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Mercapto-terminated organic phosphorus/sulfur-containing ester and preparation method thereof, and flame-retardant polyester fiber HOY yarn prepared from ester

A flame-retardant polyester and esterification technology, which is applied in the field of flame retardants, can solve the problems of environmental pollution in 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: 2017-06-13
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. High solid type mercapto-terminated organophosphorus-thioester compound

Method used

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  • Mercapto-terminated organic phosphorus/sulfur-containing ester and preparation method thereof, and flame-retardant polyester fiber HOY yarn prepared from ester
  • Mercapto-terminated organic phosphorus/sulfur-containing ester and preparation method thereof, and flame-retardant polyester fiber HOY yarn prepared from ester
  • Mercapto-terminated organic phosphorus/sulfur-containing ester and preparation method thereof, and flame-retardant polyester fiber HOY yarn prepared from ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] A preparation method of a mercapto-terminated organic phosphorus-thioester compound, the steps are as follows:

[0054] 1) Mix the side group phosphorus-containing dicarboxylic acid and pentaerythritol in a molar ratio of 4:1, carry out the melt esterification reaction under the protection of argon and mechanical stirring, the stirring speed of the mechanical stirring is 300rpm, and the melt esterification reaction The temperature is 180°C, and the reaction time is 1h. 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:

[0055]

[0056] 2) Mix organic mercapto-containing monocarboxylic acid and ethylene glycol at a molar ratio of 1:1, add 4-methylbenzenesulfonic acid, the molar ratio of organic mercapto-containing monocarboxylic acid to 4-methylbenzenesulfonic acid is 1 : 0.01, carry out melt condensation reac...

Embodiment 2

[0068] A preparation method of a mercapto-terminated organic phosphorus-thioester compound, the steps are as follows:

[0069] 1) Mix the side group phosphorus-containing dicarboxylic acid and pentaerythritol in a molar ratio of 4:1, carry out the melt esterification reaction under the protection of argon and mechanical stirring, the stirring speed of the mechanical stirring is 300rpm, and the melt esterification reaction The temperature is 185°C, and the reaction time is 1h. 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:

[0070]

[0071] 2) Mix organic mercapto-containing monocarboxylic acid and propylene glycol at a molar ratio of 1:1, add 4-methylbenzenesulfonic acid, and the molar ratio of organic mercapto-containing monocarboxylic acid to 4-methylbenzenesulfonic acid is 1:0.01 , under the conditions of nitr...

Embodiment 3

[0083] A preparation method of a mercapto-terminated organic phosphorus-thioester compound, the steps are as follows:

[0084] 1) Mix the side group phosphorus-containing dicarboxylic acid and pentaerythritol in a molar ratio of 4:1, carry out the melt esterification reaction under the protection of argon and mechanical stirring, the stirring speed of the mechanical stirring is 350rpm, and the melt esterification reaction The temperature is 190°C, and the reaction time is 2 hours. After the reaction, the product is collected, dissolved, filtered and dried to obtain DAPER with a carboxyl group at the end, and the structural formula of the side group phosphorus-containing dicarboxylic acid is:

[0085]

[0086] 2) Mix the organic mercapto-containing monocarboxylic acid and 1,4-butanediol in a molar ratio of 1:1, add 4-methylbenzenesulfonic acid, the organic mercapto-containing monocarboxylic acid and 4-methylbenzenesulfonic acid The molar ratio is 1:0.01, and the melt condens...

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Abstract

The invention relates to a mercapto-terminated organic phosphorus / sulfur-containing ester and a preparation method thereof, and a flame-retardant polyester fiber HOY yarn prepared from the ester. The method comprises the following steps: carrying out reaction on side-group phosphorus-containing dicarboxylic acid and pentaerythritol to obtain carboxy-terminated DAPER, carrying out reaction on organic mercapto-containing monocarboxylic acid and dibasic alcohol to obtain DADA of which one terminal is mercapto and the other terminal is hydroxy, and finally, carrying out reaction on the DAPER and DADA to obtain the final product. The final product is the high-molecular-weight solid ester, and the terminal group of the molecule is carboxy or phospho; and the mercapto-terminated organic phosphorus / sulfur-containing ester contains 12.4-13.13 wt% of phosphorus and sulfur, and has the advantages of high heat stability, wide applicability and the like. The final product can be used as a flame retardant to prepare the flame-retardant polyester fiber HOY yarn by melt spinning. The limited oxygen index of the flame-retardant polyester fiber HOY yarn is greater than or equal to 34%, the filament number is 0.3-2.0dtex, and the fracture strength is greater than or equal to 3.0 cN / dtex.

Description

technical field [0001] The invention belongs to the field of flame retardants, and relates to a mercapto-terminated organic phosphorus-thio ester compound, a preparation method thereof, and a flame-retardant polyester fiber HOY yarn prepared therefrom, in particular to a solid mercapto-terminated organic phosphorus-sulfur The esterified product and its melt condensation preparation method based on the difference in the reactivity of the multifunctional groups of the reactants. 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 retardancy of p...

Claims

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Application Information

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IPC IPC(8): D01F6/92D01F1/07C08G63/692
CPCC08G63/6924D01F1/07D01F6/92
Inventor 承婷婷孙宾杜军朱美芳江晓泽周哲
Owner HAITAI TEXTILE SUZHOU