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Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester

A technology of dialkyl succinate and succinic acid, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve the problem of large sewage discharge, accelerated resin saturation, production scale and application constraints of succinic acid And other issues

Inactive Publication Date: 2010-06-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to cost and environmental pollution, the production scale and application of succinic acid are greatly restricted by petrochemical legal system
In the microbial fermentation method, a large amount of calcium and magnesium salts need to be added during the fermentation process to control the normal progress of the fermentation, so the high content of ionic substances accelerates the saturation of the resin, increases the number of resin regenerations, and causes problems such as large sewage discharge.

Method used

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  • Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester
  • Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester
  • Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The raw material is pure dibutyl 1,4-succinate

[0036] 1,4-dibutyl succinate inlet: 4

[0037] Reactive distillation tower temperature: 210°C

[0038] Reaction tower pressure: 1.9MPa

[0039] Reaction tower kettle temperature: 190°C

[0040] Steam generator temperature: 190°C

[0041] 1,4-dibutyl succinate conversion rate: close to 100%

[0042]

[0043] The bottom stream composition (weight percent) at the bottom of the tower:

[0044] 1,4-dibutyl succinate: close to 0.0%

[0045] 1,4-Monobutyl succinate: close to 0.0%

[0046] 1,4-dibutyl succinate: 25.80%

[0047] Water: 74.20%

[0048] The top stream composition (percentage by weight) at the top of the tower:

[0049] Butanol: 6.43%

[0050] Water: 93.57%

Embodiment 2

[0052] The raw material is pure dibutyl 1,4-succinate

[0053] 1,4-dibutyl succinate inlet: 4

[0054] Reactive distillation tower temperature: 190°C

[0055] Reaction tower pressure: 1.2MPa

[0056] Reaction tower kettle temperature: 190°C

[0057] Steam generator temperature: 190°C

[0058] 1,4-dibutyl succinate conversion rate: close to 100%

[0059]

[0060] The bottom stream composition (weight percent) at the bottom of the tower:

[0061] 1,4-dibutyl succinate: close to 0.0%

[0062] 1,4-Monobutyl succinate: close to 0.0%

[0063] 1,4-Succinic acid: 22.94%

[0064] Water: 77.06%

[0065] The top stream composition (percentage by weight) at the top of the tower:

[0066] Butanol: 5.36%

[0067] Water: 94.64%

Embodiment 3

[0069] The raw material is pure dibutyl 1,4-succinate

[0070] 1,4-dibutyl succinate inlet: 3

[0071] Reactive distillation tower temperature: 190°C

[0072] Reaction tower pressure: 1.2MPa

[0073] Reaction tower kettle temperature: 190°C

[0074] Steam generator temperature: 190°C

[0075] 1,4-dibutyl succinate: close to 100%

[0076]

[0077] The bottom stream composition (weight percent) at the bottom of the tower:

[0078] 1,4-dibutyl succinate: close to 0.0%

[0079] 1,4-Monobutyl succinate: grade 0.0%

[0080] 1,4-Succinic acid: 48.58%

[0081] Water: 51.42%

[0082] The top stream composition (percentage by weight) at the top of the tower:

[0083] Butanol: 8.26%

[0084] Water: 91.74%

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Abstract

A device and a method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester, wherein the method comprises: preheating a raw material which contains dialkyl succinate ester to the temperature of between 30 and 200 DEG C and selecting feeding holes with different heights to input the pre-heated raw material into a reaction distillation tower; making reaction water which is preheated to the temperature of between 30 and 200 DEG C and water which produces stripping steam enter the reaction distillation tower from water vapor on the lower part of the reaction distillation tower through a vapor generator, wherein the weight ratio of the dialkyl succinate ester to the water is 1:1-1:5; at the hydrolysis reaction temperature of between 140 and 350 DEG C, hydrolyzing the dialkyl succinate ester into volatile alcohol and less volatile butane diacid; exporting the alcohol from a top product outlet of the reaction distillation tower and condensing and recycling the alcohol; and exporting the butane diacid to a column reactor from a bottom discharge hole of the reaction distillation tower and separating out solid butane diacid through a separating unit. Complete hydrolysis of the dialkyl succinate ester can be realized by the control of reaction conditions and a process.

Description

technical field [0001] The present invention relates to a method for hydrolyzing dialkyl succinates into succinic acid and corresponding alcohols by reactive distillation in the absence of acidic (or basic) catalysts. [0002] The invention also relates to a device for implementing the above method. Background technique [0003] 1,4-Succinic acid, also known as succinic acid, is a dibasic organic acid. It is an important C4 platform compound. It is mainly used as a fluxing acid in electronic chemicals, soldering flux, and solder paste. It has good soldering and acidizing activity, and can improve the soldering ability and prepare high-quality rosin-type and environment-friendly flux with good solderability when combined with adipic acid, certain surfactants and some additives. Succinic acid is used in the chemical industry to produce dyes, alkyd resins, glass fiber reinforced plastics, ion-interaction resins, and pesticides; in the pharmaceutical industry, it is used to syn...

Claims

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Application Information

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IPC IPC(8): C07C55/10C07C51/09
Inventor 严丽丁云杰郁俊冬程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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