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Preparation method of DOA (dioctyl adipate)

A technology of dioctyl adipate and adipic acid, which is applied in the field of preparation of dioctyl adipate, can solve the problems of easy deterioration of tetrabutyl titanate and decline in product quality, and solve the problem of high production cost Effect

Inactive Publication Date: 2018-06-01
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

[0004] In view of this, the purpose of the present invention is to propose a kind of preparation method of dioctyl adipate, it has prevented the generation of tetrabutyl titanate perishable problem in the preparation process, has solved the problem in the production process of dioctyl adipate 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

[0024] A kind of preparation method of dioctyl adipate comprises the steps:

[0025] S1, drop into the raw material alcohol of 1000kg adipic acid and 2000kg in the reactor;

[0026] S2. When the temperature in the reactor rises to 100°C, continue to add 0.8kg of tetrabutyl titanate and 1.8kg of raw material alcohol to the reactor;

[0027] S3. When the temperature in the reactor rises to 125°C, continue to add 1.5kg of tetrabutyl titanate, 0.5kg of tin triisooctoate and 3.0kg of raw material alcohol into the reactor;

[0028] S4. When the temperature in the reactor rises to 160°C, continue to add 1.5kg of tetrabutyl titanate and 2.0kg of raw material alcohol to the reactor;

[0029] S4a. When the temperature in the reaction kettle rises to 170°C, start to add 0.3m of raw material alcohol from the distributor of the fractionation tower. 3 / h save 1.3h;

[0030] S5. When the temperature in the reactor rises to 190°C, continue to add 0.3kg of SiO to the reactor 2 and 0.2kg Al...

Embodiment 2

[0040] A kind of preparation method of dioctyl adipate comprises the steps:

[0041] S1, drop into the raw material alcohol of 1000kg adipic acid and 3000kg in the reactor;

[0042] S2. When the temperature in the reactor rises to 115°C, continue to add 2.0kg of tetrabutyl titanate and 3.0kg of raw material alcohol to the reactor;

[0043] S3. When the temperature in the reactor rises to 135°C, continue to add 3.5kg of tetrabutyl titanate, 1.5kg of tin triisooctoate and 5.0kg of raw material alcohol into the reactor;

[0044] S4. When the temperature in the reactor rises to 170°C, continue to add 3.5kg of tetrabutyl titanate and 2.5kg of raw material alcohol to the reactor;

[0045] S4a. When the temperature in the reaction kettle rises to 177°C, start to add 0.6m of raw material alcohol from the distributor of the fractionation tower. 3 / h save 1.5h;

[0046] S5. When the temperature in the reactor rises to 190°C, continue to add 1.5kg of SiO to the reactor 2 and 0.5kg Al...

Embodiment 3

[0056] A kind of preparation method of dioctyl adipate comprises the steps:

[0057] S1, drop into the raw material alcohol of 1000kg adipic acid and 2500kg in the reactor;

[0058] S2. When the temperature in the reactor rises to 110°C, continue to add 1.5kg of tetrabutyl titanate and 2.2kg of raw material alcohol to the reactor;

[0059] S3. When the temperature in the reactor rises to 130°C, continue to add 2.0kg of tetrabutyl titanate, 1.0kg of tin triisooctoate and 4.0kg of raw material alcohol into the reactor;

[0060]S4. When the temperature in the reactor rises to 165°C, continue to add 2.0kg of tetrabutyl titanate and 2.2kg of raw material alcohol to the reactor;

[0061] S4a. When the temperature in the reaction kettle rises to 175°C, start to add 0.5m of raw material alcohol from the distributor of the fractionation tower. 3 / h save 1.4h;

[0062] S5. When the temperature in the reactor rises to 190°C, continue to add 1.0kg of SiO to the reactor 2 and 0.3kg Al ...

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Abstract

The invention provides a preparation method of DOA (dioctyl adipate). The preparation method comprises the following steps of adding hexanedioic acid and raw alcohol into a reaction kettle; along withthe increasing of temperature, feeding a catalyst (tetrabutyl titanate) and the raw alcohol into the reaction kettle by sections and batches; finally, adding SiO2 and Al2O3; after reaction is finished, dealcoholizing under the vacuum condition; after dealcoholizing is finished, adding Na2CO3; finally, adding activated carbon, sucking and filtering, so as to obtain the product. The preparation method has the advantages that by adding the catalyst and the raw alcohol by multiple times, the easiness in deterioration of the catalyst (tetrabutyl titanate) is avoided, and the adding amount is precisely controlled each time; the problem that the product quality is degraded due to adding of excessive catalyst in the production process because the tetrabutyl titanate is easy to decompose under thewater condition and form esterification reaction to generate water when the tetrabutyl titanate is used as the catalyst; the volume resistivity is improved; the problem of overhigh production cost due to usage of a large amount of catalyst in the production process of DOA is also solved.

Description

technical field [0001] The invention relates to a preparation method of a plasticizer, in particular to a preparation method of dioctyl adipate. Background technique [0002] Dioctyl adipate (DOA) is a cold-resistant plasticizer that can improve the low-temperature flexibility and impact resistance of polymers, and is widely used as a plasticizer in agricultural films, artificial leather, frozen food packaging, and synthetic rubber . [0003] In the existing dioctyl adipate preparation process, because tetrabutyl titanate as a catalyst is easily decomposed by water, an esterification reaction occurs and water is generated. In order to deal with this problem, the solution is to add more tetrabutyl titanate to supplement the tetrabutyl titanate that has been reacted, but adding too much tetrabutyl titanate will cause the quality of the product to decline. In addition, such treatment The method will increase the production cost. Contents of the invention [0004] In view o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C67/56C07C69/44
CPCC07C67/08C07C67/48C07C67/56C07C69/44
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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