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Preparation method of low-color-number tri(C8-10 alcohol) trimellitate

A technology for trimellitic acid tris and trimellitic anhydride is applied in the field of preparation of low-color trimellitic acid triesters, which can solve the problems of serious equipment corrosion, high impurities and high acid value, and achieve the effects of less waste water and less side reactions.

Pending Publication Date: 2021-03-26
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to provide a preparation method of trimellitate tris(C8-10 alcohol) ester with low color number, which can solve the problem of severe corrosion of equipment when strong acid is used as a catalyst, and many impurities produced by side reactions during esterification. , The color of the product is deepened, the acid value is high, the volume resistivity is low, and the problems affecting product quality

Method used

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  • Preparation method of low-color-number tri(C8-10 alcohol) trimellitate
  • Preparation method of low-color-number tri(C8-10 alcohol) trimellitate
  • Preparation method of low-color-number tri(C8-10 alcohol) trimellitate

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Experimental program
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Effect test

Embodiment 1

[0026] (1) Esterification: 115.3 g of raw material trimellitic anhydride and 389.44 g of C8-10 alcohol are dropped into the reaction kettle, put into under the protection of nitrogen, add 50 g of water-carrying agent xylene, heat up to 120 DEG C under stirring so that the solid trimellitic anhydride is completely dissolved, When the temperature was raised to 170°C, the reaction solution began to produce water, and after 30 minutes, 0.5g of stannous oxide was added, and finally the temperature was raised to 195°C, and the acid value of the reaction solution was measured to be 0.056mgKOH / g when the temperature was kept at 3h;

[0027] (2) Dealcoholization: Stop heating, turn on the vacuum, the vacuum degree is -0.095MPa, use the remaining temperature of the reaction solution to remove most of the excess C8-10 alcohol under stirring, and the vacuum time is 1h;

[0028] (3) Filtration: when the temperature of the above reaction solution is cooled to about 120°C, the solid catalyst ...

Embodiment 2

[0035] (1) Esterification: Put 115.3g of raw materials trimellitic anhydride and 346.2g of C8-10 alcohol into the reaction kettle, and put them into the reactor under the protection of nitrogen. Dissolve, the reaction solution starts to flow out at around 170°C, keep the solution for 60 minutes before adding solid super acid SO 4 2- / ZrO 1.0g, and finally raised the temperature to 200°C, and when the timer was started for 4 hours, the acid value of the reaction solution was measured to be 0.045mgKOH / g;

[0036] (2) Dealcoholization: stop heating, turn on the vacuum, the vacuum degree is -0.095MPa, use the remaining temperature of the reaction solution to remove most of the excess C8-10 alcohol under stirring, and the vacuum time is 0.5h;

[0037] (3) Filtration: when the temperature of the above reaction solution is cooled to about 120°C, the solid catalyst is recovered by filtration while it is hot;

[0038] (4) Oxidation: Add 15.0 g of pre-prepared 12% hydrogen peroxide to...

Embodiment 3

[0044](1) Esterification: Put 115.3g of raw materials trimellitic anhydride and 302.9g of C8-10 alcohol into the reaction kettle, put them into the reactor under nitrogen protection, add 70g of water-carrying mesitylene, heat up to about 120°C under stirring to make the solid trimellitic anhydride completely Dissolve, and the reaction liquid starts to flow out at around 170°C, keep the liquid out for 45 minutes, then add 0.8g of solid stannous chloride, and finally raise the temperature to 205°C, start timing and keep warm for 3.5h, the acid value of the reaction liquid is measured as 0.062mgKOH / g;

[0045] (2) Dealcoholization: stop heating, turn on the vacuum, the vacuum degree is -0.095MPa, use the remaining temperature of the reaction solution to remove most of the excess C8-10 alcohol under stirring, and the vacuum time is 0.5h;

[0046] (3) Filtration: when the temperature of the above reaction solution is cooled to about 120°C, the solid catalyst is recovered by filtrati...

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Abstract

The invention discloses a preparation method of low-color-number tri(C8-10 alcohol) trimellitate, belonging to the technical field of organic chemical production. The method comprises the following steps: esterification: putting raw materials into a reaction kettle, and adding a water-carrying agent and a solid catalyst for a reaction; dealcoholization: starting vacuum, and pumping out most of excessive C8-10 alcohol; filtering: filtering a reaction product in the previous step while the reaction product is still hot to recover the solid catalyst; oxidation: adding hydrogen peroxide; alkali washing: adding an alkaline reagent solution, conducting standing for layering, and removing a water phase; dealcoholization: pumping out residual moisture and C8-10 alcohol; adsorption: adding an adsorbent and a filter aid, namely diatomite; and filtering: filtering a decolorized solution while the decolorized solution is still hot to obtain a filtrate, namely the finished product tri(C8-10 alcohol) trimellitate. The method has the advantages that the solid catalyst is adopted, a dehydrating agent is added, and an oxidizing agent is added, so the high-quality product with a low color number, alow acid value and high volume resistivity can be obtained, less wastewater is generated, the catalyst can be recycled, and the purposes of environmental protection and clean production are achieved.

Description

technical field [0001] The invention relates to the technical field of organic chemical production, in particular to a method for preparing tris(C8-10 alcohol) trimellitate with low color number. Background technique [0002] Trimellitic acid triester plasticizer is a plastic processing aid with excellent performance. These esters are characterized by low volatility, extraction resistance, migration resistance, and similar advantages to polyester plasticizers. At the same time, its Compatibility, processability, low temperature performance, etc. are similar to monomeric phthalates, so it has the characteristics of both monomeric plasticizers and polyester plasticizers. As a heat-resistant and durable plasticizer, it has a wide range of industrial and civil uses. It has been widely used in developed countries such as the United States and Germany. Not only in the plastics industry, but also in automobile manufacturing, civil entertainment and sports venues. Wait. [0003] T...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C67/60C07C67/58C07C67/56C07C69/76
CPCC07C67/08C07C67/48C07C67/60C07C67/58C07C67/56C07C69/76Y02P20/584
Inventor 郑铁江蒋国强孙百亚周国君赵跃缪世军章培伟张晓陶植
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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