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Process for preparing flame-retarding phosphorus copolymerized terylene chips

A technology for copolymerizing flame retardant and polyester chips, applied in the polyester chemical field, can solve the problems of affecting the flame retardant effect, decreasing spinnability, and high iron content in chips, achieving uniform and lasting flame retardant effect, easy production and promotion, and spinnability. good effect

Inactive Publication Date: 2002-07-24
济南齐鲁化纤集团有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The method of directly adding flame retardants can be used to prepare phosphorus-based copolymerized flame-retardant polyester chips. It has been reported that 2-carboxyethylphenylphosphoric acid is used as a copolymerized flame retardant to produce flame-retardant polyester through direct esterification. The process route is The flame retardant is directly added to the system, and this process has the following disadvantages: (1) The flame retardant production process leads to the flame retardant inevitably containing chloride ions, so the slice production equipment is corroded, the iron content in the slice is high, and the spinnability is reduced
(3) The flame retardant participates in the esterification reaction. Due to the low decomposition temperature of the flame retardant, the limit esterification temperature cannot be high, otherwise it will cause the decomposition of the flame retardant and affect the flame retardant effect
(4) Residual reducing substances in the flame retardant reduce the catalyst antimony trioxide to antimony, resulting in poor hue or even graying of the slices

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Take 100kg of EG and put it into a preparation tank, add 100kg of flame retardant 2-carboxyethylphenylphosphoric acid under stirring, and heat up to 160°C to obtain 50wt% ethylene glycol (EG) preparation solution of flame retardant.

[0025] Take 2000kg of purified terephthalic acid (PTA) and 950kg of ethylene glycol (EG) into the beating tank for beating. After beating evenly, it will be continuously entered into the esterification tank for esterification at 255°C under normal pressure. After the esterification is completed, 440kg will be transferred to the polymerization tank. , add 190kg of the above-mentioned flame retardant preparation solution, precondense in low vacuum at a temperature of 240 to 270° C., and polymerize in a high vacuum (90 Pa) at a temperature of 283° C. to obtain polyester chips. The slice index is shown in Table 1.

Embodiment 2

[0031] Example 2: Get 100kg EG and add it to the preparation tank, add 133kg of flame retardant 2-carboxyethylphenylphosphoric acid (water content 25%) under stirring, heat up to 160°C to obtain ethylene glycol (EG) modulation of 50wt% flame retardant liquid.

[0032] Take 2000kg of purified terephthalic acid (PTA) and 950kg of ethylene glycol (EG) into the beating tank for beating. Kettle, add 190kg of the above-mentioned flame retardant preparation solution, precondense polycondensation at a low vacuum temperature of 240-270°C, and polymerize polyester chips at a high vacuum (90Pa) at a temperature of 284°C.

Embodiment 3

[0033] Example 3: Get 100kg EG and add it to the preparation tank, add 83kg of flame retardant 2-carboxyethylphenylphosphoric acid (water content 25%) under stirring, heat up to 160°C to obtain ethylene glycol (EG) modulation of 40wt% flame retardant liquid.

[0034] Take 2000kg of purified terephthalic acid (PTA) and 950kg of ethylene glycol (EG) into the beating tank for beating. Add 210kg of the above-mentioned flame retardant preparation solution to the kettle, pre-condense in low vacuum at a temperature of 240-270°C, and polymerize in a high vacuum (85Pa) at a temperature of 285°C to obtain polyester chips.

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PUM

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Abstract

A flame-retarding copolymerized terylene chip is prepared on the basis of ordinary preparing process of terylene chip and is characterized by that after the esterifying step in the process to prepare polyester is finished, the flame-retarding agent, which is prepared from 2-carboxyethyl phenylphosphoric acid through dissolving it in ethylene glycol (EG), is added. Its advantages are high and durable flame-retarding effect, no toxicity and high spinnability.

Description

(1) Technical field [0001] The invention relates to a method for manufacturing flame-retardant polyester, in particular to a method for preparing phosphorus-based copolymerized flame-retardant polyester slices, and belongs to the technical field of polyester chemical industry. (2) Background technology [0002] There are two methods of flame retardant modification of polyester: blending modification and copolymerization modification. Blending modification is to add a blending flame retardant in the polyester manufacturing process to make a blended flame retardant polyester fiber or add a flame retardant to the spinning process to make a flame retardant polyester fiber. The blending method is poorly dispersed in the product due to the flame retardant , it is difficult to mix evenly with the melt, and it is easy to dissociate during spinning, resulting in difficulty in spinning, affecting the flame retardant effect of the product and the physical properties of the fiber; copol...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/78C08G63/83C08K5/521D01F1/07
Inventor 王国德王红边树昌杜章森孙砚军刘俊卿
Owner 济南齐鲁化纤集团有限责任公司
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