A kind of phosphorus-containing flame-retardant polyester and its preparation method and application

A technology of flame-retardant polyester and polyester, applied in the field of phosphorus-containing flame-retardant polyester and its preparation, can solve the problems of the viscosity not meeting the requirements, the yellowing of the product, the increase of the b value of the product, the color difference of the sample, etc. Degradation degree, shortened polymerization time, good flame retardant performance

Active Publication Date: 2021-07-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the increase of phosphorus content in polyester, 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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  • A kind of phosphorus-containing flame-retardant polyester and its preparation method and application
  • A kind of phosphorus-containing flame-retardant polyester and its preparation method and application
  • A kind of phosphorus-containing flame-retardant polyester and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Purified terephthalic acid and ethylene glycol are beaten in a molar ratio of 1:1.1, and the anti-ether agent and catalyst are added according to the content of the final polyester, and the content of the anti-ether agent in the polyester is 20mg / kg Add sodium acetate and ethylene glycol antimony with an antimony content of 250mg / kg, add the slurry to a batch reactor for esterification, control the esterification temperature at 230°C-250°C, and the esterification pressure at 0.1MPa-0.3 MPa, when the esterification rate is 85%, the pressure is released, and the flame retardant methyl phosphate di(ethylene glycol) ester and BCP are added in a compound flame retardant with a mass ratio of 10:90, and the flame retardant addition is according to The phosphorus content in the polyester is added at 6500mg / kg, the polycondensation temperature is controlled at 260°C-280°C, the vacuum is ≤80Pa, the discharge time is judged by the change value of the stirring current, and the viscos...

Embodiment 2

[0038] Purified terephthalic acid and ethylene glycol are beaten in a molar ratio of 1:1.8, and the anti-ether agent and catalyst are added according to the content of the final polyester, and the content of the anti-ether agent in the polyester is 10mg / kg Add sodium acetate and ethylene glycol antimony with an antimony content of 200mg / kg, add the slurry to a batch reactor for esterification, control the esterification temperature at 230°C-260°C, and the esterification pressure at 0.1MPa-0.4 MPa, when the esterification rate is 99%, the pressure is released, and the flame retardant phenyl phosphate di(ethylene glycol) ester and BCP are added in a compound flame retardant with a mass ratio of 40:60, and the flame retardant addition is according to The phosphorus content in the polyester is added at 15000mg / kg, the polycondensation temperature is controlled at 260°C-285°C, the vacuum is ≤80Pa, the discharge time is judged by the change value of the stirring current, and the visc...

Embodiment 3

[0041] Purified terephthalic acid and ethylene glycol are beaten in a molar ratio of 1:1.3, and the anti-ether agent and catalyst are added according to the content of the final polyester, and the content of the anti-ether agent in the polyester is 80mg / kg Add sodium acetate and ethylene glycol antimony with an antimony content of 300mg / kg, add the slurry to a batch reactor for esterification, control the esterification temperature at 240°C-260°C, and the esterification pressure at 0.2MPa-0.4 MPa, when the esterification rate reaches 92%, the pressure is released, and the flame retardant ethyl phosphate di(ethylene glycol) ester and BCP are added in a compound flame retardant with a mass ratio of 70:30, and the flame retardant addition is as follows: The phosphorus content in the polyester is added at 9000mg / kg, the polycondensation temperature is controlled at 270°C-280°C, the vacuum is ≤80Pa, the discharge time is judged by the change value of the stirring current, and the vi...

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Abstract

The invention discloses a phosphorus-containing flame-retardant polyester and its preparation method and application. The flame-retardant polyester is mainly prepared by mixing terephthalic acid and ethylene glycol, and adding auxiliary agents and flame retardants for polymerization; The flame retardant is a flame retardant compounded by alkyl substituted diethylene glycol phosphate and 2-(tert-butanol cyclotriphosphazene) 1,3-benzenediol diglycidyl ether (BCP). The flame retardant polyester prepared by the present invention has short polycondensation time, good product hue, and good flame retardant performance. The L value of the prepared polyester reaches 85, the b value is within 3, and the flame retardant performance of the sample is LOI ≥ 29%; the obtained polyester Widely used in the field of fiber and film, the polyester can be added as a masterbatch or directly used to prepare fibers and films. Fibers prepared from the polyester are used in industrial textiles, architectural interior decoration materials, vehicle interior decoration materials, protective clothing, carpets, etc.; compared with conventional similar polyester films, the films prepared from the polyester have lower Haze and good flame retardant properties.

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 polyester and its preparation method and application. Background technique [0002] Polyethylene terephthalate (PET) is a polyester with excellent performance, which has the advantages of good thermal and chemical stability, high mechanical strength, low gas permeability, and good spinnability. Its output is world-wide The largest and most versatile, it is widely used in the fields of fibers, films and bottle flakes. Because the polyester fiber has good mechanical strength and tensile properties, it is widely used in clothing, industry, transportation, and decorative materials. [0003] Due to the flammability of PET, its application in the field of flame retardancy is greatly limited, such as indoor and outdoor decoration materials such as hotels and restaurants, transportation, aviation, hospitals and superm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/692C08G63/78C08L67/02C08J5/18D01F6/84D01F1/07
CPCC08G63/6926C08G63/78C08J5/18C08J2367/02D01F1/07D01F6/84
Inventor 王金堂张金峰王余伟朱兴松刘峰
Owner CHINA PETROLEUM & CHEM CORP
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