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Method for preparing triisononyl trimellitate (TINTM)

A technology of trimellitic acid and trimellitic anhydride, which is applied to the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of sewage, serious environmental pollution, and large energy consumption, and reduce waste water Quantity, good product quality, and the effect of reducing energy consumption

Inactive Publication Date: 2011-02-16
昆山合峰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Therefore, triisononyl trimellitate (TINTM) is more suitable for wire and cable products that require anti-aging properties and heat resistance. However, the current production of triisononyl trimellitate (TINTM) consumes energy Larger, the reaction produces a large amount of sewage, and the environment is seriously polluted

Method used

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  • Method for preparing triisononyl trimellitate (TINTM)
  • Method for preparing triisononyl trimellitate (TINTM)
  • Method for preparing triisononyl trimellitate (TINTM)

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment one: at 16m 3 3000Kg of trimellitic anhydride, 7875Kg of isononyl alcohol (feeding ratio of 1:3.5mol), 4.5Kg of activated carbon were put into the stainless steel reaction kettle, and the temperature was stirred, and when the mixture was heated to 185°C, titanic acid with a mass ratio of 1:1 was added Tetrabutyl ester and tetraisopropyl titanate mixed catalyst 3Kg, continue to react at 185°C to 240°C for 4 hours, dealcoholize under negative pressure, add sodium hydroxide solution with a concentration of 10% by mass for neutralization, and make the mixture acidic When it reaches below 0.07mgKOH / g, the esterified water is treated by layering to remove the oil layer, and the treated esterified water is passed into the reactor as an entrainer to dealcoholize and refine. White clay and 20Kg diatomaceous earth were stirred for 30 minutes, and filtered to obtain the finished product.

example example 2

[0030] Example 2: At 16m 3 3000Kg of trimellitic anhydride, 9000Kg of isononyl alcohol (feeding ratio of 1:4.0mol), 4.5Kg of activated carbon were put into the stainless steel reaction kettle, and the mixture was heated to 190°C, and titanic acid was added in a mass ratio of 1:2.5 Tetrabutyl ester and tetraisopropyl titanate mixed catalyst 4Kg, continue to react at 190°C to 240°C for 3.5 hours, dealcoholize under negative pressure, and neutralize with 10% sodium hydroxide solution by mass percentage to make the mixture acidic When it reaches below 0.07mgKOH / g, the esterification water is treated by layering to remove the oil layer, and the treated esterification water is passed into the reactor as an entrainer for dealcoholization and refining, and the temperature is lowered to 150°C, and 10Kg of dried activated clay and 20Kg of diatomaceous earth was stirred for 30 minutes, and filtered to obtain the finished product.

example example 3

[0031] Example 3: At 16m 3 3000Kg of trimellitic anhydride, 10125Kg of isononyl alcohol (feeding ratio is 1:4.5mol), 4.5Kg of activated carbon were put into the stainless steel reaction kettle, and the mixture was heated up to 195°C, and titanic acid with a mass ratio of 1:4 was added. Tetrabutyl ester and tetraisopropyl titanate mixed catalyst 5Kg, continue to react at 195°C to 240°C for 3.0 hours, dealcoholize under negative pressure, and neutralize with 10% sodium hydroxide solution by mass percentage to make the mixture acidic When it reaches below 0.07mgKOH / g, the esterification water is treated by layering to remove the oil layer, and the treated esterification water is passed into the reactor as an entrainer for dealcoholization and refining, and the temperature is lowered to 150°C, and 10Kg of dried activated clay and 20Kg of diatomaceous earth was stirred for 30 minutes, and filtered to obtain the finished product.

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Abstract

The invention discloses a method for preparing triisononyl trimellitate (TINTM), comprising the following steps: adding trimellitic acid anhydride and isononyl alcohol with a mole ratio of 1:3.5-1:4.5 as well as activated carbon the weight of which is 0.1-0.3% of the weight of the trimellitic acid anhydride into a reaction kettle; stirring the mixture and raising the temperature to 185-195 DEG C; then, adding catalyst the weight of which is 0.05-0.2% of the weight of the trimellitic acid anhydride, continuing to raise the temperature to 185-245 DEG C and reacting for 3-4 hours; controlling the acid value to be below 0.50mgKOH / g, and carrying out negative pressure dealcoholization until no return liquid exists; adding sodium hydroxide solution with the mass percent concentration of 10-15%, and controlling the acid value to be below 0.07mgKOH / g; introducing water into the reaction kettle to serve as an entrainer, and carrying out dealcoholization refining; and lowering the temperature to 150 DEG C, adding dried atlapulgite the weight of which is 0.07-0.2% of the total mass of the end product, evenly mixing and filtering. The method of the invention has the characteristics of no pollution, low energy consumption, short process time, high efficiency and good product quality.

Description

technical field [0001] The invention relates to a preparation method of a plasticizer, in particular to a preparation method of triisononyl trimellitate. Background technique [0002] The volatility, extraction resistance and migration resistance of trimellitate all have the advantages similar to polyester plasticizers, and at the same time, its compatibility, processability and low temperature performance are similar to monomeric phthalates Ester, so it has the advantages of both monomeric plasticizer and polymeric plasticizer. It is widely used as a heat-resistant and durable plasticizer. At present, it is mainly used in 105°C grade cable materials. Trioctyl trimellitate (TOTM), a representative of trimellitate, cannot meet the requirements in some fields, especially in wire and cable products with aging characteristics and heat resistance required by UL62 or UL1581, while trimellitic acid Compared with trioctyl trimellitate (TOTM), triisononyl formate (TINTM) has the fol...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/76B01J31/02
Inventor 程正勇
Owner 昆山合峰化工有限公司
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