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Phosphorus-containing flame-retardant PTT as well as preparation method and application thereof

A flame retardant, alcohol ring triphosphazene technology, which is applied in the field of phosphorus-containing flame retardant PTT and its preparation, can solve the problems such as the viscosity not meeting the requirements, the color of polyester chip fibers being deteriorated, and the color difference of the samples, etc. The effect of reducing the degree of thermal degradation, shortening the polymerization time, and good flame retardant performance

Active Publication Date: 2019-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the content of phosphorus in polyester increases, the color of polyester chips and even fibers will deteriorate, the product will turn yellow and the b value will increase, and the color tone will be bad, which will affect the appearance, and it is difficult to meet the needs of users.
In addition, as the phosphorus content increases, it is difficult to polymerize the sample. Even if the polycondensation time is extended, the viscosity still cannot meet the requirements, and the high temperature of the polyester for a long time will also lead to a difference in the color of the sample.

Method used

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  • Phosphorus-containing flame-retardant PTT as well as preparation method and application thereof
  • Phosphorus-containing flame-retardant PTT as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add purified terephthalic acid and propylene glycol into the batch reactor at a molar ratio of 1:1.6, and add sodium acetate anti-ether agent at the same time. The amount of anti-ether agent added is based on the content of the final polyester. According to the anti-ether agent content in the polyester is 10mg / kg, add sodium acetate to carry out esterification reaction, control the esterification temperature at 230°C-250°C, and the esterification pressure at 0.1MPa-0.4MPa, when the esterification rate reaches 92%. To release the pressure, add the compound flame retardant of the flame retardant di(propylene glycol) methyl phosphate and BCP in a mass ratio of 10:90 and the catalyst tetrabutyl titanate, and the amount of the flame retardant is based on the phosphorus content in the polyester The amount of tetrabutyl titanate added is 50 mg / kg when the titanium content in the final polyester is added, the polycondensation temperature is controlled to be 250°C-270°C, and the ...

Embodiment 2

[0035]Add purified terephthalic acid and propylene glycol into the batch reactor in a molar ratio of 1:1.1, and add lithium acetate anti-ether agent at the same time. The amount of anti-ether agent added is based on the content in the final polyester. According to the anti-ether agent content in the polyester is 10mg / kg, add lithium acetate to carry out esterification reaction, control the esterification temperature at 230°C-250°C, and the esterification pressure at 0.1MPa-0.4MPa, when the esterification rate reaches 85%. Carry out pressure relief, add flame retardant propyl phosphate di(propylene glycol) ester and BCP and be the composite flame retardant of 30:70 by mass ratio and catalyzer potassium fluorotitanate, the addition amount of flame retardant is according to the phosphorus content in polyester 15000mg / kg was added, and the amount of potassium fluorotitanate added was based on the titanium content in the final polyester being 300mg / kg. The polycondensation temperatu...

Embodiment 3

[0038] Add purified terephthalic acid and propylene glycol into the batch reactor with a molar ratio of 1:2.0, and at the same time add magnesium acetate anti-ether agent. The amount of anti-ether agent added is based on the content in the final polyester. According to the anti-ether agent content in the polyester is 50mg / kg, add magnesium acetate to carry out esterification reaction, control the esterification temperature at 230°C-250°C, and the esterification pressure at 0.1MPa-0.4MPa, when the esterification rate reaches 99%. To release the pressure, add flame retardant phenyl phosphate di(propylene glycol) ester and BCP compound flame retardant with a mass ratio of 50:50 and catalyst tetraisopropyl titanate. The content is 6500mg / kg to add, and the amount of tetraisopropyl titanate added is based on the titanium content in the final polyester is 150mg / kg, and the polycondensation temperature is controlled to be 250°C-270°C, and the vacuum is ≤80Pa. The discharge time is ju...

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Abstract

The invention discloses phosphorus-containing flame-retardant PTT as well as a preparation method and application thereof. The phosphorus-containing flame-retardant PTT is mainly prepared by mixing terephthalic acid and propylene glycol, and adding a flame retardant and an auxiliary agent for polymerization, wherein the flame retardant is obtained by compounding alkyl substituted dipropylene phosphate and 2-(tert-butyl alcohol cyclotriphosphazenyl)1,3-benzenediol diglycidyl ether (BCP). The phosphorus-containing flame-retardant PTT prepared by the method provided by the invention has short polycondensation time, good product color and good flame-retardant performance; the L value of the prepared phosphorus-containing flame-retardant PTT reaches 86, the b value is within 6.8, and the polyester flame-retardant property LOI is more than or equal to 26%; and the obtained phosphorus-containing flame-retardant PTT can be widely applied to the fields of fibers and films.

Description

technical field [0001] The invention belongs to the technical field of polymer chemical industry, and in particular relates to a phosphorus-containing flame-retardant PTT and its preparation method and application. Background technique [0002] Polytrimethylene terephthalate (PTT) is a new type of semi-crystalline aromatic polyester, its performance is between polyethylene terephthalate (PET) and polybutylene terephthalate (PBT) ), it has many excellent properties of PET and PBT at the same time. Therefore, in recent years, PTT has developed rapidly at home and abroad, and the synthetic fibers, films and engineering plastics made of it have broad application prospects. But PTT fiber, like most other fibers, is flammable, easy to cause fire or spread fire. With the increasing application of PTT materials, in order to better protect people's lives and property safety, the flame retardant modification of PTT has become an important topic. People use a variety of methods to m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/85D01F6/84D01F1/07C08J5/18C08L67/02
Inventor 何胜君王金堂张金峰王余伟朱兴松
Owner CHINA PETROLEUM & CHEM CORP
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