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Method for preparing polyester polyol by recovering white mud and/or PET (Polyethylene Terephthalate)

A polyester polyol and white mud technology, applied in chemical instruments and methods, separation methods, plastic recycling, etc., can solve the problem of difficulty in obtaining satisfactory recycling efficiency and economic benefits, a large number of secondary three waste pollutants, and the quality of terephthalic acid. Low problems, to achieve the effect of reducing the probability of entering the filtrate, improving the hue and quality, and reducing the probability of agglomeration

Pending Publication Date: 2022-06-28
李安琪 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the recycling methods currently used are physical and mechanical methods such as melting and granulation, which have two disadvantages: 1. The workshop-style melting and granulation produces a large amount of secondary three waste pollutants, which has a great impact on the surrounding environment
2. The performance of products regenerated by simple physical methods is extremely poor, and the value of reuse is completely lost after the first use
[0005] Because white mud is rich in terephthalic acid (TA) and has a high recovery value, many research institutes and related companies at home and abroad have developed a variety of recovery methods, but the quality of recovered terephthalic acid is low and the utilization value is not high. Generally, it can only be used as a low-quality terephthalic acid raw material for the production of low-end polyester coatings, unsaturated resins, plasticizers, fireworks flute agents, etc., and it is difficult to obtain satisfactory recovery efficiency and economic benefits

Method used

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  • Method for preparing polyester polyol by recovering white mud and/or PET (Polyethylene Terephthalate)
  • Method for preparing polyester polyol by recovering white mud and/or PET (Polyethylene Terephthalate)
  • Method for preparing polyester polyol by recovering white mud and/or PET (Polyethylene Terephthalate)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] A method for recovering white mud and / or PET to prepare polyester polyol, the preparation steps comprising:

[0051] The PET recovered in S1 is subjected to crushing, alkali washing, water washing, filtration and drying; the recovered PET is mixed with diethylene glycol, an alcoholysis catalyst is added, and at the same time, in the presence of ultrasonic waves, the alcoholysis reaction is carried out with stirring, and the reaction temperature is 150~ 190℃, N 2 Pressurize and react under pressure of 5.0-8.0 MPa for 1-1.5 h to obtain an alcoholysis product; the molar ratio of PET to diol is 1:1.5;

[0052] The ultrasonic frequency used: 20KHZ, power: 2800W;

[0053] The alcoholysis catalyst is a mixture of zinc acetate and the ionic liquid [Bmim]Br catalyst in a molar ratio of 1:1, and the alcoholysis catalyst accounts for 0.5% of the recovered PET mass;

[0054] S2 maintains the alcoholysis product obtained in step S1 to filter under a high temperature state, and the...

Embodiment 2

[0079]A method for recovering white mud and / or PET to prepare polyester polyol, the preparation steps comprising:

[0080] The acid-treated alkali-reduced white mud and PTA pool material recovered by S1 were added with diethylene glycol in a mass ratio of 1:1, and in the presence of an esterification catalyst, a pre-esterification reaction was carried out, and the reaction temperature was 200-245 ° C to obtain a pre-esterification reaction. polymer; the molar ratio of terephthalic acid and dihydric alcohol in described alkali reduction white mud and PTA pool material is 1:1.5;

[0081] S2 maintains the alcoholysis product or prepolymer obtained in step S1 to filter under a high temperature state, and the filtration temperature is > 220 ° C;

[0082] In the filtration process, stainless steel wire mesh is used for filtration, and the mesh diameter is less than or equal to 20 μm;

[0083] S3 cools down the alcoholysis product and / or the prepolymer filtrate obtained in step S2 t...

Embodiment 3

[0098] A method for recovering white mud and / or PET to prepare polyester polyol, the preparation steps comprising:

[0099] The PET recovered from S1 is crushed, washed with alkali, washed with water, filtered and dried; the recovered PET is mixed with diethylene glycol, and an alcoholysis catalyst is added. 190℃, N 2 Pressurize, react 1~1.5h under pressure 5.0~8.0MPa, obtain alcoholysis product; The mol ratio of described PET and dihydric alcohol is 1: 2;

[0100] The ultrasonic frequency used: 20KHZ, power: 2800W;

[0101] The alcoholysis catalyst is a mixture of zinc acetate and the ionic liquid [Bmim]Br catalyst in a molar ratio of 1:1, and the alcoholysis catalyst accounts for 0.8% of the recovered PET mass;

[0102] The recovered acid-treated alkali-reduced white mud is added with diethylene glycol, and in the presence of an esterification catalyst, a pre-esterification reaction is carried out, and the reaction temperature is 200 to 245° C. to obtain a prepolymer; the ...

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Abstract

The invention discloses a method for preparing polyester polyol by recovering white mud and / or PET (Polyethylene Terephthalate), which comprises the following steps: S1, reacting the recovered PET, dihydric alcohol and a catalyst under ultrasonic and stirring conditions to obtain an alcoholysis product; or recovering the alkali decrement white mud and / or PTA pool material, dihydric alcohol and a catalyst, and reacting to obtain a prepolymer; s2, filtering an alcoholysis product or a prepolymer; s3, cooling the alcoholysis product and / or prepolymer filtrate; s4, the filtrate enters an esterification kettle, dihydric alcohol and / or trihydric alcohol, dibasic acid and / or anhydride and a catalyst are added in proportion, and esterification reaction is carried out; s5, after esterification is finished, filtering the material, and transferring the filtered material to a polycondensation reaction kettle for polycondensation reaction; and S6, after polycondensation is finished, filtering and cooling the material, and packaging. The waste PET material, the alkali decrement white mud and the PTA pool material are subjected to chemical recovery treatment to obtain a standard polyester polyol product, the production cost is low, the process is stable, and energy conservation and carbon reduction are realized through waste utilization and heat recovery.

Description

technical field [0001] The invention belongs to the field of polyol preparation, and in particular relates to a method for preparing polyester polyol by utilizing recycled white mud and / or PET. Background technique [0002] Polyester made of PET is a general polymer material. Polyester PET is mainly used for polyester bottle flakes, polyester fibers and polyester films. Among them, polyester fibers are divided into polyester filaments and polyester staple fibers. , the dosage accounts for about 75% of the entire polyester production, and they are mainly used in the textile industry: polyester bottle flakes account for about 20%, mainly used for food and beverage packaging; polyester film accounts for about 5%, mainly used for The outer layer material has good printability. According to statistics, from 2016 to 2020, the apparent consumption of PET in my country showed a trend of increasing year by year. In 2020, the apparent consumption of PET in my country is 6.5975 milli...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85C08G63/87C08J11/24C08L67/02B01D24/02B01D15/08
CPCC08J11/24C08G63/183C08G63/85C08G63/87B01D24/02B01D15/08C08J2367/02Y02W30/62
Inventor 李大伟姚丙乾李安琪
Owner 李安琪
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