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Terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content and preparation method thereof and flame-retardant polyester fiber POY(polyester pre-oriented yarn) made from terminal-hydroxyl organic phosphorus-nitrogen ester content

A flame-retardant polyester and esterification technology, which is applied in the field of flame retardants, can solve the problems of environmental pollution during the preparation process, difficulties in storage and use, and low content of functional elements, so as to overcome easy migration, be beneficial to environmental protection, and have a simple method Effect

Active 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 mercapto-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 polyester fiber POY(polyester pre-oriented yarn) made from terminal-hydroxyl organic phosphorus-nitrogen ester content
  • Terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content and preparation method thereof and flame-retardant polyester fiber POY(polyester pre-oriented yarn) made from terminal-hydroxyl organic phosphorus-nitrogen ester content
  • Terminal-hydroxyl organic phosphorus-nitrogen-sulphur ester content and preparation method thereof and flame-retardant polyester fiber POY(polyester pre-oriented yarn) made from terminal-hydroxyl organic phosphorus-nitrogen ester content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A method for preparing a mercapto-terminated organic phosphorus-nitrogen-thioester compound, the steps are as follows:

[0053] 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:

[0054]

[0055] 2) Mix the thiol-terminated nitrogen-containing monocarboxylic acid and ethylene glycol at a molar ratio of 1:1, add 4-methylbenzenesulfonic acid, the molar ratio of the mercapto-terminal nitrogen-containing monocarboxylic acid to 4-...

Embodiment 2

[0067] A method for preparing a mercapto-terminated organic phosphorus-nitrogen-thioester compound, the steps are as follows:

[0068] 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 336rpm. 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:

[0069]

[0070] 2) Mix the mercapto-terminated nitrogen-containing monocarboxylic acid and propylene glycol at a molar ratio of 1:1, add 4-methylbenzenesulfonic acid, and the molar ratio of the mercapto-terminal nitrogen-containing monocarboxylic acid to 4-methylbenzenesulfonic acid i...

Embodiment 3

[0082] A method for preparing a mercapto-terminated organic phosphorus-nitrogen-thioester compound, the steps are as follows:

[0083] 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 188°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:

[0084]

[0085] 2) Mix thiol-terminated nitrogen-containing monocarboxylic acid and 1,4-butanediol at a molar ratio of 1:1, add 4-methylbenzenesulfonic acid, mercapto-terminated nitrogen-containing monocarboxylic acid and 4-methylbenzenesulfonic acid The molar ratio of the acid is 1:...

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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 polyester fiber POY(polyester pre-oriented yarn) 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, then DADA with one end being sulfydryl while is obtained through reaction of terminal-hydroxyl nitrogen contained monocarboxylic 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 molecular is the hydroxyl, 15.1-16.04wt% of phosphorus, nitrogen and sulphur are contained, and the ester content has the advantages of high thermal stability, wide application and the like; the final product is taken as a flame retardant to prepare the flame-retardant polyester fiber PLY, limit oxygen index of the flame-retardant polyester fiber POY is greater than or equal to 38%, filament number is from 0.3dtex to 1.0dtex, and breaking strength is greater than or equal to 2.1cN / dtex.

Description

technical field [0001] The invention belongs to the field of flame retardants, and relates to a mercapto-terminated organic phosphorus-nitrogen-thio ester compound, a preparation method thereof, and a flame-retardant polyester fiber POY yarn prepared therefrom, in particular to a solid mercapto-terminated organic phosphorus-containing -Nitrogen-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 retard...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C09K21/12D01F6/92D01F1/07
CPCC07F9/657172C09K21/12D01F1/07D01F6/92
Inventor 滕伟孙宾杜军朱美芳周哲李剑峰
Owner HAITAI TEXTILE SUZHOU
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