Gas phase catalytic esterification process for synthesizing butyl acetate

A gas-phase catalytic ester, butyl acetate technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of high reaction temperature, overheating, low reaction gas space velocity, etc., to achieve uniform reaction temperature, Simple process and high conversion rate

Inactive Publication Date: 2005-01-12
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In today's society, the voice of environmental protection is increasing day by day, and the chemical industry is developing towards a "zero emission" model; the current research on solid acid catalysts used in esterification is limited to catalyzing liquid-phase esterification; therefore, gas-phase esterification synthesis is a fine chemical industry An important development direction; so far, the study of gas phase esterification is relatively rare: only the former Soviet Union used clay, and Zhuang Mengfu of Nankai University and others used HZSM-5 molecular sieves to catalyze the fixed bed reaction, but the reaction temperature is high and the activity is low. Poor, the preparation and treatment of the catalyst are relatively complicated, expensive additives such as templates are used in the catalyst preparation process, and the cost of the catalyst is high; the reaction raw material gas before the bed is mixed unevenly, and the temperature of the reaction bed is uneven, which is easy to cause local overheating and promote side effects. Reaction, prone to channeling, short circuit, low reaction gas space velocity
In addition, Zeng Jinlong et al. introduced a gas-solid phase circulation reaction system in the patent (Patent No.: CN1156717A), which can reach a yield of more than 98% after 6-8 hours of circulation reaction, but it is a batch reaction. Certain raw materials need to react for a cycle of 6-8 hours

Method used

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  • Gas phase catalytic esterification process for synthesizing butyl acetate
  • Gas phase catalytic esterification process for synthesizing butyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0012] Using our invented SO 4 2- / Fe 2 o 3 -ZrO 2 -SiO 2 The solid acid catalyst (patent publication number: CN1323655A) is compressed into tablets with a hydraulic press at 25 MPa, and crushed to a size of 20-40 mesh.

[0013] Vapor-phase acetic acid / butanol esterification in figure 1 Carry out on the shown device, at first add n-butanol and glacial acetic acid in reaction raw material bottle 12, in quartz reaction tube 8, pack solid acid catalyst; After being heated to reaction temperature, start peristaltic pump 14 and N 2 Jet gas 5, after the reaction material (acetic acid / butanol molar ratio is 1: 1) enters the reaction tube, start timing, reaction conditions: reaction temperature 423K, catalyst addition: 5g, reaction material gas space velocity (GHSV)=761h -1 , reaction time: 2h, jet gas: N 2 , flow rate: 5ml.min -1 ; After the inspection, turn off the pump and the jet gas. Sampling was carried out in the snake-type condenser 9, and the composition of the produ...

Embodiment 2

[0015] Using our invented SO 4 2- / Fe 2 o 3 -ZrO 2 -SiO 2 The solid acid catalyst (patent publication number: CN1323655A) is compressed into flakes with a hydraulic press at 25 MPa, and crushed to a size of 40-60 mesh.

[0016] Vapor-phase acetic acid / butanol esterification in figure 1 Carry out on the shown device, at first add n-butanol and glacial acetic acid in reaction raw material bottle 12, in quartz reaction tube 8, pack solid acid catalyst; After being heated to reaction temperature, start peristaltic pump 14 and N 2 Jet gas 5, after the reaction material (acetic acid / butanol molar ratio is 1: 1) enters the reaction tube, start timing, reaction conditions: reaction temperature 423K, catalyst addition: 5g, reaction material gas space velocity (GHSV)=380h -1 , reaction time: 2h, jet gas: N 2 , flow rate: 5ml.min -1 ; After the inspection, turn off the pump and the jet gas. Sampling was taken from the snake-type condenser 9, and the product composition was analy...

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Abstract

This invention relates to new technology of gaseous phase catalytic esterification and its equipment, it uses straight immobilized bed reactor with fluidic apparatus. The invented new technology is low in cost, higher raw material gas space velocity, uniform mixing of raw material, can reduce channeling and short circuit effectively. The ethyl butylate yield and selectivity can reach respectively to 85.41% and 95.43%.

Description

technical field [0001] The invention relates to an organic synthesis method, in particular to a method for synthesizing butyl acetate by gas-phase catalytic esterification. Background technique [0002] As an important class of organic synthesis reactions, esterification plays a pivotal role in modern industry. Carboxylate esters synthesized by esterification, such as fatty acid esters such as acetate and lactate, and aromatic esters such as phthalate, salicylate, and substituted benzoate, are used in fragrances, daily chemicals, Important raw materials for paint, leather, medicine and other industries. The traditional esterification reaction uses sulfuric acid as a catalyst for liquid phase synthesis. It is cheap and has high catalytic activity, so it is widely used in industry. However, the disadvantages of sulfuric acid-catalyzed liquid-phase esterification cannot be ignored: it corrodes equipment severely, discharges a large amount of three wastes, and the post-treatme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08
Inventor 储伟胡健平邱发礼颜达予陈庆龄
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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