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Catalyst for preparing PTT

A polytrimethylene terephthalate and catalyst technology, applied in the field of catalysts, can solve the problems of long reaction time, high content of by-products propenyl alcohol and acrolein, deactivation of esterification catalyst, etc., and achieve shortened reaction time and content of terminal carboxyl groups. Effects of low and high intrinsic viscosity

Inactive Publication Date: 2007-07-11
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The catalysts used in these patented technologies are used to prepare PTT and often have the following disadvantages: the reaction time is long, and color-changing agents and antioxidants need to be added; phosphorus compounds need to be added before polycondensation to deactivate the esterification catalyst; the by-product propylene in the polycondensation process High alcohol and acrolein content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Catalyst preparation: Mix stannous chloride and malonic acid at a molar ratio of 0.8:1, heat to reflux in water (50mL / g malonic acid) for 4h, filter after cooling, and wash with water (50mL / g malonic acid) After drying at 0.5atm and 80°C for 3 hours, a stannous malonate catalyst was obtained.

[0027] PTT synthesis: add 24.921g PTA, 21.54mL 1,3-PDO and 100ppm stannous malonate catalyst (calculated as PTA) in a 100mL flask, feed nitrogen, control the temperature at 260-270°C, and carry out esterification under normal pressure. Chemical reaction, the generated water is distilled out as the reaction proceeds to obtain a uniform and transparent liquid, and polycondensation is carried out at 260°C under reduced pressure.

[0028] The experimental results obtained are shown in Table 1.

Embodiment 2

[0030] Catalyst preparation: by implementation example 1 method, replace malonic acid with phthalic anhydride, other conditions are identical, prepare stannous phthalate catalyst.

[0031] PTT is synthesized: by implementing the example 1 method, replace stannous malonate with stannous phthalate, other conditions are identical, synthesize PTT polyester.

[0032] The experimental results obtained are shown in Table 1.

Embodiment 3

[0034] Catalyst preparation: by implementation example 1 method, replace tin protochloride with tin protooxide, other conditions are identical, prepare stannous malonate catalyst.

[0035] PTT is synthesized: by implementing the example 1 method, synthesize PTT polyester.

[0036] The experimental results obtained are shown in Table 1.

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Abstract

The invention discloses a making method of polyterephthalic acid propanediol ester, which is reacted by terephthalic acid and 1, 3-methyl glycol, wherein the catalyst is salt generated by tin (II) compound and organic diacid with general formula I or II or corresponding acid anhydride; the tin (II) compound is one of stannous oxide, stannous chloride, stannous bromide, stannous iodide, stannous sulfate, stannous carbonate, stannous hydroxide, stannous caprylate and stannous acetate; n in the formula I is 0-16; R1 and R2 is H, halogen (Cl, Br, I) or alkyl with carbon atom number at 1-6; two carboxyls in the formula II display at adjacent position, interposition or contraposition with other replaced base L on the other positions on the phenyl ring; L is Cl, Br, I, nitro or alkyl with carbon atom number at 1-6.

Description

technical field [0001] The invention relates to a catalyst for the esterification and polycondensation process of polytrimethylene terephthalate (PTT) prepared from terephthalic acid and 1,3-propanediol, the catalyst being a tin (II) compound with an organic dibasic acid or a corresponding Salts formed by the reaction of acid anhydrides. Background technique [0002] Polytrimethylene terephthalate (PTT) is a kind of esterification (or A new type of thermoplastic aromatic polyester synthesized by transesterification) and polycondensation process. Due to its unique helical structure, it has excellent performance, which combines the softness of nylon, the bulkiness of acrylic fiber and the stain resistance of polyester, plus its inherent elasticity, moderate glass transition temperature and good processing performance. The excellent wearability of various fibers has become one of the most popular new polymer materials in the world. It is not only used in the field of synthet...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85
Inventor 王公应贾树勇杜治平姚洁曾毅王越
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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