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Preparation method capable of stably producing PBT resin for long period

A PBT resin, stable production technology, applied in the field of polyester, can solve the problems of high production cost, short production cycle of PBT, etc., achieve stable properties, reduce production costs, and excellent product quality

Active Publication Date: 2020-08-04
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The invention provides a preparation method for long-term stable production of PBT resin. Specifically, terephthalic acid and 1,4-butanediol are used as main raw materials for melt polymerization reaction, and the catalyst used in the polymerization reaction is an organic chelate water-resistant Decomposition catalyst; the purpose is to solve the problem of using tetrabutyl titanate as a catalyst in the synthesis of PBT, resulting in the long-term formation of precipitated products with esterification water, making the production cycle of PBT short and the production cost high

Method used

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  • Preparation method capable of stably producing PBT resin for long period
  • Preparation method capable of stably producing PBT resin for long period
  • Preparation method capable of stably producing PBT resin for long period

Examples

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Effect test

Embodiment 1

[0055] A kind of preparation method that can stably produce PBT resin for a long period of time, concrete steps are as follows:

[0056] (1) Stir 1,4-butanediol and basic metal compound (zinc acetate) at 40°C for 1 hour, add tetrabutyl titanate dropwise for 2 hours, and raise the temperature to 80°C after the addition After stirring and reacting for 2 hours, lower the temperature to room temperature to obtain solution I; stir ethylenediaminetetraacetic acid and industrial ammonia water with a mass concentration of 25% at 30°C for 1 hour to obtain solution II; add solution II dropwise to solution I , the dropwise addition time is 2h, after the dropwise addition is completed, the temperature is raised to 70°C and the reaction is stirred for 1h, and the low-boiling point substances are extracted, cooled to room temperature and stirred for 1h, and finally a homogeneous and clear organic chelate hydrolysis-resistant catalyst is obtained; wherein, the content of each substance The a...

Embodiment 2

[0074] A kind of preparation method that can stably produce PBT resin for a long period of time, concrete steps are as follows:

[0075] (1) Stir 1,3-propanediol and basic metal compound (zinc hydroxide) at 50°C for 0.1h, drop tetrabutyl titanate for 3h, and raise the temperature to 70°C after the addition After stirring and reacting for 1 hour, lower the temperature to room temperature to obtain solution I; stir ethylenediaminetetraacetic acid and industrial ammonia water with a mass concentration of 25% at 40°C for 1 hour to obtain solution II; add solution II dropwise to solution I , dropwise for 1h, after the dropwise addition was completed, the temperature was raised to 60°C and stirred for 2h, and the low boiling point substances were taken out, and after cooling down to room temperature and stirred for 0.1h, a homogeneous and clear organic chelate hydrolysis-resistant catalyst was finally obtained; among them, each substance The amount of addition is: the molar ratio of...

Embodiment 3

[0086] A kind of preparation method that can stably produce PBT resin for a long period of time, concrete steps are as follows:

[0087] (1) Stir ethylene glycol and basic metal compound (copper acetate) at 30°C for 3h, add dropwise tetrabutyl titanate for 5h, after the dropwise addition, raise the temperature to 60°C and stir for 4h , the temperature was lowered to room temperature to obtain solution I; ethylenediaminetetraacetic acid and industrial ammonia water with a mass concentration of 25% were stirred at 20°C for 1 hour to obtain solution II; solution II was added dropwise to solution I, and the time 3h, after the dropwise addition was completed, the temperature was raised to 50°C and the reaction was stirred for 3h, and the low-boiling point substances were extracted, cooled to room temperature and then stirred for 2h to finally obtain a homogeneous and clear organic chelate hydrolysis-resistant catalyst; wherein, the amount of each substance added was: The molar rati...

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Abstract

The invention relates to a preparation method capable of stably producing PBT resin for a long period; terephthalic acid and 1,4-butanediol are used as main raw materials for melt polymerization reaction, and a catalyst adopted in the polymerization reaction is an organic chelating hydrolysis-resistant catalyst; the preparation process of the organic chelating hydrolysis-resistant catalyst comprises the steps: (1) mixing 1,4-butanediol and an alkaline metal compound, and dropwise adding tetrabutyl titanate to obtain a solution I; (2) mixing ethylenediamine tetraacetic acid and industrial ammonia water under a condition II to obtain a solution II; and (3) finally, dropwise adding the solution II into the solution I to obtain an organic chelating hydrolysis-resistant catalyst. The intrinsicviscosity of the prepared PBT resin is greater than 0.9 dl / g, and the b value is less than 6; the thermal cleaning period of a reaction device in the three-kettle process system is more than 12 months; the method provided by the invention solves the ubiquitous problem of incapability of long-period (less than one year or even half a year) operation in PBT resin production.

Description

technical field [0001] The invention belongs to the technical field of polyester and relates to a preparation method capable of stably producing PBT resin in a long period. Background technique [0002] Polybutylene terephthalate (PBT) is a crystalline linear saturated polyester and is a thermoplastic material. Because of its easy processing and molding, excellent electrical properties, mechanical properties, and heat resistance, it is widely used in electronic and electrical components , automobiles, machinery and equipment, and fiber optic cables and other fields. Film, sheet, fiber and other fields are gradually widely used. [0003] The synthesis of PBT is mostly a direct esterification method, using tetrabutyl titanate (TBT, the molecular formula is Ti(OCH 3 ) 4 ) as a catalyzer, the reaction route of the esterification process is as shown in formula (1): [0004] [0005] It can be seen from formula (1) that PBT will generate a large amount of esterified water d...

Claims

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Application Information

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IPC IPC(8): C08G63/85C08G63/83C08G63/183
CPCC08G63/183C08G63/83C08G63/85
Inventor 关震宇张玉梅王华平
Owner DONGHUA UNIV