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Method for synthesizing ethyl acetate by ionic liquid catalytic continuous esterification distillation

An ionic liquid, ethyl acetate technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc. The effect of intensifying production

Inactive Publication Date: 2008-09-03
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the ionic liquid contains fluorine; it is also miscible with ethyl acetate and cannot separate phases automatically

Method used

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  • Method for synthesizing ethyl acetate by ionic liquid catalytic continuous esterification distillation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Reactive distillation experimental device used: glass tower body (Φ20mm), built-in Φ2×2mm stainless steel θ mesh ring packing, packing height is 1.4m, insulation sleeve diameter is 60-80mm, kettle volume is 500ml.

[0031] Add 2.00 mol of glacial acetic acid, 0.33 mol of ethanol and 0.01 mol of ionic liquid α-pyrrolidone bisulfate into the reaction kettle, set the temperature of the kettle at 110°C, keep the bottom at 95°C, and keep at the top at 70.4°C. Raise the temperature and heat up, and make it fully reflux for 15 minutes after the reflux liquid appears at the top of the tower, then continuously add the mixture of ethanol and acetic acid prepared in advance with an alkyd molar ratio of 1.05:1 into the esterification tank through the head tank, and start The reflux ratio is continuously carried out for the synthesis of ethyl acetate. The feed flow rate of the mixed raw materials is 40ml / h, the reflux ratio is 1, and the reflux ester flow rate is 35mL / h. The ester ...

Embodiment 2

[0033] Reactive distillation experimental device used: glass tower body (Φ20mm), built-in Φ2×2mm stainless steel θ mesh ring packing, packing height is 1.4m, insulation sleeve diameter is 60-80mm, kettle volume is 500ml.

[0034] Add 2.00 mol of glacial acetic acid, 0.67 mol of ethanol and 0.2 mol of ionic liquid α-pyrrolidone bisulfate into the reaction kettle, set the temperature of the kettle at 100°C, keep the bottom at 90°C, and keep at the top at 71°C. Raise the temperature and heat until there is a reflux liquid at the top of the tower, let it fully reflux for 15 minutes, then add the mixture of ethanol and acetic acid with a molar ratio of alkyd to 1.2:1 to the esterification tank continuously through the head tank, and start the process at the same time. The reflux ratio is continuously carried out for the synthesis of ethyl acetate. The feed flow rate of the mixed raw materials is 20ml / h, the reflux ratio is 4, and the reflux ester flow rate is 20mL / h. The ester con...

Embodiment 3

[0036] Reactive distillation experimental device used: glass tower body (Φ20mm), built-in Φ2×2mm stainless steel θ mesh ring packing, packing height is 1.4m, insulation sleeve diameter is 60-80mm, and the volume of the kettle is 500ml.

[0037] Add 2.00 mol of glacial acetic acid, 0.33 mol of ethanol and 0.6 mol of ionic liquid α-pyrrolidone bisulfate into the reaction kettle, set the temperature of the kettle to 110°C, keep the bottom at 95°C, and keep at the top at 70°C. Raise the temperature and heat up, and make it fully reflux for 15 minutes after the reflux liquid appears at the top of the tower, then continuously add the mixture of ethanol and acetic acid prepared in advance with an alkyd molar ratio of 1:1 into the esterification tank through the head tank, and start the process at the same time. The reflux ratio is continuously carried out for the synthesis of ethyl acetate. The feed flow rate of the mixed raw materials is 40ml / h, the reflux ratio is 1, and the reflux...

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Abstract

The invention provides a method of ionic liquid catalyze, continuously esterifying and rectifying synthesized ethyl acetate, comprising adding a definite proportion of acetic acid, ethanol and ionic liquid catalytic agent that is alpha-pyrrolidone bisulphate at the bottom of rectification column, setting an upper heat-preserving temperature, a lower heat-preserving temperature, a reactor temperature and a reflux ratio, heating up to generate refluxing liquid at the top of the column, then holding total reflux for 15min, adding the mixed liquor of ethanol and acetic acid to the esterification reactor continuously from a high-level tank at a definite ratio of alcohol and acid and a certain feed flow speed, opening reflux ratio for preparing ethyl acetate by continuous reaction and rectification; for keeping the stability of the system, refluxing partial coarse ester at a definite refluxing speed to the bottom of the reactor, and bringing out superfluous product by azeotropy. The method uses a high catalytic activity, high selectivity, low corrosive, acidic ionic liquid to take place the traditional strong corrosivity concentrated sulphuric acid as a catalytic agent for catalyzing and rectifying continuously the synthesized ethyl acetate, the method has the advantage of low cost, high utilance for raw material, and high yield of product and purity.

Description

technical field [0001] The present invention relates to a kind of continuous preparation method of ethyl acetate. In particular, it relates to a method for synthesizing ethyl acetate through continuous reaction distillation with ionic liquid catalysis. It belongs to the technical field of organic synthesis. Background technique [0002] Catalytic reaction distillation technology is a chemical technology developed in the 1980s. A lot of research work has been done on catalytic distillation technology at home and abroad. The domestic ethyl acetate production unit consists of an esterification tower, a dehydration tower, a refining tower and a recovery tower. The feature of the process is that the esterification reaction is carried out in the esterification tank, and the separation process mainly adopts the azeotropic distillation process for dehydration and dealcoholization. The main defect of its production process is that the concentrated sulfuric acid catalyst used has p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/08B01J31/02
Inventor 黄宝华黎子进汪艳飞史娜徐效陵方岩雄张焜张维刚张俊浩
Owner GUANGDONG UNIV OF TECH
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