Liquid titanium catalyst for polyester and copolyester and preparation method thereof

A technology of titanium-based catalyst and copolyester, which is applied in the field of catalyst and its preparation, can solve problems such as adverse effects, darkening of catalyst color, and affecting the color of polyester products, so as to achieve the effect of ensuring product quality and light color

Active Publication Date: 2012-03-21
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to provide a liquid titanium-based catalyst for polyester and copolyester and its preparation method. The technical problem to be solved is to overcome the following defects in the p...

Method used

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  • Liquid titanium catalyst for polyester and copolyester and preparation method thereof
  • Liquid titanium catalyst for polyester and copolyester and preparation method thereof
  • Liquid titanium catalyst for polyester and copolyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Add 42.6 g of tetraisopropyl titanate (0.15 mol), 3.1 g of tetraethyl orthosilicate (0.015 mol) and 100 g of absolute ethanol into a reactor equipped with a stirrer, a separatory funnel, and a condenser, and mix well. A mixed solution of 63.3 g of citric acid monohydrate (0.3 mol) and 150 g of absolute ethanol was slowly dropped into the reactor, and after the addition was completed, the mixture was reacted at room temperature to 100° C. for 1 hour. Precipitate a white precipitate, continue to add 4.1g sodium acetate (0.03mol) and 55.2g triethyl phosphate (0.3mol), react at 50-200°C for 0.5-3 hours, remove small molecules, until the system becomes a homogeneous liquid , to obtain catalyst A.

[0033] Preparation of polyester

[0034] With 500g terephthalic acid (PTA), 270g ethylene glycol (EG) and catalyst A (based on the amount of the polyester that generates, the weight content of titanium atom is 10 * 10 -6 ), add 2L polymerization reactor. The esterification react...

Embodiment 2

[0037] Add 51.1 g of tetrabutyl titanate (0.15 mol), 3.1 g of tetraethyl orthosilicate (0.015 mol) and 100 g of absolute ethanol into a reactor equipped with a stirrer, a separatory funnel, and a condenser, and mix well. A mixed solution of 63.3 g of citric acid monohydrate (0.3 mol) and 150 g of absolute ethanol was slowly dropped into the reactor, and after the addition was completed, the mixture was reacted at room temperature to 100° C. for 1 hour. Precipitate a white precipitate, continue to add 6.4g magnesium acetate (0.03mol) and 82.8g triethyl phosphate (0.45mol), react at 50-200°C for 0.5-3 hours, remove small molecules, until the system becomes a homogeneous liquid , to obtain catalyst B.

[0038] Preparation of polyester

[0039] Adopt the same method as embodiment 1 to prepare polyester, use catalyst B as catalyst (based on the amount of the polyester that generates, the weight content of titanium atom is 10 * 10 -6 ).

[0040] The obtained PET product was subje...

Embodiment 3

[0042] Add 42.6 g of tetraisopropyl titanate (0.15 mol), 6.2 g of tetraethyl orthosilicate (0.03 mol) and 100 g of absolute ethanol into a reactor equipped with a stirrer, a separatory funnel and a condenser, and mix well. A mixed solution of 63.3 g of citric acid monohydrate (0.3 mol) and 150 g of absolute ethanol was slowly dropped into the reactor, and after the addition was completed, the mixture was reacted at room temperature to 100° C. for 1 hour. Precipitate a white precipitate, continue to add 6.6g zinc acetate (0.03mol) and 55.2g triethyl phosphate (0.3mol), react at 50-200°C for 0.5-3 hours, remove small molecules, until the system becomes a homogeneous liquid , to obtain catalyst C.

[0043] Preparation of polyester

[0044] Adopt the same method as embodiment 1 to prepare polyester, use catalyst C as catalyst (based on the amount of the polyester that generates, the weight content of titanium atom is 10 * 10 -6 ).

[0045] The obtained PET product was subjected...

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Abstract

The invention relates to a preparation method of a liquid titanium catalyst for polyester and copolyester, which comprises the following steps of: (A) reacting a titanium compound, tetraethoxysilane and hydroxy carboxylic acid in a solvent at 0-100 DEG C for 0.1-24 hours, wherein the titanium compound is Ti(OR)4, and R is selected from alkyls of 1 to 10 carbon atoms; and (B) adding a phosphorous compound and acetate which is selected from metal elements of Na, Mg, Al, Zn and La into a reaction product in the step (A), reacting at 50-200 DEG C for 0.1-48 hours and removing micro-molecules to obtain the liquid titanium catalyst. By introducing a silicon element and other metal elements into the titanium catalyst and optimizing the preparation process condition of the catalyst, the catalyticactivity of the catalyst is regulated; the prepared catalyst can be mutual soluble with glycol and can be stably stored; and the polyester and copolyester prepared by using the catalyst have good hueand narrow molecular weight distribution.

Description

technical field [0001] The invention relates to a catalyst for polyethylene terephthalate, polyester and copolyester and a preparation method thereof, in particular to a liquid titanium catalyst for polyester and copolyester and its preparation method. Preparation. Background technique [0002] Polyester and copolyester are an important class of industrial polymers and one of the most important raw materials for synthetic fibers. They are also widely used in engineering plastics, films, bottle packaging, sheets and other fields. Polyester and copolyester that the present invention relates to are commonly referred to polyethylene terephthalate (PET) and copolyester, have following structural segment (taking PET as example): [0003] [0004] Wherein: m=2, 3 or 4; n is the degree of polymerization, n=50-70, and its molecular weight is 10000-15000. Copolyester refers to the third component added to improve the performance of polyester in the PET preparation process, such a...

Claims

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Application Information

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IPC IPC(8): C08G63/85
Inventor 臧国强郭灵通杨力芳李卫伟李军李云鹏
Owner CHINA PETROLEUM & CHEM CORP
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