Preparation method of flame retardant phosphorylation stuffing agent
A technology of phosphorylated fatliquor and flame retardancy, which is applied in the field of preparation of phosphorylated castor oil fatliquor, can solve problems such as poor flame retardancy, and achieve the effects of good compatibility, improved flame retardancy, and low price
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example 1
[0022] (1) Add 1.22 g of boric acid and 93.3 g of castor oil into a three-necked flask, stir evenly, add 1.87 g of concentrated sulfuric acid, gradually heat up to 70°C, condensate, reflux and heat for 3 hours to obtain product A;
[0023] (2) Add 1.3 g of methanol to product A, stir evenly, then gradually heat up, keep the reaction at a temperature of 70 ° C for 3 h, wash off the residual methanol with brine, and obtain product B;
[0024] (3) Add 14.2 g of phosphorus pentoxide to product B at 30°C, stir evenly, slowly heat up to 70°C, and keep the reaction for 3 hours to obtain product C;
[0025] (4) Add 0.933 g of sodium bentonite and 4.67 g of dimethyl methylphosphonate to product C, stir evenly, keep the reaction at 50°C for 1.5 h to obtain product D, and add 20% hydrogen to product D The sodium oxide solution was neutralized, and the pH was adjusted to 7.0 to obtain a brownish-yellow liquid, which was the prepared flame-retardant phosphorylated fatliquoring agent, numbe...
example 2
[0038] (1) Add 2.61 g of fluoroboric acid and 93.3 g of castor oil into a three-necked flask, stir evenly, add 1.87 g of concentrated sulfuric acid, gradually heat up to 85°C, and condense and reflux for 4 hours to obtain product A;
[0039] (2) Add 8.0 g of ethanolamine to product A, stir evenly, then gradually heat up, keep the reaction at a temperature of 130 ° C for 4 h, wash off the residual ethanolamine with brine, and obtain product B;
[0040] (3) Add 29.4 g of phosphoric acid to product B at 50 °C, and after stirring evenly, slowly heat up to 110 °C, and keep the reaction for 5 hours to obtain product C;
[0041] (4) Add 2.8 g of calcium bentonite and 9.33 g of dimethyl phosphite to product C, stir evenly, keep the temperature at 70 °C for 3.5 h to obtain product D, and add 20% sodium hydroxide to product D The solution was neutralized, and the pH was adjusted to 7.0 to obtain a brownish-yellow liquid, which was the prepared flame-retardant phosphorylated fatliquoring...
example 3
[0054] (1) Add 1.92 g of boric acid and 93.3 g of castor oil into a three-necked flask, stir evenly, add 1.87 g of concentrated sulfuric acid to the system, gradually heat up to 80°C, condensate and reflux for 3.5 hours, and obtain product A;
[0055] (2) 4.67 g of triethanolamine was added to product A, and the temperature was gradually increased after stirring to 100 °C for 3.5 h, and the residual triethanolamine was washed with brine to obtain product B;
[0056] (3) Add 21.8 g of phosphoric acid to product B at 50 °C, stir evenly, slowly heat up to 90 °C, and keep the reaction for 4 hours to obtain product C;
[0057] (4) Add 1.87 g of calcium bentonite and 7.0 g of diethyl phosphite to product C, stir evenly, keep the temperature at 60 °C for 2.5 h to obtain product D, and add 20% sodium hydroxide to product D The solution was neutralized, and the pH was adjusted to 7.0 to obtain a brownish-yellow liquid, which was the prepared flame-retardant phosphorylated fatliquoring ag...
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