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Method for producing sec-butyl acetate by synthesizing acetic acid and mixed C4

A technology of sec-butyl acetate and acetic acid, which is applied in the chemical industry, can solve problems such as environmental pollution, many side reactions, and long reaction time, and achieve the effects of reducing production costs, good stability, high activity and selectivity

Inactive Publication Date: 2012-02-08
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using sulfuric acid as a catalyst has serious equipment corrosion, continuous reaction, many side reactions, complicated post-treatment procedures, and serious environmental pollution. Moreover, because sec-butanol belongs to secondary alcohols, its dehydration property and position when esterification occurs The resistivity is obviously higher than that of primary alcohols, the conditions of esterification reaction are relatively harsh, and there are disadvantages such as long reaction time, large amount of catalyst or low yield to varying degrees.
[0005] Olefin-acetic acid addition esterification to synthesize sec-butyl acetate was part of the acetic acid process developed by German Bayer company in the 1960s. The esterification reaction was carried out in a suspension stirred tank under the catalysis of cationic sulfonic acid exchange resin. The n-butyl acetate in the C4 component The alkene content is 80%, but according to the method, the yield of esterification is only 50-80%, that is, the cost is high and the yield is small

Method used

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  • Method for producing sec-butyl acetate by synthesizing acetic acid and mixed C4
  • Method for producing sec-butyl acetate by synthesizing acetic acid and mixed C4
  • Method for producing sec-butyl acetate by synthesizing acetic acid and mixed C4

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Experimental program
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Effect test

Embodiment 1

[0032] 2.0mL of resin catalyst and 13mL of glacial acetic acid were charged into the above-mentioned autoclave, and mixed C4 (mass composition was n-butane 11.8%, isobutane 34.6%, 1-butene 17.6%, 2-butene 32.6%, Butadiene, alkyne, etc. 3.4%) 20mL, the molar ratio of n-butene (1-butene, 2-butene) to glacial acetic acid is 0.5:1 (ene-acid ratio), and nitrogen is gradually pressurized to 5.0MPa to adjust the reaction The temperature was raised to 120°C, and the reaction was stopped after 10 hours of reaction, and samples were taken for analysis. The product was analyzed by an Agilent 6890N gas chromatograph. The conversion rate of acetic acid was 90.5%, and the selectivity of sec-butyl acetate was 97.8%.

Embodiment 2

[0034] Except reaction pressure is changed to 6.0MPa, other is the same as embodiment 1, the result is: acetic acid conversion rate 88.5%, sec-butyl acetate selectivity 91.3%.

Embodiment 3

[0036] Except that the reaction temperature was changed to 160° C., the others were the same as in Example 1, and the results were: the conversion rate of acetic acid was 72.3%, and the selectivity of sec-butyl acetate was 77.9%.

[0037] The present invention makes full use of refinery by-product C 4 resources, using strongly acidic styrene-based cation exchange resins as catalysts, studied mixed C 4 (Containing 1-butene, 2-butene, n-butane, isobutane, butadiene, etc.) and glacial acetic acid to synthesize sec-butyl acetate. Through single factor experiment, the effects of reaction time, reaction temperature, reaction pressure, catalyst dosage and molar ratio of enoic acid on the conversion of acetic acid were investigated, and the optimum process conditions for the synthesis of sec-butyl acetate were determined.

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Abstract

The invention relates to a method for producing sec-butyl acetate by synthesizing acetic acid and mixed C4, which belongs to the chemical field. The invention aims to provide the method for producing the sec-butyl acetate by synthesizing the acetic acid and the mixed C4, which is used for fully and reasonably utilizing byproduct mixed C4 resources of petrochemical enterprises, broadening the way to comprehensively utilize C4 hydrocarbon, and producing fine chemical products with high added value. According to the invention, a kettle type batch reactor is adopted, strong-acid cation exchange resin is adopted as solid catalyst, the acetic acid and the mixed C4 are used as the raw materials to synthesize the sec-butyl acetate, the reaction pressure is 2.0-6.0MPa, the reaction temperature is 80-160 DEG C, the reaction time is 5-15h, the molar ratio of olefine acid is 0.2-1.5, and the catalyst amount is 4-12 percent of the acetic acid. According to the synthetic process of the sec-butyl acetate, the acetic acid and butane (refinery byproduct mixed C4 contains 1-butane and 2-butane) are adopted as the raw materials to be directly synthesized through addition reaction under the action of acid catalysts, an olefin resource is directly utilized, and ethanol is unnecessary to be an intermediate, so that the production cost of the sec-butyl acetate is reduced, the obvious economic advantage is achieved, the refinery mixed C4 resource is effectively utilized, and the method is an effective way to improve chemical utilization of C4 hydrocarbon.

Description

Technical field [0001] The present invention belongs to the field of chemical industry. Background technique [0002] The hybrid C4 is an important petrochemical resource. It is the general term of the alkanide, monocular and dinolefins. It is mainly composed of orthopedic, isotonne, orthopedane, isotide, and butadiene.Hybrid C4 hydrocarbons are mainly derived from the alchemy factories catalyzed and steam cracking. In addition, there are pilefield gas recycling, ethylene cluster, isher, and acrylic coin oxidine.With the improvement of my country's ethylene production and crude oil processing capabilities, the steam cracking device and catalytic cracking device will mix a large number of by -production C4 hydrocarbons.At present, a large number of C4 hydrocarbons are mainly used for fuel (liquefied petroleum gas). Data show that about 90%are used for fuel and only 10%are used in the chemical market.From this point of view, how to fully and reasonably use these by -production reso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/04
Inventor 杜长海李冰冰孟祥春孙德
Owner CHANGCHUN UNIV OF TECH
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