Solvent-free esterification-distillation integrated process

The technology of esterification reaction and esterification reaction kettle is applied in the field of solvent-free esterification reaction-distillation integration process, which can solve the problems of increased production cost, poor compatibility, and higher requirements for esterification raw materials.

Active Publication Date: 2013-10-30
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some shortcomings in the esterification reaction under the condition of solvent. During the process of carrying water, due to the continuous reflux and condensation of the solvent, part of the heat is taken away by heat exchange, which increases energy consumption. At the same time, after the reaction is completed, the solvent must be evaporated. In the process of solvent recovery, there will be some losses. Solvents such as toluene and xylene are expensive, resulting in increased production costs. The use of solvents will pollute the environment, and some solvents are toxic, causing harm to operators. harm
[0003] Another method is the solvent-free method. The solvent-free method is divided into two types. One uses excess organic components in the esterification reaction as water-carrying agents. Usually, the excess organic components are not compatible with water. (such as butanol), which can form an azeotrope with water, or continuously blow organic component vapor (such as methanol) into the reaction system, and the organic component vapor will take away the water generated by the reaction to promote the esterification reaction. This method has higher requirements for esterification raw materials, and its application range is narrower; another method is to vacuumize the reaction system and steam the water generated by the reaction. This method generally requires the use of soluble catalysts in the system, and it is easy to cause The degree of esterification is not high, and the esterification time is long

Method used

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  • Solvent-free esterification-distillation integrated process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 (the synthesis of trimethylolpropane triheptanoate):

[0022] a. Add 134 kg of raw material trimethylolpropane and 2 kg of catalyst p-toluenesulfonic acid into the high-level feeding tank 1, add 400 kg of heptanoic acid into the high-level feeding tank 2, fill the high-level feeding tank 1 with nitrogen protection and start the heating system, so that the three Melt methylolpropane and p-toluenesulfonic acid, after the raw materials are fully melted, open the vacuum system 19, the vacuum pressure is 1000pa, close the valves 18 and 21 at the same time, open the valves 6, 7, 11 and 16, and the high-level feeding tanks 1 and 2 The raw materials inside are sucked into the esterification reactor 12 under the condition of negative pressure, and after the raw materials are completely sucked, the valve 11 is closed;

[0023] b. Turn on the vacuum system 19, turn on the condenser 15 and the high-temperature-resistant circulation pump 17 at the same time, and the mat...

Embodiment 2

[0025] Embodiment 2 (the synthesis of trimethylolpropane triheptanoate):

[0026] a. Add 134kg of raw material trimethylolpropane to the high-level feeding tank 1, add 400kg of heptanoic acid to the high-level feeding tank 2, fill the high-level feeding tank 1 with nitrogen protection and start the heating system to melt the trimethylolpropane. After the raw materials are fully melted, open the vacuum system 19, the vacuum pressure is 2000pa, close the valves 18 and 21 at the same time, open the valves 6, 7, 11 and 16, the raw materials in the high-level feeding tanks 1 and 2 are sucked into the In the esterification reaction kettle 12, after the raw materials are completely inhaled, close the valve 11;

[0027] b, open the vacuum system 19, open the condenser 15 and the high temperature resistant circulating pump 17 at the same time, the material is pumped out from the esterification reactor 12 through the high temperature resistant circulating pump 17, pass through the catalys...

Embodiment 3

[0029] Embodiment 3 (the synthesis of dumbbell-shaped product 2-trimethylolpropane-adipate-4-heptanoate):

[0030] a. Add 134kg of raw material trimethylolpropane to the high-level feeding tank 1, add 73kg of adipic acid to the high-level tank feeding 2, put 280kg of heptanoic acid into the high-level tank 3, fill the high-level feeding tanks 1 and 2 with nitrogen protection and start the heating system , to dissolve trimethylolpropane and p-toluenesulfonic acid. After the raw materials are fully dissolved, open the vacuum system 19, the vacuum pressure is 3000pa, close the valves 18 and 21 at the same time, open the valves 6, 7, 11 and 16, and the high-level feeding tank The raw materials in 1 and 2 are sucked into the esterification reactor 12 under the condition of negative pressure, and after the raw materials are completely sucked, the valve 11 is closed;

[0031] b, open the vacuum system 19, open the condenser 15 and the high temperature resistant circulating pump 17 at...

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Abstract

The invention discloses a solvent-free esterification-distillation integrated process. In the process, a high feeding tank, an esterification kettle, a storage tank and a thin-film evaporator are connected in series; aliphatic alcohol and acid raw materials which is subjected to pretreatment is fed into the circulating esterification kettle with a catalyst fixed bed from the high tank; an esterification is accomplished by means of circulating esterification, and water generated in the reaction is evaporated out by means of constantly vacuumizing to promote the esterification to advance in a forward direction; after the esterification is accomplished, the coarse product is delivered by the circulating pump to the thin-film evaporator from the nitrogen protected storage tank; unreacted excessive organic materials with small molecular weights are evaporated out; and through refining, the pure product is obtained. Compared with the conventional process, the process disclosed by the invention has the advantages that: solvent is not needed in the whole process; excessive organic raw materials with small molecular weights can be recycled; and the process is an energy-saving, emission-reducing and environment-friendly esterification synthesis process.

Description

Technical field: [0001] The invention relates to a solvent-free esterification reaction-distillation integration process, which is applied to the synthesis of aliphatic alkyd esters, and has the characteristics of energy saving, emission reduction, green and pollution-free. Background technique: [0002] The esterification reaction generally consists of aliphatic alcohol and aliphatic carboxylic acid in the presence of a catalyst, dehydration reaction to generate aliphatic ester. The traditional esterification process is divided into two types: one is the solvent method, the aliphatic alkyd uses a homogeneous or heterogeneous catalyst, and the esterification reaction is carried out under the condition of a solvent. The solvent can form an azeotrope with water, and the water is continuously removed from the reaction system. It is taken out in the middle, and the reaction is promoted to proceed forward. The solvents that can be used as water-carrying agents include toluene, xy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C67/52C07C69/34C07C69/003
CPCY02P20/10
Inventor 吾满江·艾力蔡国星宋平张乐涛严晓虎马莉古丽米热·吐尔地
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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