Catalyst composition comprising titanium compound, phosphorus compound and solubility promoter, preparation and use thereof

A technology for dissolving accelerators and titanium compounds, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, catalytic reactions, etc., and can solve problems such as non-uniform distribution of catalysts, yellowing in color, etc.

Inactive Publication Date: 2001-05-30
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, organic titanates are generally not used in the production of PET because of the tendency of residual titanates to react with trace impurities such as aldehydes formed during PET polycondensation and processing, resulting in The color that does not meet the requirements turns yellow
In addition, many organotitanate catalysts are largely insoluble in the polymerization mixture, resulting in a non-uniform distribution of the catalyst in the mixture

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1A

[0051] Preparation of antimony-free DMT oligomers:

[0052] The oligomer used in these examples contained dimethyl terephthalate, ethylene glycol, and no antimony added. It is prepared as follows:

[0053] 100 lbs (45.4 Kg) of dimethyl terephthalate, 67 lbs (30.4 Kg) of ethylene glycol, and 4.4 g of zinc acetate dihydrate were charged into the autoclave. The material was heated to 240° C. with stirring at 15 rpm, and 33 lbs (15.0 Kg) of methanol and 14.3 lbs (6.5 Kg) of ethylene glycol were removed. The charge was then heated to 275°C over the course of 90 minutes and the remaining ethylene glycol was removed at 285°C under a vacuum of less than 2 mm Hg. Once the condensation of the identified material is complete, the molten material is squeezed into a water bath to solidify the product. The resulting polymer is dried to remove residual moisture before use. Example 1B

Embodiment 1B

[0054] Tests of catalysts in oligomers:

[0055] A liter of resin reaction kettle with a transient mixing agitator, a thermocouple, a condenser and a nitrogen purge port at 40rpm is equipped with a rotating speed, and the DMT low as prepared in the example 1A is added to the still to be tested catalyst, 115ml ethylene glycol, 400g Polymer. The stirrer was started and the temperature was raised to 275°C over a period of about 2.5 hours. The reactor contents were polymerized with stirring at 275°C, 120 Torr for 20 minutes and at 280°C, 30 Torr for an additional 20 minutes. The contents were then maintained under agitation at 285°C under a pressure of 1-2 mmHg for a time sufficient to achieve a torque of 15 oz-in (oz-in), as measured with an Electro-Craft Motomatic torque controller. The time taken for this step is recorded as the completion time, which varies with the catalyst used. The molten polymer is then poured into a water tank to allow the melt to solidify. The result...

Embodiment 2

[0057] A 500ml flask equipped with a stirrer, condenser, dropping funnel and nitrogen purging was charged with 240g (3.87mol) of ethylene glycol. Start stirring and add 25g (0.176mol) phenylphosphinic acid, heat the slurry to 35-45°C until the solid dissolves, then add 50g (0.176mol) tetraisopropyl titanate (TYZOR) dropwise at 35°C for 1 hour _ TPT, available from E.I. du Pont de Nemours and Co.). After the addition was complete, the reaction was stirred for 30 minutes, then 36.6 g (0.176 mol) of tetraethyl orthosilicate (TEOS) was added over 30 minutes to obtain a clear solution containing 2.4% titanium. Example 3

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PUM

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Abstract

A catalyst composition is disclosed. The composition comprises a titanium compound, a solubility promoter selected from the group consisting of orthosilicates, orthozirconates, and combinations thereof, a phosphorus source, a solvent, and optionally a sulfonic acid, a cocatalyst, or both. The cocatalyst can be a cobalt / aluminum catalyst, and antimony compound, or combinations thereof. Also disclosed is a process for producing the composition. The process comprises combining a titanium compound, a solubility promoter, a phosporous source, a solvent, and optionally a sulfonic acid, a cocatalyst, or both. Further disclosed is a process for using the composition which comprises contacting a carbonyl compound, in the presence of the composition, with an alcohol under a condition suitable for esterification, transesterification, polymerization, or combinations thereof.

Description

field of invention [0001] The present invention relates to a catalyst composition comprising a titanium compound, a method of preparing the composition, and a method of using the composition, for example in the esterification, transesterification or polymerization of carbonyl compounds. Background of the invention [0002] Polyesters, such as polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), commonly referred to as "polyalkylene terephthalate," are a important industrial polymers. They are widely used in thermoplastic fiber, film, and molding applications. [0003] Polyalkylene terephthalates can be prepared by transesterification of a dialkyl terephthalate with diols or direct esterification of terephthalic acid with selected diols followed by polycondensation. Catalysts are used to catalyze this esterification, transesterification or polycondensation. [0004] Many commercial processes use manganese or zinc salts as cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/24B01J27/14B01J31/02B01J31/12B01J31/26C08G63/82C08G63/85
CPCB01J27/14B01J31/0212B01J31/0225B01J31/0259B01J31/0261B01J31/0262B01J31/0274B01J31/128B01J2231/14B01J2231/40B01J2231/49C08G63/82C08G63/85
Inventor D·E·普特兹格E·F·麦布里德H·Q·杜J·A·特赖恩哈姆H·L·杰格尔H·舒尔特
Owner EI DU PONT DE NEMOURS & CO
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