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
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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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