A kind of synthetic method of triisodecyl trimellitate

A technology for the synthesis of triisodecyl trimellitate and its synthesis method, which is applied in the field of synthesis of triisodecyl trimellitate, can solve problems such as dissolution, and achieve the effects of bright color, reduced acid value, and high ester content

Active Publication Date: 2022-03-29
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional plasticizers, such as phthalate plasticizers, are extremely volatile and migratory, and will cause dissolution during processing, heating, packaging, etc., which are carcinogens

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put 121g of trimellitic anhydride into the esterification reaction kettle, then add 504g of 2-propyl-1-heptanol, and add 90g of mesitylene, heat up to 115°C to dissolve, then raise the temperature to 160°C to keep the liquid out for 50min, then add 1g Tetrabutyl titanate, finally heated up to 220°C and kept for 5 hours, and the esterification was completed when the acid value of the reaction solution to be detected was less than or equal to 0.1mgKOH / g;

[0027] Under the condition of 195°C, exhaust the remaining isodecyl alcohol in the reaction system under negative pressure vacuum, and the exhaust time is 2h;

[0028] Lower the temperature to 75°C, prepare a solution of 0.1g of sodium bicarbonate dissolved in 21g of water, add it to the reaction solution, and stir for 0.5h to destroy the unhydrolyzed catalyst in the reaction solution;

[0029] Then add 0.5g active soil, stir evenly for decolorization for 1.5h, then filter, and add a small amount of perlite as a filter ...

Embodiment 2

[0033] (1) Put 115g of trimellitic anhydride into an esterification reaction kettle, then add 465g of 2-propyl-1-heptanol, and add 65g of trimethylene, heat up to 140°C to dissolve, then heat up to 175°C to keep the liquid out for 15min, Then add 2g of tetrapropyl titanate, and finally raise the temperature to 215°C and keep it warm for 3h. When the acid value of the reaction solution to be detected is less than or equal to 0.1mgKOH / g, the esterification is completed;

[0034] (2) Under the condition of 200°C, exhaust the remaining isodecyl alcohol in the reaction system under negative pressure vacuum, and the exhaust time is 1.5h;

[0035] (3) Lower the temperature to 95° C., prepare a solution of 0.2 g of sodium bicarbonate dissolved in 32 g of water, add it to the reaction solution, and stir for 1 hour to destroy the unhydrolyzed catalyst in the reaction solution;

[0036] (4) Then add 1.5g activated alumina, stir evenly for decolorization for 2h, then add a small amount of...

Embodiment 3

[0039] (1) Put 109g of trimellitic anhydride into an esterification reaction kettle, then add 475g of 2-propyl-1-heptanol, and add 85g of xylene, heat up to 130°C to dissolve, then heat up to 165°C to keep the liquid out for 45min, then Add 1.5g of tetraisopropyl titanate, and finally raise the temperature to 205°C and keep it warm for 3.5h. When the acid value of the reaction solution to be detected is less than or equal to 0.1mgKOH / g, the esterification is completed;

[0040] (2) Under the condition of 195°C, exhaust the remaining isodecyl alcohol in the reaction system under negative pressure vacuum, and the exhaust time is 2.5h;

[0041] (3) Lower the temperature to 85°C, prepare a solution of 0.15 g of potassium bicarbonate dissolved in 35 g of water, add it to the reaction solution, and stir for 1.5 h to destroy the unhydrolyzed catalyst in the reaction solution.

[0042] (4) Then add 2g of activated carbon, uniformly stir and decolorize for 2h, then add a small amount o...

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Abstract

The invention relates to the technical field of triisodecyl trimellitate, and specifically discloses a method for synthesizing triisodecyl trimellitate, comprising the following steps: esterification reaction, negative pressure dealcoholization, alkali washing and water washing, adsorption decolorization , Hot filtration, oxidation decolorization, secondary adsorption decolorization and secondary hot filtration. The catalyst used in the present invention is a composite inorganic acid ester, which can not only improve the conversion efficiency of raw materials, but also the prepared triisodecyl trimellitate product has the characteristics of high ester content, bright color and stable quality; The obtained product is subjected to further decolorization treatment, so that the chroma of the product can be further reduced, and in addition, the esterification temperature is significantly lowered, which plays a good role in reducing the acid value and reducing energy consumption.

Description

technical field [0001] The invention relates to the technical field of triisodecyl trimellitate, in particular to a method for synthesizing triisodecyl trimellitate. Background technique [0002] A trimellitate plasticizer is an essential plasticizer with high heat resistance and weather resistance. Because of its low volatility, low migration, good electronic resistance and many advantages such as processability, aging resistance, heat resistance, and cold resistance. It can be widely used in PVC products that require high oil resistance, water resistance and heat resistance, and can improve the processing performance of products, fully meeting the requirements of green chemical industry and sustainable development. [0003] With the increasing concern of plasticizers in recent years, the development of new non-toxic and environmentally friendly plasticizers has gradually become the focus of various countries. However, traditional plasticizers, such as phthalate plasticiz...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07C67/08C07C67/48B01J31/02C07C69/76
CPCC07C67/08C07C67/48B01J31/0275B01J31/0272B01J2231/49C07C69/76
Inventor蒋国强孙百亚邹淼赵跃周国君万鹏夏海峰张晓刘丰震骏
OwnerNANTONG BAICHUAN NEW MATERIAL CO LTD