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Method for preparing flame-retarding PTT polyester

A polyester and copolymer flame retardant technology, applied in the field of the preparation of flame retardant PTT polyester, can solve the problems of decreased breaking strength of polyester fibers, no elimination of polyester fibers, poor effect, etc. Good effect of delaying combustion and anti-melting dripping

Active Publication Date: 2009-09-23
JIANGSU ZHONGLU TECH DEV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (3) Copolymerization method: the flame retardant is introduced into the polyester macromolecular chain as a copolymerization modification component, which is in a random copolymerization state, and the flame retardant polyester fiber and fabric are obtained by copolymerization. The flame retardant obtained by this method The flame retardancy of polyester is longer, but the effect is not good, and other properties of polyester fibers such as breaking strength are reduced due to the introduction of flame retardant components
However, the actual strength of the obtained fibers still cannot meet the requirements of practical applications, which makes it difficult to carry out the subsequent textile and fabric production processes. In addition, the impact of the addition of flame retardants on other properties of polyester fibers has not been eliminated, such as The degradation rate of polyester fiber is fast, and the droplet phenomenon is serious when burning

Method used

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  • Method for preparing flame-retarding PTT polyester
  • Method for preparing flame-retarding PTT polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] According to the preparation method of the flame-retardant PTT polyester of the present embodiment, comprises the steps:

[0031] (1), the first esterification reaction: take 18kg of purified terephthalic acid (PTA), 8.4kg of 1.3-propylene glycol (PDO) in a molar ratio of 1:1.25 into a 70L polyester reactor, and add 0.2g of zinc acetate and stir After uniformity, start to heat up and pressurize to 0.15-0.30Mpa to carry out the esterification reaction. The esterification temperature is controlled at 220-260°C. After the esterification is completed and the water is discharged, return to normal pressure.

[0032] (2), the second esterification reaction: add 1.5LPDO to cool down in the reaction kettle through (1), make the temperature in the kettle drop to 220 ℃, mix the 2-carboxyethylphenylphosphinic acid prepared in advance with The mixed slurry 1250g (2-carboxyethylphenyl phosphinic acid 850g) of PDO is added, then implement normal pressure esterification, to the end of ...

Embodiment 2

[0035] According to the preparation method of the flame-retardant PTT polyester of the present embodiment, comprises the steps:

[0036] (1), the first esterification reaction: take 18kg of purified terephthalic acid (PTA), 8.4kg of 1.3-propanediol (PDO) in a molar ratio of 1:1.25 into a 70L reactor, and add 0.2g of zinc acetate and stir evenly , start to heat up and pressurize to 0.15-0.30Mpa to carry out the esterification reaction, the esterification temperature is controlled at 220-260°C, and return to normal pressure after the esterification is completed.

[0037] (2), the second esterification reaction: add 1.5LPDO to the reaction kettle that has passed through (1) to cool down, so that the temperature in the kettle is reduced to 220 ° C, and the pre-prepared 2-carboxyethylethylphosphonic acid and PDO 1250g of mixed slurry (containing 790g of 2-carboxyethylethylphosphonic acid) was added, and then the normal pressure esterification was carried out until the esterificatio...

Embodiment 3

[0040] According to the preparation method of the flame-retardant PTT polyester of this embodiment, the difference is that in this example, the phosphorus-based copolymerized flame retardant used is 1380g of the flame retardant and 870g of PDO are made into a mixed slurry and added to the reaction kettle passing through (1), and the ethylene glycol preparation solution of the inorganic nanomaterial barium sulfate is 2.0% of the total amount of the chips. After the polymerization is complete, the pellets are cut and tested. The slice index is shown in Table 1. Slice limiting oxygen index: 29.2%.

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Abstract

The invention relates to a method for preparing a flame-retarding PPT polyester, comprising the following steps of (1) mixing 1,3-propanediol with terephthalic acid and carrying out esterification reaction; (2) adding a mixed slurry of 1,3-propanediol and phosphorus-containing copolymerization flame retardant or 1, 3-propylene glycol blending solution of the phosphorus-containing copolymerization flame retardant to carry out the esterifiction reaction, thus obtaining a second esterification outcome; and (3) carrying out a condensation polymerization of the second esterification outcome, thus obtaining the flame-retarding PTT polyester, wherein the phosphorus-containing copolymerization flame retardant has a dual-reaction functional group and the phosphorus occupies the proportion of 1.2%-8.5wt% in the polyester; after step (2) and before the condensation polymerization in step (3) is carried out, an alkyl diol blending solution of inorganic nano-material is added in the condensation polymerization system; and the adding amount of the inorganic nano-material is 0.1%-5.0wt% of that of the PTT polyester. The PTT polyester obtained by the method has the advantages of excellent and durable flame-retarding performance, high rupture strength and excellent fiber-forming performance, thermal stability and thermo-oxidative stability performance.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a preparation method of flame-retardant PTT polyester. Background technique [0002] Flame-retardant polyester fibers and flame-retardant textiles are hot spots developed in the field of chemical fibers at home and abroad in recent years. Making materials flame retardant is one of the strategic measures to reduce the incidence of fire. Both the National Bureau of Standards (NBS) and the European Chemical Industry Association have put forward flame-retardant requirements for materials in different application fields, including polyester fibers. [0003] In the prior art, the preparation of flame-retardant polyester fibers mainly contains the following three methods: [0004] (1) Post-treatment method: The fiber or fabric is impregnated and absorbed a certain amount of flame retardant during the post-treatment process. The disadvantage of this method is that the flame retardancy ...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G63/692C08K3/00C08K3/26C08K3/36C08K3/30
Inventor 边树昌
Owner JIANGSU ZHONGLU TECH DEV
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