Method for preparing sec-butyl acetate

A technology of sec-butyl acetate and acetic acid, which is applied in the field of preparation of sec-butyl acetate, can solve problems affecting product purification, increase tendency of olefin polymerization, increase energy consumption, etc., and achieve the effect of simplifying the product separation process and reducing energy consumption

Active Publication Date: 2008-03-19
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
Moreover, th

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0014] Example 1:

[0015] Strong acid ion exchange resin is used as catalyst. Commercially available ZH-100 type, the catalyst with a total amount of 250Kg is charged into the reaction section of the catalytic distillation column, and thus a catalyst layer is obtained.

[0016] Acetic acid and mixed C 4 Respectively enter the column from the upper rectifying section and the lower stripping section of the catalytic distillation column, the two are in countercurrent contact on the catalyst surface, and the acetic acid and mixed C 4 The reaction generates sec-butyl acetate, and the unreacted mixed C 4 It is distilled from the top of the column and the product mixture flows out from the bottom of the column.

[0017] The operating conditions of the catalytic distillation column are: the top pressure of 0.65 MPa, the top temperature of 50 °C, the temperature of the middle part of the reaction section of 100 °C, the temperature of the tower still of 180 °C, the reflux ratio of 5...

Example

[0019] Embodiments 2 to 4:

[0020] The experimental method and catalyst are the same as those of Example 1, and the operating conditions are different from those of Example 1. The acid-ene ratio, reaction space velocity, reaction pressure, and reaction temperature were changed, and the reaction results were obtained as shown in the following table. In none of these experiments, catalyst deactivation was found.

[0021] Table 1

[0022]

Example Embodiment

[0023] Example 5: (heteropolyacid catalyst)

[0024] A heteropolyacid catalyst is used. A total amount of 10 L of catalyst was charged into the reaction section of the catalytic distillation column, and thus a catalyst layer was obtained.

[0025] The operating conditions of the catalytic distillation column are: pressure at the top of the column 0.5 MPa, temperature at the top of the column 60 °C, temperature in the middle of the reaction section 110 °C, temperature in the tower still 175 °C, reflux ratio 5, acetic acid and mixed C 4 The molar ratio of butene (acid-ene ratio) is 1.5, and the acetic acid feed space velocity is 1.0hr -1 . Other reaction steps are the same as in Example 1.

[0026] Samples were taken every 4 hr to analyze the composition of the reaction product by gas chromatography. The conversion rate of acetic acid is measured to be over 70%, the selectivity of sec-butyl acetate is over 99.2%, and the content of butene in the bottom material of the cataly...

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PUM

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Abstract

A preparation method of secondary butyl acetate applies the method of catalytic distillation to enable acetic acid and mixed C4 (or butylene) to respectively enter into a catalytic distillation column from the upper rectifying section and the lower stripping section of the tower, a catalyzer is loaded in a reaction section, the acetic acid is countercurrent contacted with the mixed C4 (or butylene) on the surface of the catalyzer, the unreacted mixed C4 (or butylene) is evaporated from the top of the column, and a product mixture flows out from the bottom of the column. By applying the method to prepare the secondary butyl acetate, in the follow-up working procedure of separation, a flash column which is used to remove the unreacted mixed C4 (or butylene) is not needed, as a result, the separation technique of products is simplified, and energy consumption is reduced.

Description

technical field [0001] The present invention relates to a kind of preparation method of sec-butyl acetate, particularly relate to a kind of method that adopts catalytic distillation technology to prepare sec-butyl acetate. 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. U.S. Patent No. 5,457,228 discloses a kind of method for preparing sec-butyl acetate, is that reaction material is acetic acid and mixing C 4 (or butene) is introduced from the upper part of the tubular fixed-bed reactor, and the product mixture includes unreacted mixture C 4 (or butene), unreacted acetic acid and product sec-butyl acetate flow out from the bottom of the reactor simultaneously. After the product mixture passes through the circulating pump and heat exchanger in sequence, a part of the product mixture is sent to the s...

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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