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

Inactive Publication Date: 2017-06-09
HAITAI TEXTILE SUZHOU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of traditional liquid esters such as difficulties in storage and use, environmental pollution during the preparation process, low content of functional elements, and low molecular weight, and to prepare a product with less pollution in the preparation process, high content of functional elements, and low molecular weight. Highly solid hydroxyl-terminated organic phosphorus-nitrogen-thioester compounds

Method used

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  • 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
  • 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
  • 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

Examples

Experimental program
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Effect test

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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Abstract

The invention relates to a terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content and a preparation method thereof and flame retardant cotton fabric made from the terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content. Firstly, DAPER with terminal being hydroxyl is obtained through reaction of lateral-group phosphorous dicarboxylic acid with pentaerythritol, DADA with the terminal being the hydroxyl is obtained through reaction of organic nitrogen-dicarboxylic acid with dihydric alcohol, and finally a final product is obtained through reaction of the DAPER with the DADA. The final product is of the solid ester content with high molecular weight, the terminal of the molecule is the hydroxyl, and 12.36-13.58wt% of phosphorus, nitrogen and sulfur are contained; the ester content has the advantages of high thermal stability, wide application and the like, shortcomings that a traditional liquid ester content is difficult in storage and use, singular purpose due to simple structure, environment is polluted by preparation process and the like are overcome; the prepared ester content is taken as a flame retardant, the cotton fabric is treated through a two-dip two-rolling process, and the flame retardant cotton fabric finally obtained is good in flame retardance and washing fastness.

Description

technical field [0001] The invention belongs to the field of flame retardants, and relates to a hydroxyl-terminated organic phosphorus-nitrogen-thio ester compound and a preparation method thereof, and a flame-retardant cotton fabric prepared therefrom, in particular to a solid hydroxyl-terminated organic phosphorus-nitrogen-thio ester compound. Thioester compound and its melt condensation preparation method based on the difference in reactivity of reactants with multifunctional groups. Background technique [0002] With the development of my country's synthetic material industry and the continuous expansion of application fields, it has been widely used in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, basic necessities of life, etc. But most of them are flammable materials, which are easy to cause fire and pose a great threat to life and property safety. Therefore, the flame retar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692D06M15/507D06M101/06
CPCC08G63/6926C08G63/6924D06M15/507D06M2101/06D06M2200/30
Inventor 计虎泉孙宾承婷婷江晓泽相恒学杜亚
Owner HAITAI TEXTILE SUZHOU
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