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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, 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, which increases the polymerization tendency of olefins and affects the product purification; (3) the use of circulating pumps and heat exchangers increases energy consumption. consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A strongly acidic ion exchange resin is used as a catalyst. Commercially available ZH-100 type, the catalyst with a total amount of 250Kg is loaded into the reaction section of the catalytic distillation tower, and thus the catalyst layer is obtained.

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

[0017] The operating conditions of the catalytic distillation tower are: tower top pressure 0.65 MPa, tower top temperature 50°C, temperature in the middle of the reaction section 100°C, tower bottom temperature 180°C, reflux ratio 5, acetic acid mixed with C 4 The molar ratio (acid-ene ratio) ...

Embodiment 2~4

[0020] Experimental method and catalyzer are with embodiment 1, and operating condition is different from embodiment 1. Change the acid-ene ratio, reaction space velocity, reaction pressure, and reaction temperature to obtain the reaction results as shown in the table below. In these experiments, no catalyst deactivation phenomenon was found.

[0021] Table 1

[0022]

Embodiment 5

[0023] Embodiment 5: (heteropolyacid catalyst)

[0024] A heteropolyacid catalyst is used. A total of 10 L of the 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 tower are: tower top pressure 0.5 MPa, tower top temperature 60°C, temperature in the middle of the reaction section 110°C, tower bottom temperature 175°C, reflux ratio 5, acetic acid mixed with C 4 The molar ratio (acid-ene ratio) of middle butene is 1.5, and the space velocity of acetic acid feed is 1.0hr -1 . Other reaction steps are with embodiment 1.

[0026] The composition of the reaction product was analyzed by sampling every 4hr, and the analysis was carried out by gas chromatography. It is measured that the conversion rate of acetic acid is above 70%, the selectivity of sec-butyl acetate reaches above 99.2%, and the content of butene in the bottom material of 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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