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Method for preparing trioctyltrimellitate through ester exchange method

A technology for trimethyl trimellitic acid and trimellitic acid, which is applied in the field of preparing trioctyl trimellitic acid by transesterification method, can solve the problems such as the invention report of no useful components of trimellitic anhydride waste products, and achieves convenient operation. , the effect of easy production

Inactive Publication Date: 2018-11-27
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] After consulting a large number of documents, there is no invention report about recycling useful components in trimellitic anhydride waste products both at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 1000g of isooctyl alcohol, 500g of trimethyl trimellitate and 1g of catalyst tetraisopropyl titanate in sequence in the transesterification kettle, stir and heat to 210°C, and the reaction time is 2h; open the vacuum and gradually increase from 7500Pa to 500Pa, The temperature of the reaction solution dropped from 210°C to 160°C, the dealcoholization was completed, the temperature of the reaction solution continued to drop to 90°C, 15g of deionized water was added, stirred at constant temperature for 0.5h, the vacuum was turned on and gradually increased from 7500Pa to 500Pa, the dehydration was completed, and 2g of activated carbon was added , stirred and refined at 90°C for 0.5h, filtered while it was hot, and 1150g of the product trioctyl trimellitate could be obtained, the content was 99.75%, and the color number was 11#.

Embodiment 2

[0026] Add 1500g of isooctyl alcohol, 500g of trimethyl trimellitate and 1g of catalyst tetraisopropyl titanate in sequence in the transesterification kettle, stir and heat to 220°C, and the reaction time is 3h; open the vacuum and gradually increase from 7500Pa to 500Pa , the temperature of the reaction solution dropped from 210°C to 160°C, the dealcoholization was completed, the temperature of the reaction solution continued to drop to 90°C, 15g of deionized water was added, stirred at constant temperature for 0.5h, the vacuum was turned on and gradually increased from 7500Pa to 500Pa, the dehydration was completed, and activated carbon was added 2g, stirred and refined at 90°C for 0.5h, filtered while it was hot, and 1150g of the product trioctyl trimellitate could be obtained, the content was 99.82%, and the color number was 12#.

Embodiment 3

[0028] During industrial production, 28t of isooctyl alcohol, 7t of trimethyl trimellitate and 15Kg of catalyst tetraisopropyl titanate were sequentially added to the transesterification kettle, stirred and heated to 230°C, and the reaction time was 4h; the vacuum was gradually increased from 7500Pa to As high as 500Pa, the temperature of the reaction solution drops from 210°C to 160°C, the dealcoholization is completed, the temperature of the reaction solution continues to drop to 90°C, add 300Kg of deionized water, stir at constant temperature for 0.5h, turn on the vacuum and gradually increase from 7500Pa to 500Pa, and the dehydration is completed , adding 30Kg of activated carbon, stirring and refining at 90°C for 0.5h, and filtering while hot, the product trioctyl trimellitate 16.1t can be obtained, the content is 99.82%, and the color number is 10#.

[0029] The beneficial effect of the present invention is: the preparation method of the present invention is easy to opera...

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PUM

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Abstract

The invention relates to the technical field of environment-friendly solvents, and particularly discloses a method for preparing trioctyltrimellitate through an ester exchange method. The method comprises the following steps that isooctanol, trimellitic acid trimethy phosphate and a catalyst are sequentially added into an ester exchange kettle, heating is performed to extract methyl alcohol and excessive isooctyl alcohol, and the reaction is ended after heating is performed; the vacuum degree is increased to remove excessive isooctyl alcohol, the ester exchange kettle stops heating, the reaction solution is naturally cooled, and dealcoholization is ended after cooling is performed; water is added into the reaction solution, after heating, washing is performed to remove a catalyst, and dehydration is performed after washing is ended; activated carbon is added, after stirring heating, refining is performed, and immediate filtration is performed to obtain the product trioctyltrimellitate.According to the preparation method, the trimellitic acid trimethy phosphate and the isooctyl alcohol are subjected to an ester exchange reaction, and then the product is obtained after dealcoholization, catalyst removal, refining and filtering; the content of the obtained trioctyltrimellitate is 99.5% or above, the platinum and cobalt color number is smaller than 15, and the requirement for thequality of the product trioctyltrimellitate is met.

Description

technical field [0001] The invention relates to the technical field of environment-friendly solvents, in particular to a method for preparing trioctyl trimellitate by transesterification. Background technique [0002] Trioctyl trimellitate, referred to as TOTM, also known as tris(2-ethylhexyl) trimellitate, can be used as a plasticizer with low volatility, excellent heat resistance, low mobility, and Good insulation, durability, low toxicity, water resistance and proper compatibility, suitable for polyvinyl chloride, vinyl chloride copolymer, nitrocellulose, ethyl cellulose and other plastics, and can also be used as heat-resistant wire and cable materials, plates , sheets, gaskets, etc. [0003] Trimethyl trimellitate can be used as a transesterification intermediate to prepare trioctyl trimellitate. Trimellitic anhydride synthesizes low-boiling trimethyl trimellitate through esterification reaction with low-molecular alcohols, which can convert waste products of poor qua...

Claims

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Application Information

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IPC IPC(8): C07C67/03C07C67/48C07C69/76
CPCC07C67/03C07C67/48C07C69/76
Inventor 郑铁江蒋国强曹圣平杜法举陶植郑立新杨伟浩马俊华
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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