Method and device for preparing carboxylic acids by hydrolysis of polybasic carboxylic acid ester

A polycarboxylic acid ester and carboxylic acid ester technology, which is applied in the fields of chemistry, materials and mechanical science, can solve the problems of catalyst regeneration, replacement and recovery difficulties, and troublesome catalyst production and filling methods, so as to achieve the effect of excellent technical effect.

Active Publication Date: 2008-09-03
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

The use of resin catalysts still has problems such as troublesome preparation and loading of catalysts, difficulties in regeneration, replacement and recycling of catalysts, etc.

Method used

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  • Method and device for preparing carboxylic acids by hydrolysis of polybasic carboxylic acid ester
  • Method and device for preparing carboxylic acids by hydrolysis of polybasic carboxylic acid ester
  • Method and device for preparing carboxylic acids by hydrolysis of polybasic carboxylic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] The raw material is pure dimethyl 1,4-cyclohexanedicarboxylate

[0078] Carboxylate feed inlet: 4 (the number 4 refers to the number of feed inlets and the number of segments for segmented feeding)

[0079] Reactive distillation tower temperature: 200°C

[0080] Reaction tower pressure: 1.5MPa

[0081] Reactor tower kettle temperature: 165°C

[0082] Steam generator temperature: 170°C

[0083] Dimethyl 1,4-cyclohexanedicarboxylate conversion rate: 100%

[0084]

[0085] The bottom stream composition (weight percent) at the bottom of the tower:

[0086] Dimethyl 1,4-cyclohexanedicarboxylate: 0.0%

[0087] 1,4-Cyclohexanedicarboxylic acid monomethyl ester: 0.0%

[0088] 1,4-Cyclohexanedicarboxylic acid: 25.80%

[0089] Water: 74.20%

[0090] The top stream composition (percentage by weight) at the top of the tower:

[0091] Methanol: 5.33%

[0092] Water: 94.67%.

Embodiment 2

[0094] The raw material is pure dimethyl 1,4-cyclohexanedicarboxylate

[0095] Carboxylate feed ports: 4

[0096] Reactive distillation tower temperature: 170°C

[0097] Reaction tower pressure: 0.80MPa

[0098] Reactor tower kettle temperature: 165°C

[0099] Steam generator temperature: 170°C

[0100] Dimethyl 1,4-cyclohexanedicarboxylate conversion rate: 100%

[0101]

[0102] The bottom stream composition (weight percent) at the bottom of the tower:

[0103] Dimethyl 1,4-cyclohexanedicarboxylate: 0.0%

[0104] 1,4-Cyclohexanedicarboxylic acid monomethyl ester: 0.0%

[0105] 1,4-Cyclohexanedicarboxylic acid: 22.94%

[0106] Water: 77.06%

[0107] The top stream composition (percentage by weight) at the top of the tower:

[0108] Methanol: 4.41%

[0109] Water: 95.59%.

Embodiment 3

[0110] Embodiment 3 (ester water ratio is 1: 6)

[0111] The raw material is pure dimethyl 1,4-cyclohexanedicarboxylate

[0112] Carboxylate feed ports: 3

[0113] Reactive distillation tower temperature: 170°C

[0114] Reaction tower pressure: 0.80MPa

[0115] Reactor tower kettle temperature: 165°C

[0116] Steam generator temperature: 170°C

[0117] Dimethyl 1,4-cyclohexanedicarboxylate conversion rate: 100%

[0118]

[0119] The bottom stream composition (weight percent) at the bottom of the tower:

[0120] Dimethyl 1,4-cyclohexanedicarboxylate: 0.0%

[0121] 1,4-Cyclohexanedicarboxylic acid monomethyl ester: 0.0%

[0122] 1,4-Cyclohexanedicarboxylic acid: 48.58%

[0123] Water: 51.42%

[0124] The top stream composition (percentage by weight) at the top of the tower:

[0125] Methanol: 6.59%

[0126] Water: 93.41%.

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Abstract

The invention provides a method for preparing carboxylic acid by hydrolyzing the corresponding polybasic carboxylic acid ester, comprising: hydrolyzing carboxylic acid ester to be the corresponding carboxylic acid and alcohol at a certain temperature and under existing condition of water; the range of temperatures is 100-400 degree C required by hydrolyze, and the ratio by weight of carboxylic acid ester and water as reactants are 1:1-1:15. The invention provides a device for preparing carboxylic acid by hydrolyzing corresponding polybasic carboxylic acid ester, comprising a reaction distilling column and a reaction tower connected to the lower thereof; 2-20 carboxylic acid ester fluid inlets with different heights; and the water feed tube is directly connected to the reaction distilling column or by a steam generation arrangement. The invention has no use for a pre-reactor and acidic/basic catalyst, the method is easy to carry out, the cost and use of the equipment is low, and conversion efficiency is high, and the technology effect is sufficiently better than that of the prior art.

Description

technical field [0001] The invention relates to chemistry, materials and mechanical sciences, and in particular provides a method and a device for preparing corresponding carboxylic acids by hydrolyzing polycarboxylic acid esters without an acidic / alkaline catalyst. Background technique [0002] The reverse reaction of the esterification reaction is the hydrolysis of the carboxylic acid ester to the corresponding carboxylic acid and alcohol. Carboxylate esters are commonly used in the chemical industry as solvents or plasticizers, or are produced as by-products or main products in various reactions. Since carboxylate is a low-value solvent, both are of higher value if hydrolyzed to the corresponding carboxylic acid and alcohol by a hydrolysis reaction followed by conventional separation processes such as distillation, crystallization, etc. [0003] The hydrolysis of esters is generally carried out in a homogeneous medium with acids or bases as catalysts. Use alkali as cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/09
CPCY02P20/10
Inventor 严丽丁云杰林培滋程显波
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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