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Production method of poly(trimethylene terephthalate) with low cyclic dimer content

A polytrimethylene terephthalate and cyclic dimer technology, which is applied in the production field of polytrimethylene terephthalate with low cyclic dimer content, can solve problems such as environmental hazards and increased production costs, Achieve the effects of reducing downtime for cleaning, prolonging the service life, improving production and product quality

Active Publication Date: 2020-04-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can effectively reduce the content of the cyclic dimer and suppress the blooming phenomenon. However, a large amount of toxic solvents are used in this method. If large-scale application will cause serious harm to the environment, and due to the large-scale use of solvents, it will cause Substantial increase in production costs

Method used

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  • Production method of poly(trimethylene terephthalate) with low cyclic dimer content
  • Production method of poly(trimethylene terephthalate) with low cyclic dimer content
  • Production method of poly(trimethylene terephthalate) with low cyclic dimer content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040]Mix 142g of tetraisopropyl titanate with 124g of ethylene glycol and 22.5g of tartaric acid, and react for 4 hours at a temperature of 100°C in a stirred reactor, add 37g of zinc lactate to the reactant, In the reaction at 120°C for 4 hours. The reaction product is placed in a reactor equipped with a fractionation device, and isopropanol and water are distilled off to make a catalyst. The catalyst is mixed with 1,3-propanediol, wherein the mass fraction of titanium atoms is 4%.

[0041] 600 grams of terephthalic acid, 440 grams of 1,3 propylene glycol, 1.49 g of catalyst and stabilizer are mixed to form a slurry, which is added to a polymerization kettle for esterification reaction. The esterification temperature is 230 °C and the pressure is 0.25 MPa. The rectifying device discharges the water generated by the reaction, and reacts for 2 hours. After the esterification is completed, the pressure is lowered to normal pressure, and it begins to enter the pre-condensation...

Embodiment 2-4

[0044] Adopt the catalyst preparation method identical with embodiment 1, difference is that the addition amount of tartaric acid is respectively 75g, 120g and 190g.

Embodiment 5-6

[0046] The same catalyst preparation method as in Example 1 was adopted, except that 172 g of 1,3 propanediol and 180 g of 1,4 butanediol were used as straight chain diols.

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Abstract

The invention relates to a method for producing poly(trimethylene terephthalate) with low-content cyclic dimer. The problems of fogging, white frost and other phenomena which are caused by excessive cyclic dimer in poly(trimethylene terephthalate) during the production in the prior art are solved mainly. The technical scheme comprises the following steps of: (a) adopting terephthalic acid, other aromatic diacids and 1,3-propylene glycol as raw materials, adding catalysts with at least one structure of the general formulas of (I), (II), (III) or (IV), and performing an esterification reaction at an esterification reaction temperature of 220-300 DEG C and esterification reaction pressure of 0.1-0.5 MPa to obtain a prepolymer; and (b) performing pre-polycondensation on the obtained prepolymer, and then performing a melt phase polycondensation reaction to obtain the polymerization product. Through the technical scheme, the problems can be solved well, and the method can be applied to industrial production of poly(trimethylene terephthalate) with the low-content cyclic dimer.

Description

technical field [0001] The invention relates to a production method of polytrimethylene terephthalate, which can be used to manufacture polytrimethylene terephthalate with low cyclic dimer content, so as to reduce "fogging" and "fogging" during spinning and film processing. target of the Hoarfrost phenomenon. The use of the invention can effectively suppress the formation of low-cyclic dimers in the polymerization process, and the final content of the cyclic dimers is lower than 2% of the total weight of the polymer. Background technique [0002] The step-by-step polymerization technique used in the production of polyester will be accompanied by the formation of some structures with low degree of polymerization. The cyclic dimer structure snaps into a ring by itself, which has high thermal stability and does not have the activity required for continued molecular weight growth. groups, and thus will be mixed in the polytrimethylene terephthalate polymer and difficult to remo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/85C08G63/183
CPCC08G63/183C08G63/85
Inventor 周文乐宋歌熊金根章瑛虹
Owner CHINA PETROLEUM & CHEM CORP
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