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Preparation method and use of titanium catalyst for synthesis of polybutylene terephthalate

A polybutylene terephthalate and titanium-based catalyst technology, which is applied in the field of polyester synthesis, can solve the problems of reducing catalytic activity, affecting thermal stability of chips, melting stability, and long-term operation of devices, achieving The effect of excellent performance

Active Publication Date: 2014-06-25
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem that the present invention needs to solve is to disclose a kind of preparation method that is used for the synthetic titanium series catalyst of polybutylene terephthalate, to overcome the following defective that exists in the prior art: in the actual production of PBT at present, most Tetrabutyl titanate is used as the catalyst, which is easy to be hydrolyzed and partially inactivated. Its hydrolysis not only reduces the catalytic activity but also easily blocks the pipeline, causing fouling of the reactor and pipeline, which affects the long-term operation of the device; when the titanium content increases, it affects the slice. Thermal stability, melting stability, so that the molecular weight is reduced, the carboxyl end value is increased, and the color is darkened

Method used

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  • Preparation method and use of titanium catalyst for synthesis of polybutylene terephthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The molar ratio of tetraisopropyl titanate to glycerol is 1:0.5, the molar ratio of tetraisopropyl titanate to sodium hydroxide is 1:0.5, and the molar ratio of tetraisopropyl titanate to triethyl phosphate The molar ratio of tetraisopropyl titanate to the magnesium acetate tetrahydrate is 1:0.5, and the molar ratio of tetraisopropyl titanate to 1,4-butanediol solvent is 1:3.73.

[0026] Add 42.6g tetraisopropyl titanate (0.15mol) and 6.9g glycerol (0.075mol) and 50g 1,4-butanediol (0.56 mol), mix well. A solution of 3.0 g of sodium hydroxide (0.075 mol) and 50 g of deionized water was slowly dropped into the reactor, and after the addition was completed, the reaction was carried out at room temperature to 100° C. for 1 hour. Precipitate a white precipitate, continue to add 16.1g magnesium acetate tetrahydrate (0.075mol) and 13.7g triethyl phosphate (0.075mol), start to react at 50°C and gradually increase the temperature to 160°C for 3 hours, remove small molecules, t...

Embodiment 2

[0031] The molar ratio of tetrabutyl titanate to glycerol is 1:0.1, the molar ratio of tetrabutyl titanate to sodium hydroxide is 1:0.05, and the molar ratio of tetrabutyl titanate to triethyl phosphate is 1: 10. The molar ratio of tetrabutyl titanate to the sodium acetate trihydrate is 1:10, and the molar ratio of tetrabutyl titanate to 1,4-butanediol solvent is 1:50.

[0032] Add 51.1g tetrabutyl titanate (0.15mol) and 1.4g glycerol (0.015mol) and 675g 1,4-butanediol (7.5mol) into the reactor equipped with stirrer, separatory funnel and condenser ),well mixed. A solution of 0.3 g of sodium hydroxide (0.0075 mol) and 50 g of deionized water was slowly dropped into the reactor, and after the addition was completed, the reaction was carried out at room temperature to 50° C. for 0.1 hour. Precipitate a white precipitate, continue to add 204.2g sodium acetate trihydrate (1.5mol) and 273.1g triethyl phosphate (1.5mol), start at 50°C and gradually raise the temperature to 200°C fo...

Embodiment 3

[0037] The molar ratio of tetraisopropyl titanate to glycerol is 1:20, the molar ratio of tetraisopropyl titanate to sodium carbonate is 1:5, and the molar ratio of tetraisopropyl titanate to trimethyl phosphate is 1:0.1, the molar ratio of tetraisopropyl titanate to the magnesium acetate tetrahydrate is 1:0.02, and the molar ratio of tetraisopropyl titanate to 1,4-butanediol solvent is 1:2.

[0038] Add 42.6g tetraisopropyl titanate (0.15mol) and 276.0g glycerol (3.0mol) and 27.0g 1,4-butanediol ( 0.30mol), mix well. A solution of 79.5 g of sodium carbonate (0.75 mol) and 100 g of deionized water was slowly dropped into the reactor, and after the addition was completed, the reaction was carried out at room temperature to 100° C. for 12 hours. Precipitate a white precipitate, continue to add 6.4g of magnesium acetate tetrahydrate (0.003mol) and 2.1g of trimethyl phosphate (0.015mol), at 50°C, gradually increase the temperature to 200°C for 0.1 hour, remove small molecules, un...

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Abstract

The invention discloses a preparation method and a use of a titanium catalyst for synthesis of polybutylene terephthalate. The preparation method comprises the following steps that 1, at least one titanium compound, glycerol and at least one alkaline material undergo a reaction in the presence of at least one solvent at a temperature of 0 to 100 DEG C for 0.1 to 12 hours, wherein the titanium compound is Ti(OR)4 and R represents a C1-10 alkyl group; and 2, the reaction products are added with at least one phosphorus compound; the mixture and an acetate of Na, Li, Mg or Zn undergoes a reaction at a temperature of 50 to 200 DEG C for 0.1 to 12 hours; and micro-molecules in the reaction products are removed and the titanium catalyst which is uniform and stable and has hydrolysis resistance is obtained. The titanium catalyst as an esterification and polymerization catalyst can be directly added into raw materials for synthesis of polybutylene terephthalate, or can be added into the raw materials after being diluted and dissolved in 1,4-butanediol. In polybutylene terephthalate synthesis, the titanium catalyst has the advantages of good activity, small tetrahydrofuran produced by side reactions, stable slice hue and good slice heat stability.

Description

technical field [0001] The invention belongs to the technical field of polyester synthesis, and in particular relates to a preparation method and application of a titanium-based catalyst used in the synthesis of polybutylene terephthalate. Background technique [0002] Polybutylene terephthalate (PBT for short) has excellent mechanical, electrical, chemical corrosion resistance, easy molding and low moisture absorption properties, etc. It is a new type of engineering plastic with excellent comprehensive properties. Since its inception, it has developed quite rapidly. At present, it has become the fastest-growing one among the five major engineering plastics. It is used in many fields such as automobiles, electronics, machinery, optical fiber coating, and fibers, and new application fields are constantly expanding. [0003] The technical route of PBT production can be divided into transesterification method and direct esterification method. The production process of direct e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85
Inventor 臧国强杨力芳郭灵通马颖涛李云鹏
Owner CHINA PETROLEUM & CHEM CORP
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