Terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content and preparation method thereof and flame retardant cotton fabric made from terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content
A technology of terminal hydroxyl and esterification products, which is applied in the direction of flame-retardant fibers, plant fibers, textiles and papermaking, etc., can solve the problems of environmental pollution in the preparation process, difficulties in storage and use, and the content of small functional elements, so as to overcome the problems of easy migration, Conducive to environmental protection, good synergistic effect
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Embodiment 1
[0051] A method for preparing hydroxyl-terminated organic phosphorus-nitrogen-thioester compounds, the steps are as follows:
[0052] 1) The side group phosphorus-containing dicarboxylic acid and pentaerythritol are mixed with a molar ratio of 4:1, and the melt esterification reaction is carried out under the conditions of nitrogen protection and mechanical stirring. The stirring speed of the mechanical stirring is 300rpm, and the melting esterification reaction The temperature is 180°C, and the reaction time is 1 hour. After the reaction, the product is collected, dissolved, filtered and dried to obtain DAPER with a carboxyl group at the end. The structural formula of the side group phosphorus-containing dicarboxylic acid is:
[0053]
[0054] 2) Mix organic nitrogen-sulfur dicarboxylic acid and ethylene glycol at a molar ratio of 1:2, add 4-methylbenzenesulfonic acid, organic nitrogen-sulfur dicarboxylic acid and 4-methylbenzenesulfonic acid The molar ratio of the acid is...
Embodiment 2
[0066] A method for preparing hydroxyl-terminated organic phosphorus-nitrogen-thioester compounds, the steps are as follows:
[0067] 1) The side group phosphorus-containing dicarboxylic acid and pentaerythritol are mixed with a molar ratio of 4:1, and the melt esterification reaction is carried out under the conditions of nitrogen protection and mechanical stirring, and the stirring speed of the mechanical stirring is 345rpm. The temperature is 185°C, and the reaction time is 1 hour. After the reaction, the product is collected, dissolved, filtered and dried to obtain DAPER with a carboxyl group at the end. The structural formula of the side group phosphorus-containing dicarboxylic acid is:
[0068]
[0069] 2) Mix the organic nitrogen-sulfur dicarboxylic acid and propylene glycol at a molar ratio of 1:2, add 4-methylbenzenesulfonic acid, the mixture of organic nitrogen-sulfur dicarboxylic acid and 4-methylbenzenesulfonic acid The molar ratio is 1:0.01, the melt condensati...
Embodiment 3
[0081] A method for preparing hydroxyl-terminated organic phosphorus-nitrogen-thioester compounds, the steps are as follows:
[0082] 1) The side group phosphorus-containing dicarboxylic acid and pentaerythritol are mixed with a molar ratio of 4:1, and the melt esterification reaction is carried out under the conditions of nitrogen protection and mechanical stirring, and the stirring speed of the mechanical stirring is 365rpm. The temperature is 190°C, and the reaction time is 2 hours. After the reaction is completed, the product is collected, dissolved, filtered and dried to obtain DAPER with a carboxyl group at the end. The structural formula of the side group phosphorus-containing dicarboxylic acid is:
[0083]
[0084] 2) Mix organic nitrogen-sulfur dicarboxylic acid and 1,4-butanediol at a molar ratio of 1:2, add 4-methylbenzenesulfonic acid, organic nitrogen-sulfur dicarboxylic acid and 4- The molar ratio of toluenesulfonic acid is 1:0.01, the melt condensation reacti...
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