Continuous esterification production method for mixed dibasic acid dimethyl ester

A technology of dimethyl dibasic acid and a production method, which is applied in the field of continuous esterification production of mixed dibasic acid dimethyl ester, can solve the problem of unstable impurity content and acid value, inability to handle high molecular polymers, intermittent esterification Incomplete reaction and other problems, to achieve the effect of reducing reaction heating time, reducing equipment investment and improving reaction conversion rate

Inactive Publication Date: 2010-11-24
WEIFANG YUANLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. Intermittent esterification has high energy consumption, low product yield, unstable quality, and unstable impurity content and acid value in different batches of products;
[0006] 2. The intermittent esterification reaction is not complete and the product yield is low;
[0007] 3. The residence time of the mixed acid in the esterification tank is too long, resulting in the formation of a large amount of polymers, resulting in a decrease in product yield, blockage of equipment, frequent cleaning, and increased labor costs;
[0008] 4. The high molecular polymer produced by the reaction cannot be processed, causing serious pollution problems;
[0009] 5. Methanol has a lot of loss and high consumption during the reaction process;
[0010] 6. The output of intermittent production is low, which is not conducive to large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Using the mixed dibasic acid (containing 20wt% succinic acid, 50wt% glutaric acid, 29wt% adipic acid, and 1wt% impurities) obtained from the mother liquor of adipic acid and methanol as raw materials, the mixed dibasic acid and Methanol is mixed in a pre-esterification kettle at a molar ratio of 1:2, and pre-esterified under normal temperature and pressure to obtain a pre-esterified material.

[0031] The methanol is pressurized and preheated to 135°C with a pressurized preheater, and then heated to a superheated methanol gas of 150°C with a steam heater through hot steam.

[0032] In the continuous esterification tower of a fixed-bed reactor with a catalyst ferric chloride in the middle, the added amount of the catalyst ferric chloride is 10wt% of the mixed dibasic acid, and the pre-esterified material is driven from a magnetically driven pump from The top of the continuous esterification tower is fed, and the pre-esterified material passes through the fixed-bed reactor loa...

Embodiment 2

[0034] Using the mixed dibasic acid (containing 25% succinic acid, 53% glutaric acid, 20% adipic acid, and 2% impurities) obtained from the mother liquor of adipic acid and methanol as raw materials, the mixed dibasic acid and Methanol is mixed in a pre-esterification kettle at a molar ratio of 1:2.2, and pre-esterified under normal temperature and pressure to obtain a pre-esterified material.

[0035] The methanol is pressurized and preheated to 137°C with a pressurized preheater, and then heated to 152°C overheated methanol gas with a steam heater through hot steam.

[0036] In the continuous esterification tower of a fixed-bed reactor with a catalyst sodium bisulfate in the middle, the added amount of the catalyst sodium bisulfate is 8wt% of the mixed dibasic acid, and the pre-esterified material is driven from the continuous ester by a magnetic drive pump. The pre-esterified material passes through the fixed bed reactor loaded with sodium bisulfate from the top under gravity, a...

Embodiment 3

[0038] Using the mixed dibasic acid (containing 15% succinic acid, 38% glutaric acid, 45% adipic acid, and 2% impurities) obtained from the mother liquor of adipic acid and methanol as raw materials, the mixed dibasic acid and Methanol is mixed in a pre-esterification kettle at a molar ratio of 1:2.5, and pre-esterified under normal temperature and pressure to obtain a pre-esterified material.

[0039] The methanol is pressurized and preheated to 134°C with a pressurized preheater, and then heated to a superheated methanol gas of 148°C with a steam heater through hot steam.

[0040] In the continuous esterification tower of a fixed-bed reactor with a catalyst ferric chloride in the middle, the addition amount of the catalyst ferric chloride is 12wt% of the mixed dibasic acid, and the pre-esterified material is driven by a magnetic force from the pump The top of the continuous esterification tower is fed, and the pre-esterified material passes through the fixed-bed reactor loaded wi...

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PUM

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Abstract

The invention discloses a continuous esterification production method for mixed dibasic acid dimethyl ester. The method comprises the following steps of: (1) pre-esterifying, namely, mixing dibasic acid and methanol in a mole ratio of 1:2-3 and performing pre-esterification at the normal temperature and normal pressure to obtain a pre-esterified material; (2) pre-heating the methanol, namely, pressurizing and pre-heating the methanol to form overheated methanol gas with the temperature of between 145 and 155 DEG C; and (3) continuously esterifying, namely, adding the pre-esterified material into a continuous esterification reactor, of which the middle part is provided with a catalyst reaction bed, from the top, adding the overheated methanol gas into the continuous esterification reactor from the bottom, performing a reverse flow reaction on the ascending methanol gas and the descending pre-esterified material on the catalyst reaction bed, and continuously discharging the mixed dibasic acid dimethyl ester which is generated by the esterification from the bottom of the esterification reactor.

Description

Technical field [0001] The invention relates to the technical field of esterification synthesis, in particular to a continuous esterification production method of dimethyl mixed dibasic acid. Background technique [0002] Mixed Dimethyl Dibasic Acid (MDBE) is a kind of high boiling point solvent, which is the by-product dicarboxylic acid (C4, C5, C6 mixed dibasic acid) and methanol esterified by the production of adipic acid. . MDBE solvent has the characteristics of high boiling point, uniform distillation, mild odor, low toxicity and biodegradability. It has super dissolving ability and is called a universal solvent. It is compatible with polyurethane resin, acrylic resin, polyester resin, and epoxy resin. It has excellent compatibility and can widely replace ketones (such as cyclohexanone, isophorone, etc.), ethers (such as ethylene glycol monobutyl ether, propylene glycol monomethyl ether, etc.), and esters (such as glycol ethyl ether) Acetate, propylene glycol methyl ether...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/003
Inventor 张敏刘修华杨辉谭立文秦国栋
Owner WEIFANG YUANLI CHEM
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