washing and drying to obtain 2. , 15.65 g of 3-dichloroacrylic acid, yield 74.52%.

[0036] Prepare to weigh 27.05g stearyl alcohol, 0.18g polymerization inhibitor, 1.86g p-toluenesulfonic acid; measure 186.30g toluene, add it to the reaction kettle, heat until stearyl alcohol is completely melted; add 14....

Synthetic example 2

[0038] [Synthesis of (Z)-2-(stearylamide)-2,3-dichloroacrylate (C18AmClA)]

[0039] Put 105.00g of deionized water into the four-necked bottle, start stirring, and then put 28.75g of sodium hydroxide into it. When the temperature dropped to 40°C, 25.00 g of furochloric acid was added in batches, and the temperature was controlled at about 40-45°C to react for 3 hours. The reaction solution was cooled to 22°C, and 37.50 mL of concentrated hydrochloric acid (36%) was added dropwise to the reaction solution. The temperature during the dropwise addition was controlled below 30°C. After the dropwise addition, a large amount of solid was precipitated. , 15.65 g of 3-dichloroacrylic acid, yield 74.52%.

[0040] Prepare to weigh 32.75g stearic acid monoethanolamide, 0.18g polymerization inhibitor, 1.86g p-toluenesulfonic acid; weigh 186.30g toluene, add it to the reaction kettle, heat until the stearic acid monoethanolamide is completely melted; add 14.09g 2,3-Dichloroacrylic acid w...

Embodiment 1

[0042] In a 500mL beaker, add 33.6g (Z)-2-stearyl-2,3-dichloroacrylate (C18ClA), 22.4g octadecyl acrylate, 1.2g glycidyl methacrylate, 101.1g deionized Water, 16.0 g of tripropylene glycol, 5.0 g of polyoxyethylene lauryl ether, and 2.0 g of octadecyl ammonium chloride were heated to 60° C., and emulsified and dispersed by ultrasonic waves for 10 minutes to obtain a pre-emulsion. The pre-emulsion was transferred to a 500 mL autoclave, and 0.2 g of dodecyl mercaptan, 0.5 g of 2,2-azobis(2-amidinopropane) dihydrochloride (hereinafter referred to as V-50) and 6.0 g of dodecyl mercaptan were added. g deionized water solution; after nitrogen replacement is carried out in the autoclave, 8.0 g of vinyl chloride is pressed into it. The reaction was carried out at 60° C. for 4 hours, and finally the temperature of the system was lowered to room temperature and filtered through a 300-mesh filter cloth to obtain a fluorine-free water repellent.

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Abstract

The invention provides a preparation method of a fluoride-free waterproof agent. The fluoride-free waterproof agent comprises 20-35% of a fluoride-free copolymer component, 2-8% of a surfactant, 2-10% of an auxiliary agent and deionized water. The fluorine-free copolymer component comprises a fluorine-free copolymer generated by polymerization in the presence of a chain transfer agent: an alpha, beta-halogenated acrylate monomer (a), a non-crosslinked (meth) acrylate comonomer (b) and a functional monomer (c); the structural formula of the non-crosslinked (methyl) acrylate comonomer is CH2 = C (R3) COOR4, R3 is H or CH3, and R4 is saturated alkyl or cyclic alkyl with the carbon atom number of 1-30; the preparation method comprises the following steps: adding a water-soluble monomer, an initiator and a substance with a boiling point lower than an emulsification temperature into a pre-emulsion, and reacting. The polymer disclosed by the invention avoids the use of a fluorine-containing acrylate monomer, is environment-friendly and has a very high commercial value.

Description

technical field [0001] The invention relates to a preparation method of a fluorine-free water repellent. Background technique [0002] At present, the most widely used water repellents on the market are fluorine-containing water repellents, which are difficult to degrade and have high bioaccumulation toxicity, so their application in textiles is severely restricted. There are quite a few fabrics finished with fluorine-containing water repellants, such as sportswear, home textiles, outdoor clothing and casual wear, etc. In actual work, only water repellency is required, and oil repellency is not required. Water-functional finishing agent treatment. In today's increasingly popular concept of ecological environmental protection, fluorine-free waterproofing agents are more easily accepted by consumers, so the development of fluorine-free waterproofing agents has become a new research hotspot. [0003] Ordinary fluorine-free water repellents containing long-chain alkyl groups h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M15/273D06M15/263C08F220/22C08F220/18C08F220/32C08F220/36
CPCD06M15/273D06M15/263C08F220/22C08F220/36D06M2200/12C08F220/1818C08F220/325
Inventor 黄尚东方伟镇
Owner DYMATIC CHEM
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