Preparation method for dimethyl sebacate

A technology of dimethyl sebacate and sebacic acid, which is applied in the field of preparation of dimethyl sebacate to achieve the effects of reducing production costs, reducing costs and prolonging service life

Active Publication Date: 2012-02-15
SHANDONG TIANXING BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method adopts three-step esterification, and the steps are complicated, and the amount of methanol is relatively large. The ratio of sebacic acid to methanol is 1:2-3, and in the actual reaction, the amount of methanol is excessive, so The cost of producing dimethyl sebacate in this method is relatively high; in addition, the catalyst used is concentrated sulfuric acid, the cost is relatively high, and the operation of the staff also has certain dangers
In addition, if concentrated sulfuric acid is used as a catalyst, the color of the obtained product is not good. At the same time, concentrated sulfuric acid is easy to corrode equipment, and produces a large amount of acidic waste liquid to pollute the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of dimethyl sebacate comprises the following steps:

[0037] Esterification reaction

[0038] (1) Prepare materials according to the following molar ratio: sebacic acid: methanol: catalyst = 1: 0.9: 0.004;

[0039] (2) Get 30% of the total mass fraction of methanol in step 1 and add it into the esterification kettle, close the alcohol release door, open the agitator again, drop into all the sebacic acid prepared in step 1, and add the solid catalyst SiO 2 -Al 2 o 3 ; Its addition is 0.15% of the mass fraction of sebacic acid, close the lid tightly, and open the recorder;

[0040] (3) Open the steam valve to raise the temperature until the liquid temperature reaches about 70°C and keep it warm for 1 hour, then carry out the first esterification reaction, the esterification time is 3-4 hours, after the first esterification reaction, continue to heat up to 90°C and start alcohol distillation;

[0041] (4) When the temperature rises to 110-125°C, ...

Embodiment 2

[0049] The preparation method of dimethyl sebacate comprises the following steps:

[0050] Esterification reaction

[0051] (1) Prepare materials according to the following molar ratio: sebacic acid: methanol: catalyst = 1: 1: 0.005;

[0052] (2) Take 30% of the total mass fraction of methanol in step 1 and add it to the esterification kettle, close the alcohol release door, open the agitator, put all the sebacic acid prepared in step 1, and add solid catalyst B 2 o 3 -Al 2 o 3 ; Its addition is 0.15% of the mass fraction of sebacic acid, close the lid tightly, and open the recorder;

[0053] (3) Open the steam valve and raise the temperature until the liquid temperature reaches about 80°C, keep it warm for 1 hour, and carry out the first esterification reaction. The esterification time is about 3 hours. After the first esterification reaction, continue to heat up to 90°C and start alcohol distillation;

[0054] (4) When the temperature rises to 120°C, continue to add alcoh...

Embodiment 3

[0062] The preparation method of dimethyl sebacate comprises the following steps:

[0063] Esterification reaction

[0064] (1) Prepare materials according to the following molar ratio: sebacic acid: methanol: catalyst = 1: 1.1: 0.004;

[0065] (2) Get 40% of the total mass fraction of methanol in step 1 and add it into the esterification kettle, close the alcohol release door, open the agitator again, drop into all the sebacic acid prepared in step 1, and add the solid catalyst SiO 2 -Al 2 o 3 ; Its addition is 0.15% of the mass fraction of sebacic acid, close the lid tightly, and open the recorder;

[0066] (3) Open the steam valve to raise the temperature until the liquid temperature reaches about 85°C, keep it warm for 1 hour, and carry out the first esterification reaction. The esterification time is 3 to 4 hours. After the first esterification reaction, continue to heat up to 90°C and start alcohol distillation;

[0067] (4) When the temperature rises to 110°C, start...

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PUM

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Abstract

The invention belongs to the field of chemical product preparation and particularly relates to a preparation method for dimethyl sebacate. A production method for the dimethyl sebacate comprises the following steps of esterification reaction and rectification process and has the concrete steps that: sebacic acid is mixed with methanol, then, solid catalysts are added, the esterification reaction is carried out, and then, products are purified through a rectification process. The method has the beneficial effect that the consumption mol ratio of the sebacic acid to the methanol is 1 / 0.9 to 1.2. Compared with the prior art, the method has the advantages that the consumption of the methanol is greatly saved, about 3 percent of the cost is saved, the solid acid is used as catalysts, the reaction efficiency is greatly improved, in addition, compared with the prior art adopting concentrated sulfuric acid as catalysts, the method has the advantage that the solid catalysts adopted by the method can be cyclically utilized, and compared with the method adopting liquid catalysts, the method has the advantage that about 5 percent of the cost is saved.

Description

technical field [0001] The invention belongs to the field of chemical product preparation, and in particular relates to a method for preparing dimethyl sebacate. Background technique [0002] At present, the method for preparing dimethyl sebacate is mainly to mix sebacic acid and methanol in a certain proportion. Under the action of a catalyst, after the sebacic acid is completely dissolved, carry out esterification reaction, and wait until the temperature drops to the solution to form an interface. Afterwards, separate the aqueous phase; then add sebacic acid and methanol to carry out the second step esterification esterification reaction, in the above esterification reaction, the catalyst generally used is concentrated sulfuric acid, with liquid as the catalyst, which cannot be recovered. Not only the cost is higher, but also the operator has certain danger when working. [0003] CN1025916C discloses a kind of preparation method of dimethyl sebacate, this method is to t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/50C07C67/08
Inventor 怀进步
Owner SHANDONG TIANXING BIOTECH
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