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Preparation method of sec-butyl acetate

A technology of sec-butyl acetate and acetic acid, applied in the field of preparation of sec-butyl acetate, can solve the problems of long separation process, poor selectivity of sec-butyl acetate, low acetic acid conversion rate, etc., and achieves reduced energy consumption and high reaction conversion rate , the effect of simple process

Active Publication Date: 2014-08-06
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The technical problem to be solved by the present invention is to overcome the problems of low conversion rate of acetic acid, poor selectivity of sec-butyl acetate and long separation process in the prior art, and provide a synthetic process with simple process flow, simplified separation process, low energy consumption and high reaction selectivity. High method for synthesizing and isolating sec-butyl acetate

Method used

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  • Preparation method of sec-butyl acetate
  • Preparation method of sec-butyl acetate
  • Preparation method of sec-butyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-7

[0031] 98% chemically pure acetic acid and carbon tetracarbonate (2-butene mass content 58%) are metered and mixed in a molar ratio of 1: 1 through a plunger pump and injected into a fixed-bed pre-reactor equipped with a resin catalyst. After pre-reaction The mixture then enters the catalytic distillation tower, and the unreacted acetic acid is fully reacted with the supplemented carbon four. Wherein, the molar ratio of 2-butene and unreacted acetic acid in the C4 after supplementing ether is 1.2:1. The loading amount of catalyst in the fixed bed pre-reactor is 40ml, and the loading amount of catalyst in the catalytic distillation tower is 100ml.

[0032] The test results under different temperature and space velocity conditions are shown in Table 1.

[0033] Table 1 Effects of different temperatures and space velocities on the reaction

[0034]

[0035] It can be seen that the acetic acid in Example 3 has been completely converted, and the selectivity of sec-butyl acetate ...

Embodiment 8-10

[0037] The operating conditions adopted by the fixed-bed prereactor and the catalytic distillation tower are the same as in Example 3, and the reflux ratio of the catalytic distillation tower is changed to investigate the influence on the reaction. The results are shown in Table 2.

[0038] Table 2 The influence of different reflux ratios on the reaction (%)

[0039]

[0040] It can be seen that with the increase of the reflux ratio, the selectivity of the ester can be increased to more than 99%.

Embodiment 11-13

[0042] The fixed bed prereactor and the catalytic distillation tower adopt the operating conditions of 3, and the influence of changing the pressure on the reaction is shown in Table 3 for the test results.

[0043] Table 3 Effects of different pressures on the reaction

[0044]

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Abstract

The invention provides a preparation method of sec-butyl acetate. The method is characterized by comprising the following steps: firstly reacting an etherified C4 raw material or an etherified C4 raw material containing inert gases with acetic acid through a fixed bed pre-reaction device; feeding a mixture after pre-reaction into a catalytic distillation tower from the upper part of the reaction section of the catalytic distillation tower, feeding the supplemental etherified C4 raw material or etherified C4 raw material containing inert gases into the catalytic distillation tower from a stripping section at the lower part of the catalytic distillation tower, and carrying out counter-flow contact reaction on two materials at the surface of a catalyst; and enabling unreacted mixed C4 to flow out from the top of the catalytic distillation tower, and enabling the product sec-butyl acetate to flow out from the kettle of the catalytic distillation tower, wherein the fixed bed pre-reaction device and the catalytic distillation tower are filled with the same solid catalyst. By utilizing the method provided by the invention, the acetic acid conversion rate can reach 100%, separation and refinement processes are completed in one catalytic distillation tower, the qualified sec-butyl acetate product can be obtained in the kettle of the tower, the reaction selectivity is high, the separation process is effectively simplified, the process flow is simple, and the manufacturing cost is low.

Description

technical field [0001] The invention relates to a method for preparing sec-butyl acetate, in particular to a method for preparing and separating sec-butyl acetate by using acetic acid and ether carbon four as raw materials and adopting a process combining a fixed-bed pre-reactor and catalytic distillation technology. Background technique [0002] As an organic solvent, sec-butyl acetate has the advantages of environmental protection, low toxicity, and good solubility, and can replace n-butyl acetate, which is currently on the market with a higher price. [0003] At present, most of the techniques for synthesizing sec-butyl acetate are alcohol esterification methods, that is, acetic acid and sec-butanol are dehydrated and esterified under the condition of sulfuric acid as a catalyst, but the separation process of this method is complicated and water separation is difficult; using sulfuric acid as a catalyst leads to waste acid Not only the equipment is severely corroded, but ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/04
CPCY02P20/10
Inventor 朱相春孙强刘淑芝何宗华李刚李玉田
Owner CHINA PETROLEUM & CHEM CORP
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