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Method for preparing flame-resisting polyester in phosphorus series

A manufacturing method and a flame-retardant technology, which are applied in the field of polymer synthesis of halogen-free flame-retardant polymer new materials, can solve the problems of many types of raw materials, many reaction steps, long process routes, etc., and achieve less types of raw materials, low cost, The effect of short process routes

Active Publication Date: 2006-11-15
SHAOXING SANLIDA TEXTILE FLAME RETARDANT NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these two methods all have the disadvantages of longer process routes, more reaction steps, too many types of raw materials, and the need for refining by-products.

Method used

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  • Method for preparing flame-resisting polyester in phosphorus series
  • Method for preparing flame-resisting polyester in phosphorus series

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. The first step is to prepare a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant:

[0027] Take 45kg of commercially available 2-carboxyethylphenylphosphoric acid containing 14.5% of phosphorus and 2% of water, and 55kg of ethylene glycol, and add them to the esterification kettle, and gradually raise the temperature to 165°C under stirring, and carry out under normal pressure conditions. Esterification reaction, properly increase the reaction temperature to 170°C before the end of the esterification, collect the distilled water to reach 7.6kg, take the reaction product to measure the acid value to control and determine the desired reaction end point, the esterification rate is 90%, filter for later use . The product is a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant, which contains ethylene glycol p...

Embodiment 2

[0031] 1. The first step is to prepare a mixed solution of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant: the method is the same as in Example 1.

[0032] 2. The second step, polymerization of flame retardant polyester:

[0033] Get 200kg of purified terephthalic acid (PTA), 185kg of ethylene glycol (EG), the esterification process conditions and operation method are the same as in Example 1, after the esterification product is moved into the polycondensation tank, add the flame retardant made in the first step and mix Liquid 20kg (wherein contains EG6.9kg) in the polymerizer, catalyzer, auxiliary agent add-on, polycondensation process condition and operating method are with embodiment 1, obtain the required flame retardant polyester chip of the present invention. The phosphorus content in the flame-retardant polyester chip was 5560 ppm.

Embodiment 3

[0035] 1. The first step is to prepare the mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant: take commercially available 2% phosphorus containing 14.5% and 2% water - 45kg of carboxyethylphenylphosphoric acid and 55kg of ethylene glycol are added to the esterification kettle, and the temperature is gradually raised to 165°C under stirring, and the esterification reaction is carried out under normal pressure conditions. 170°C, collect the distilled water to reach 6.1kg, take the reaction product to measure the acid value to control and determine the desired reaction end point, the esterification rate is 70%, and filter for later use. The product is a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol, which contains ethylene glycol propionate-based phenylphosphate 46.4%, 2 -Carboxyethylphenylphosphoric acid 14.1%, ethylene glycol ...

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Abstract

The invention relates to a method for manufacturing phosphorus-based flame-retardant polyester, which comprises the use of purified terephthalic acid, ethylene glycol, catalysts, and auxiliary agents for esterification, and adding ethylene glycol propionate before polymerization after esterification The mixture of ester group ethylene glycol phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant is polycondensed according to a conventional polycondensation process to obtain flame retardant polyester chips. The fibers and fabrics made of flame-retardant polyester chips produced by this method have good flame-retardant stability, and can keep the flame-retardant performance basically unchanged after dyeing. The flame-retardant performance LOI of curtain fabric products exceeds 32%. There are few kinds of raw materials, the process flow is simple, and the economic cost can be reduced.

Description

Technical field: [0001] The present invention relates to the technical field of a new polymer synthesis halogen-free flame-retardant polymer material, in particular to a method for manufacturing a halogen-free phosphorus-based flame-retardant copolyester with good flame-retardant stability. Background technique: [0002] With the enhancement of people's awareness of fire safety and the improvement of economic and technological level, in order to ensure the safety of people's lives and property, countries all over the world have imposed mandatory regulations on textiles and grade standards for flame-retardant textiles to varying degrees. The flame retardant performance of flame retardant textiles is mainly judged by checking the limiting oxygen index (LOI%) and damage degree of the product to judge its pros and cons. Grade" (LOI%≥32%) and "Flame Retardant B2 Grade" (32%>LOI%≥26%). [0003] There are two ways to obtain the flame retardant of textiles. One is post-treatment...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08K5/523
Inventor 李远明叶光斗
Owner SHAOXING SANLIDA TEXTILE FLAME RETARDANT NEW MATERIALS
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