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A method of adding titanium dioxide to prepare semi-dull and full-dull titanium series polyester

A technology of titanium-based polyester and titanium dioxide, which is applied in the field of preparing semi-dull and full-dull titanium-based polyester by adding titanium dioxide, which can solve the problems of decreased catalyst activity, inaccurate catalyst metering, and inability to use polyester.

Active Publication Date: 2018-06-15
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The inventors have noticed that when titanium dioxide is added to the existing titanium-based catalysts to produce titanium-based polyesters, the activity of the catalysts decreases and polyesters with acceptable viscosity cannot be produced; or when using titanium-based catalysts, additional A co-catalyst is used to offset the decline of the titanium catalyst. Since the co-catalyst is solid or corrosive, it will cause inaccurate metering, uneven addition or corrosion of pipeline equipment when the catalyst is continuously added, so it cannot be applied in the actual production of polyester

Method used

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  • A method of adding titanium dioxide to prepare semi-dull and full-dull titanium series polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 42.6g tetraisopropyl titanate (0.15mol), 93.0g ethylene glycol (1.5mol), 5.8g sodium p-toluenesulfonate (0.03mol) to the reactor equipped with stirrer, separatory funnel and condenser ) and 3.0 g of sodium hydroxide (0.075 mol), the temperature was gradually increased from 30 ° C to 200 ° C for 1 hour, and the reaction system became a homogeneous liquid after removing low-boiling small molecular substances, and catalyst A was obtained.

[0029] Preparation of semi-dull titanium-based polyester

[0030] 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 5 * 10 -6 ), add 2L polymerization reactor. The esterification reaction is carried out under the conditions of 230°C-260°C and 0-0.4MPa. When the amount of distilled water reaches more than 95% of the theoretical value, the esterification is over, and 1.4g of titanium dioxide is added to the esterific...

Embodiment 2

[0033] Add 42.6g tetraisopropyl titanate (0.15mol), 13.8g glycerol (0.15mol), 2.6g sodium dodecylsulfonate ( 0.0075 mol) and 1.6 g of sodium carbonate (0.015 mol), the temperature was gradually increased from 30°C to 200°C for 1 hour, and the reaction system became a homogeneous liquid after removing small molecular substances with low boiling points, and catalyst B was obtained.

[0034] Preparation of full-dull titanium-based polyester

[0035] With 500g terephthalic acid (PTA), 270g ethylene glycol (EG) and catalyst B (based on the amount of the polyester that generates, the weight content of titanium atom is 50 * 10 -6), add 2L polymerization reactor. The esterification reaction is carried out under the conditions of 230°C-260°C and 0-0.4MPa. When the amount of distilled water reaches more than 95% of the theoretical value, the esterification is over, and 16.5g of titanium dioxide is added to the esterification product (to generate The amount of polyester is 3.0%). After...

Embodiment 3

[0038] Add 25.8g of tetramethyl titanate (0.15mol), 135g of 1,4-butanediol (1.5mol), 10.9g of potassium dodecylsulfonate to the reactor equipped with stirrer, separatory funnel and condenser (0.03mol) and 10.4g salt of wormwood (0.075mol), at 30 ℃ gradually warming up to 200 ℃ for 1 hour, reaction system becomes homogeneous liquid after removing low-boiling point small molecules, obtains catalyst C.

[0039] Preparation of semi-dull titanium-based polyester

[0040] Adopt the same method as embodiment 1 to prepare polyester, use catalyst C as catalyst (based on the amount of the polyester of generation, the weight content of titanium atom is 5 * 10 -6 ).

[0041] The synthetically obtained semi-dull polyester product was tested for performance, and the esterification, polymerization time and analysis results are shown in Table 1.

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Abstract

The invention relates to a method for preparing semi-dull and full-dull titanium polyester through adding titanium dioxide, and solves a problem that titanium dioxide used as a delustering agent in the prior art has an inhibition effect on the activity of titanium polyester catalysts. The method comprises the following steps: adding titanium dioxide used as the delustering agent to raw materials comprising terephthalic acid and ethylene glycol, carrying out an esterification reaction in the presence of a liquid titanium polyester catalyst, and carrying out a pre-polycondensation and polycondensation reaction under vacuum conditions to obtain the polyester product, wherein the liquid titanium polyester catalyst is a product prepared through a reaction of titanate, polyol, sulfonate and an alkaline metal compound, a molar ratio of titanate to polyol is 1:1 to 1:10, a molar ratio of titanate to sulfonate is 20:1 to 5:1, and a molar ratio of titanate to the alkaline metal compound is 10:1 to 2:1. The method allows semi-dull and full-dull titanium polyester with superior performances to be obtained, and can be used in practical industrial production of polyester.

Description

technical field [0001] The invention relates to a method for preparing semi-dull and full-dull titanium series polyester by adding titanium dioxide. Background technique [0002] Polyethylene terephthalate (hereinafter referred to as polyester) is an important polymer material. Due to its various excellent properties, it is widely used in the fields of fibers, bottles, films, engineering plastics, etc. It is currently used The largest variety of synthetic fibers. [0003] Catalyst is a very important link in polyester production process. The catalysts that can be used for polyester polymerization mainly include antimony series, germanium series, titanium series and so on. Due to the general activity of antimony-based catalysts and the small degree of influence on thermal degradation reactions, almost all types of polyesters can be prepared using antimony-based catalysts. Therefore, the commercial production of polyester has been using the heavy metal antimony as The main c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85C08K3/22
Inventor 臧国强杨力芳郭灵通张丽梅
Owner CHINA PETROLEUM & CHEM CORP
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