Preparation method and application of polyester titanium catalyst

A technology of titanium-based catalyst and polyester, which is applied in the field of synthesis of titanium-based catalysts for polyester preparation, and can solve problems such as polyester yellowing

Active Publication Date: 2017-09-08
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by the present invention is the problem of yellowing of polyester caused by titanium-based catalysts in the past, and a synthesis method and application of titanium-based catalysts for polyester preparation are provided

Method used

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  • Preparation method and application of polyester titanium catalyst
  • Preparation method and application of polyester titanium catalyst
  • Preparation method and application of polyester titanium catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Titanium Catalyst I 1 preparation of

[0050] Add diethylene glycol monomethyl ether (5.94g, 49.44mmol), p-toluenesulfonyl chloride (7.85g, 41.20mmol), and potassium carbonate (22.78g, 164.80mmol) into a mortar. Cover with plastic wrap to isolate oxygen, grind for 10 minutes, and place until no heat release (about 4 hours) to obtain a reaction mixture. Dissolve the mixture with dichloromethane, filter the suspension containing the mixture, take the liquid phase and dry it with anhydrous magnesium sulfate, filter the liquid phase, and remove the solvent by rotary evaporation to obtain the product A 1 (9.11 g), yield 80.6%. The reaction formula is as follows:

[0051] .

[0052] Add acetonide (4.61g, 34.87mmol) to the three-necked flask under nitrogen protection, dissolve it in 60mL of anhydrous tetrahydrofuran (THF), put it in an ice-water bath, add sodium hydride (60% dispersed in kerosene, 2.09g, 52.30 mmol). After 30min, the temperature was raised to 40°C, and...

Embodiment 2

[0059] Titanium Catalyst I 2 preparation of

[0060] Add ethylene glycol monomethyl ether (4.00 g, 52.04 mmol), p-toluenesulfonyl chloride (8.27 g, 43.36 mmol), and potassium carbonate (23.98 g, 173.47 mmol) into a mortar. Cover with plastic wrap to isolate oxygen, grind for 10 minutes, and place until no longer exothermic (about 4 hours). Dissolve the mixture with dichloromethane, filter the liquid phase, dry with anhydrous magnesium sulfate, filter the liquid phase, remove the solvent by rotary evaporation, and weigh the product A 2 (8.39 g), yield 84.0%. The reaction formula is as follows:

[0061] .

[0062] Add acetonide (5.06g, 38.26mmol) to the three-necked flask under nitrogen protection, dissolve it in 60mL of anhydrous tetrahydrofuran (THF), put it in an ice-water bath, add sodium hydride (60% dispersed in kerosene, 2.29g, 57.38 mmol). After 30min, the temperature was raised to 40°C, and the product A 2 (8.39g, 36.44mmol) was dissolved in anhydrous THF, drop...

Embodiment 3

[0069]Preparation of polyester

[0070] Mix 500 grams of purified terephthalic acid and 246 grams of ethylene glycol to form a slurry, add it to a polymerization kettle, and carry out esterification reaction. The esterification temperature is 240-250 ° C, the pressure is 0.25 MPa, and it is discharged through a rectification device. water produced by the reaction. After the esterification is finished, it is lowered to normal pressure, and the catalyst I is added 1 , the amount of catalyst is based on the quality of the polyester produced, the mass ratio of titanium atoms is 1.35ppm, vacuumize and depressurize until the system pressure is lower than 150Pa, at the same time, the reaction temperature gradually rises to 280°C, stop the reaction after the intrinsic viscosity reaches the standard, and then put The reaction product is continuously extruded in strip form from the bottom of the polymerization tank, cooled and cut into pellets, and the polyester product is dried, cryst...

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Abstract

The invention relates to synthesis and application of a polyester titanium catalyst. The synthesis of the polyester titanium catalyst comprises grinding monohydric alcohol, para-toluene sulfonyl chloride and inorganic base 1 in a mortar to obtain a product A; performing stirring reaction on glycerol acetonide, inorganic base 2, the product A and phase transfer catalyst to obtain a product B; hydrolyzing the product B under acidic conditions to obtain a product C; reacting the product C with titanium tetrachloride and performing neutralization and reduced pressure distillation to obtain the polyester titanium catalyst I. The invention also relates to application condition optimization of the polyester titanium catalyst I during polyester synthesis. The synthesis and application of the polyester titanium catalyst has the advantages that (1) the obtained polyester titanium catalyst contains no heavy metal during the entire process from preparation to application and is free from toxicity and damage; (2) the polyester titanium catalyst is higher in activity compared with ordinary titanium catalysts, thereby being little in consumption and residue and low in influence of subsequent polyester processing; (3) polyesters prepared through the polyester titanium catalyst saves additional dyes, namely, can reach a relatively low b value and accordingly can be applied to fields such as chemical fiber fabric and food bottles.

Description

technical field [0001] The invention relates to a preparation method and application of a titanium-based catalyst, in particular to a synthesis method and application of a titanium-based catalyst for polyester preparation. The catalyst can be used for the synthesis of polyethylene terephthalate slices. Background technique [0002] Polyethylene terephthalate (PET for short) is the most productive variety among polyester fibers. The synthesis process of PET polyester chips usually uses pure terephthalic acid (PTA for short) and ethylene glycol (EG for short) as raw materials, and is synthesized by direct esterification and polycondensation reaction. The polycondensation reaction requires A catalyst is added to promote molecular weight growth. At present, the catalysts for polyester polycondensation that are widely used and studied in industry are classified according to the active center, mainly including three types: antimony, germanium and titanium. [0003] Antimony-base...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/85C08G63/183
CPCC08G63/183C08G63/85
Inventor 孙芳刘斌刘洪春刘永滨乔玥
Owner BEIJING UNIV OF CHEM TECH
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