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Preparation method of dioctyl sebacate

A technology of dioctyl sebacate and sebacic acid, which is applied in the field of preparation of dioctyl sebacate, can solve the problems of product quality decline, easy deterioration of tetrabutyl titanate and the like, and achieves the effect of slow heating

Inactive Publication Date: 2018-09-21
珠海市高栏联合新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the purpose of the present invention is to propose a kind of preparation method of dioctyl sebacate, it has prevented the generation of tetrabutyl titanate perishable problem in the preparation process, has solved the problem in the production process of dioctyl sebacate Excessive use of catalyst causes the problem of product quality decline and saves costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of dioctyl sebacate comprises the steps:

[0026] S1, drop into the raw material alcohol of 5000kg sebacic acid and 8000kg in the reactor;

[0027] S2. When the temperature in the reactor rises to 100°C, continue to add 5.0kg of tetrabutyl titanate and 12.0kg of alcohol to the reactor;

[0028] S3. When the temperature in the reactor rises to 125°C, continue to add 10.0kg of tetrabutyl titanate, 3.5kg of tin triisooctoate and 20.0kg of alcohol into the reactor;

[0029] S4. When the temperature in the reactor rises to 160°C, continue to add 10.0kg of tetrabutyl titanate and 15.0kg of alcohol to the reactor;

[0030] S4a. When the temperature in the reaction kettle rises to 170°C, start to add 2.5m of raw material alcohol from the distributor of the fractionation tower. 3 / h save 1.5h;

[0031] S5. When the temperature in the reactor rises to 185°C, continue to add 2.5kg of SiO to the reactor 2 and 1.8kg Al 2 o 3 ;

[0032] S6, pump to...

Embodiment 2

[0042] A kind of preparation method of dioctyl sebacate comprises the steps:

[0043] S1, drop into the raw material alcohol of 5000kg sebacic acid and 12000kg in the reactor;

[0044] S2. When the temperature in the reactor rises to 115°C, continue to add 12.0kg of tetrabutyl titanate and 21.0kg of raw material alcohol to the reactor;

[0045] S3. When the temperature in the reactor rises to 135°C, continue to add 20.0kg of tetrabutyl titanate, 10.0kg of tin triisooctoate and 35.0kg of raw material alcohol into the reactor;

[0046] S4. When the temperature in the reactor rises to 170°C, continue to add 25.0kg of tetrabutyl titanate and 20.0kg of raw material alcohol into the reactor;

[0047] S4a. When the temperature in the reaction kettle rises to 177°C, start to add 1.5m of raw material alcohol from the distributor of the fractionation tower. 3 / h save 1.5h;

[0048] S5. When the temperature in the reactor rises to 190°C, continue to add 8.0kg of SiO to the reactor 2 ...

Embodiment 3

[0058] A kind of preparation method of dioctyl sebacate comprises the steps:

[0059] S1, drop into the raw material alcohol of 5000kg sebacic acid and 10500kg in the reactor;

[0060] S2. When the temperature in the reactor rises to 105°C, continue to add 8.0kg of tetrabutyl titanate and 15.0kg of raw material alcohol to the reactor;

[0061] S3. When the temperature in the reactor rises to 130°C, continue to add 13.0kg of tetrabutyl titanate, 6.0kg of tin triisooctoate and 30.0kg of raw material alcohol into the reactor;

[0062] S4. When the temperature in the reactor rises to 165°C, continue to add 15.0kg of tetrabutyl titanate and 15.0kg of raw material alcohol to the reactor;

[0063] S4a. When the temperature in the reaction kettle rises to 175°C, start to add 2.0m of raw material alcohol from the distributor of the fractionation tower. 3 / h save 1.5h;

[0064] S5. When the temperature in the reactor rises to 185°C, continue to add 3.5.0kg of SiO to the reactor 2 an...

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Abstract

The invention provides a preparation method of dioctyl sebacate. Sebacic acid and raw alcohol are added into a reaction kettle, then, along with increase of temperature, and a catalyst-tetrabutyl titanate and capryl alcohol are added into the reaction kettle in batches section by section; finally, SiO2 and Al2O3 are added, after the reaction is ended, vacuum dealcoholization is performed, after dealcoholization is ended, Na2CO3 is added, and finally activated carbon is added to perform suction filtration to obtain dioctyl sebacate. The catalyst and capryl alcohol are added separately and repeatedly, the catalyst-tetrabutyl titanate is likely to go bad, each added quantity is precisely controlled, the problems that in the prior art, due to the fact that tetrabutyl titanate is adopted a catalyst and is easily decomposed when meeting water, and an esterification reaction can generate water, and excessive catalysts need to be added in the production process, and the product quality is lowered are solved; in addition, the problem that the production cost is excessively high due to the fact that the consumption of the catalysts in the DOS production process is excessively large is further solved.

Description

technical field [0001] The invention relates to a preparation method of a plasticizer, in particular to a preparation method of dioctyl sebacate. Background technique [0002] Dioctyl sebacate (DOS), also known as dioctyl sebacate (bis(2-ethylhexyl) sebacate), bis-2-ethylhexyl sebacate, molecular formula: C 26 h 50 o 4 , the molecular weight is 426.66. It is light yellow liquid in standard state, slightly soluble in water, easily soluble in ethanol and ether. It is the raw material for making nylon-610 fiber and nylon-9 fiber. Its esters are plasticizers in the plastics industry. [0003] The preparation method of existing dioctyl sebacate is: sebacic acid and octanol (mass ratio 1: 1.6) carry out esterification under the catalysis of sulfuric acid (0.25% of the total mass of sebacic acid and octanol), First generate monooctyl ester, this step of esterification is relatively easy. The second step produces a diester, which is more difficult. To control the higher temp...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/50
CPCC07C67/08C07C69/50
Inventor 黄涛任海澜
Owner 珠海市高栏联合新材料有限公司
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