Preparation method for sec-butyl acetate with product separating and reclaiming technique

A sec-butyl acetate and process technology, which is applied in the field of preparation of sec-butyl acetate, can solve problems affecting product purification, increase of olefin polymerization tendency, increase energy consumption, etc., and achieve product separation process simplification, energy consumption reduction, and production cost Reduced effect

Active Publication Date: 2008-04-30
HUNAN ZHONGCHUANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The deficiency of this method is: (1) adopt shell-and-tube fixed bed to make reactor, send that part product mixture of separation generally need to pass through flash tower first, unreacted mixed C 4 (or butene) is removed from the product mixture, thus increasing the difficulty of the subsequent product separation process; and the temperature and pressure of the flash tower are high, and the energy consumption is high; (2) the reaction material is circulated into the reactor to make the olefin The polymerization tendency in

Method used

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  • Preparation method for sec-butyl acetate with product separating and reclaiming technique
  • Preparation method for sec-butyl acetate with product separating and reclaiming technique
  • Preparation method for sec-butyl acetate with product separating and reclaiming technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] As shown in Figure 1, a strong acidic ion exchange resin is used as a catalyst, commercially available ZH-100 type. The catalyst in a total amount of 250 Kg was charged into the reaction section A2 of the catalytic distillation column A, and thus a catalyst layer was obtained.

[0026] Acetic acid 1, mix C 4 2 Enter the tower from the upper rectifying section A1 and the lower stripping section A3 of the catalytic distillation tower A respectively, and the two contact the catalyst surface in the reaction section A2 countercurrently, the acetic acid 1 and the mixed C 4 2 reaction generates sec-butyl acetate, unreacted mixed C 4 3 is distilled from the top of the column and the product mixture 4 is taken from the bottom of the column.

[0027] The operating conditions of catalytic distillation tower A are: tower top pressure 0.65MPa, tower top temperature 50°C, reaction section A2 middle temperature 100°C, tower kettle temperature 180°C, reflux ratio 5, acetic acid 1 ...

Embodiment 2

[0033] As shown in Figure 1, heteropolyacid is selected as the catalyst. A total of 10 L of the catalyst was charged into the reaction section A2 of the catalytic distillation column A, and thus a catalyst layer was obtained.

[0034] Acetic acid 1, mix C 4 2 Enter the tower from the upper rectifying section A1 and the lower stripping section A3 of the catalytic distillation tower A respectively, and the two contact the catalyst surface in the reaction section A2 countercurrently, the acetic acid 1 and the mixed C 4 2 reaction generates sec-butyl acetate, unreacted mixed C 4 3 is distilled from the top of the column and the product mixture 4 is taken from the bottom of the column.

[0035] The operating conditions of the catalytic distillation tower are: tower top pressure 0.5MPa, tower top temperature 52°C, temperature in the middle of reaction section A2 138°C, tower bottom temperature 155°C, reflux ratio 5, acetic acid 1 mixed with C 4 The molar ratio (acid-ene ratio)...

Embodiment 3

[0043] As shown in Figure 1, the catalyst selected in the catalytic distillation reaction stage and its preparation, the operating conditions of the catalytic distillation tower, the reaction steps, etc. are all the same as in Example 2, and the process of the azeotropic rectification of the resulting mixed product after the reaction and its control Condition is identical with embodiment 2, but the recovery process of reaction gained mixed product is carried out as follows.

[0044] Fraction 7 is extracted from the lower part of the azeotropic distillation tower, and its mass composition is: 12.10% of sec-butyl acetate, 77.69% of acetic acid, 5.93% of water, 4.28% of hydrocarbons and other substances. The fraction 7 extracted from the lower part of the azeotropic distillation tower is removed from the acid concentration tower D, and the entrainer benzene 8 is added to the acid concentration tower D at the ratio of benzene:water=91:9 (mass ratio). The temperature at the bottom ...

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Abstract

The invention relates to a process for preparing sec-butyl acetate, with product separation and reclamation technology, which is characterized in that the reaction is processed in one catalysis distillation column composed of a column reactor, an exhausting section, a reaction section, a distillation section, and a column top reflux condenser, wherein the reaction section is filled with catalyst,acetic acid and mixture C4 or butene which are reversely contacted and reacted on the surface of catalyst, the non-reacted mixture C4 or butene is evaporated out from the top of the catalyst distillation column, the product mixture is fed into an azeotropic distillation column, added with an entrainer a which can form azeotropic material with sec-butyl acetate, the distillate at the top of the azeotropic distillation column is fed into a treating column, to be distilled to obtain sec-butyl acetate, and the fraction at the lower portion of the azeotropic distillation column, is fed into an acidconcentrating tower, added with an entrainer b which can form azeotropic material with the entrainer a, to process azeotropic distillation to be circulated and feedback to the reaction system. The invention has the advantages of simplified separation, low cost, low energy consumption, high material utilization and the like.

Description

technical field [0001] The invention relates to a method for preparing sec-butyl acetate, in particular to a method for preparing sec-butyl acetate with a product separation and recovery process. Background technique [0002] Currently, using acetic acid and mixing C 4 (or butene) as raw material, the method for preparing sec-butyl acetate usually obtains by carrying out esterification in a tubular fixed-bed reactor. Compared with the traditional process, by mixing C 4 (or butene) as a raw material, utilizing it to react with acetic acid to prepare sec-butyl acetate has the advantages of wide source of raw material and low cost, good economic benefit, and environmental friendliness. U.S. Patent No. 5,457,228 discloses a method for preparing sec-butyl acetate, which is to mix reaction material acetic acid with C 4 (or butene) is introduced from the upper part of the tubular fixed bed reactor, including unreacted mixed C 4 (or butene), unreacted acetic acid and the product...

Claims

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Application Information

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IPC IPC(8): C07C69/14C07C67/04
CPCY02P20/10
Inventor 胡先念李华
Owner HUNAN ZHONGCHUANG CHEM
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