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Method for refining dibasic acid dimethyl ester plasticizer

A technology of dimethyl dibasic acid and refining method, which is applied in the refining field of aliphatic dibasic acid dimethyl ester plasticizer, can solve the problem of unstable impurity content and acid value, inability to further recover monoester, and poor product quality. Stability and other issues, to achieve the effect of clear segmentation, increased variety, and high product yield

Active Publication Date: 2009-09-09
WEIFANG YUANLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since there are many impurities in the plasticizer crude product obtained after the reaction, the distillation process adopts the method of batch rectification, and impurities such as methanol and water are sequentially distilled from the top of the tower, and then the plasticizer product dimethyl succinate Esters, dimethyl glutarate and dimethyl adipate mixture are steamed from the top of the tower, and batch rectification and refining plasticizer products have the following defects: 1. The product quality is unstable, and the impurity content and The acid value is unstable; 2. The energy consumption is large, and the reflux ratio required to reach the target is large; 3. There is a transitional fraction section in the intermittent distillation, and the yield is reduced; 4. The residence time of the monoester in the tower tank is too long, resulting in the generation of a large amount of tar , resulting in blockage of equipment, frequent cleaning, and increased labor costs. 5. Monoesters cannot be further recovered, resulting in a decrease in product yield; 6. Tar cannot be processed, causing serious pollution problems

Method used

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  • Method for refining dibasic acid dimethyl ester plasticizer

Examples

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Effect test

Embodiment 1

[0023] As shown in the attached figure, the crude plasticizer synthesized from nylon acid (containing succinic acid, glutaric acid and adipic acid) obtained from the mother liquor of adipic acid is used as raw material, and the crude plasticizer contains methanol 2% by weight, 1% by weight of water, 80% by weight of dimethyl dibasic acid, 14% by weight of monomethyl ester, 2% by weight of impurities such as tar, etc. The crude plasticizer 1 enters the light removal tower after being filtered. The light removal tower is operated under reduced pressure, the operating pressure is 20kPa, and the operating temperature at the top of the tower is 120°C. The gas phase light component 3 is removed by the light removal tower. The light component 3 is mainly composed of methanol, water and dimethyl succinate. After condensation, it enters the oil-water separator and is divided into two liquid phases. Methanol and water 4 are in the upper layer It is the water phase, and the dimethyl suc...

Embodiment 2

[0026] As shown in the attached figure, the crude plasticizer synthesized from nylon acid (containing succinic acid, glutaric acid and adipic acid) obtained from the mother liquor of adipic acid is used as raw material, and the crude plasticizer contains methanol 2% by weight, 1% by weight of water, 80% by weight of dimethyl dibasic acid, 14% by weight of monomethyl ester, 2% by weight of impurities such as tar, etc. The crude plasticizer 1 enters the light removal tower after being filtered. The light removal tower is operated under reduced pressure, the operating pressure is 10kPa, and the operating temperature at the top of the tower is 104°C. The gas phase light component 3 is removed by the light removal tower. The light component 3 is mainly composed of methanol, water and dimethyl succinate. After condensation, it enters the oil-water separator and is divided into two liquid phases. Methanol and water 4 are in the upper layer It is the water phase, and the dimethyl suc...

Embodiment 3

[0029]The process steps are the same as in Example 2, except that the weight-removing tower is provided with two side lines, the reflux ratio is 1.0, and the plasticizer product at the top of the weight-removing tower contains: 34% by weight of dimethyl succinate, 64% by weight of dimethyl glutarate , dimethyl adipate 1% by weight, monoester total content 1ppm, the plasticizer product that the lower part extracts from the side line at 15 theoretical plates contains: dimethyl succinate 3% by weight, dimethyl glutarate 21 % by weight, 75% by weight of dimethyl adipate, 10ppm of total monoester content, and the upper part contains 25% by weight of dimethyl succinate, dimethyl glutarate, and 40 theoretical boards. 52% by weight of ester, 22% by weight of dimethyl adipate, and a total monoester content of 20ppm. After the above process, three grades of plasticizers are obtained. Impurities such as methanol and water are below 1ppm, and the content of monomethyl ester is 20ppm. The ...

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Abstract

The invention discloses a method for refining a dibasic acid dimethyl ester plasticizer, which comprises the following steps: dibasic acid dimethyl ester plasticizer crude product is refined by adopting a continuous decompression and rectification light-component and heavy-component removing method, after being filtered, the plasticizer crude product firstly enters a lightness-removing column, the lightness-removing column performs decompression operation to remove light components on the top of the lightness-removing column, the bottom materials of the lightness-removing column enter a weight-removing column to remove weight components, the weight-removing column performs decompression operation to remove monoester and little tar in the plasticizer crude product, and the top of the weight-removing column extracts the refined plasticizer produce. The plasticizer product has high purity, stable quality, lower energy consumption, simple operation and high product yield and reduces the generation of tar and environmental pollution.

Description

technical field [0001] The invention belongs to chemical separation engineering, and relates to a method for refining an aliphatic dibasic acid dimethyl plasticizer synthesized from nylon acid in adipic acid mother liquor by adopting a continuous rectification method. Background technique [0002] Aliphatic dibasic acid ester plasticizer has the characteristics of excellent low temperature performance, good impact resistance, good plasticizing efficiency and viscosity performance, and is currently mainly used as a plasticizer to improve low temperature performance. Because the price of aliphatic dibasic acid is higher, the cost of aliphatic dibasic acid ester is also higher, so the nylon acid (containing succinic acid, glutaric acid and adipic acid) obtained in the mother liquor of adipic acid ) as a raw material for plasticizers has attracted people's attention. The production process of fatty dibasic acid esters is roughly the same. Taking sulfuric acid catalysis as an ex...

Claims

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Application Information

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IPC IPC(8): C08K5/11C07C67/54
Inventor 刘修华杨辉谭立文秦国栋
Owner WEIFANG YUANLI CHEM
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