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Method for producing n-butyl acetate through microwave pipeline

A n-butyl acetate, pipeline technology, applied in the direction of chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of reduced yield, no production practicability, complexity, etc., and achieve increased reaction speed , Simplified production operation, fast esterification reaction

Active Publication Date: 2011-11-30
ZHEJIANG JIANYE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, whether sulfuric acid or other new catalysts are used for catalytic esterification, or catalytic esterification under microwave radiation, the reaction of synthesizing n-butyl acetate is carried out in a tank reactor, which is a batch operation and is relatively complicated; Simultaneously, the use of catalyst is also indispensable, and the consumption is generally between 1-10% of raw material quality; In the case of no catalyst, it will cause the yield to be greatly reduced, that is, it will cause no production practicability

Method used

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  • Method for producing n-butyl acetate through microwave pipeline
  • Method for producing n-butyl acetate through microwave pipeline
  • Method for producing n-butyl acetate through microwave pipeline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1, figure 1 A pipeline reactor is provided, comprising a raw material tank 1, a metering pump 4, a pipeline reactor 14 and a condenser 11; the outlet of the raw material tank 1 is connected to the metering pump 4 through a pipeline I 3, and the metering pump 4 passes through the pipeline II 5 is connected to the inlet of the tube reactor 14, the outlet of the tube reactor 14 is connected to the inlet of the condenser 11 through the pipeline III9, and the outlet of the condenser 11 is connected to the pipeline IV13. A cut-off valve I 2 is arranged on the pipeline I 3, a pressure gauge I 6 and a shut-off valve II 7 are respectively arranged on the pipeline II 5 according to the flow direction, a thermometer 8 is arranged on the pipeline reactor 14, and a thermometer 8 is arranged on the pipeline III9. A pressure gauge II 10 is provided, and a stop valve III 12 is provided in the pipeline IV 13 . The entire tube reactor 14 is placed in a microwave generator 15 ...

Embodiment 2

[0017] Embodiment 2, a kind of method of pipeline production n-butyl acetate, adopt the pipeline reactor described in embodiment 1, carry out following steps successively:

[0018] 1), raw material preparation:

[0019] Add 74 g (1.0 mol) of n-butanol and 60 g (1.0 mol) of acetic acid into the raw material tank 1, and mix thoroughly to obtain a mixed solution.

[0020] 2), esterification reaction:

[0021] Use the metering pump 4 to pump the above-mentioned mixed solution into the pipeline reactor 14, the reaction temperature is 60°C, the reaction pressure is normal pressure, and the power of the microwave generator is adjusted to 400w; the flow rate of the metering pump 4 is controlled to make the reactant (i.e. the mixed solution ) is 1000ml / h at the flow rate of pipeline reactor, and promptly reaction time is about 6mins, obtains the crude product liquid containing n-butyl acetate.

[0022] 3), post-processing:

[0023] The above-mentioned crude product liquid containing...

Embodiment 3

[0024] Embodiment 3, a kind of method of pipeline production n-butyl acetate, adopt the pipeline reactor described in embodiment 1, carry out following steps successively:

[0025] 1), raw material preparation:

[0026] Add 74 g (1.0 mol) of n-butanol and 90 g (1.5 mol) of acetic acid into the raw material tank 1, and mix thoroughly to obtain a mixed solution.

[0027] 2), esterification reaction:

[0028] Use the metering pump 4 to inject the above-mentioned mixed solution into the pipeline reactor 14, the reaction temperature is 80°C, the reaction pressure is normal pressure, and the power of the microwave generator is adjusted to 600w; the flow rate of the metering pump 4 is controlled to make the reactant (i.e. the mixed solution ) is 500ml / h at the flow rate of pipeline reactor, promptly reaction time is about 12mins, obtains the crude product liquid containing n-butyl acetate.

[0029] 3), post-processing:

[0030] The above-mentioned crude liquid containing n-butyl a...

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Abstract

The invention discloses a method for producing n-butyl acetate in a microwave pipeline. The n-butanol and acetic acid with a molar ratio of 1:1-2 are used as raw materials to prepare a mixed solution; the mixed solution is pumped into a pipeline reactor with a metering pump The esterification reaction is carried out under microwave irradiation to obtain a crude product solution containing n-butyl acetate. The reaction pressure is normal pressure, the reaction temperature is 40-80°C, the reaction time is 2-15mins, and the power of the microwave generator is 300-600W. The crude product liquid containing n-butyl acetate is rectified, and the fractions at 124-126° C. are collected to obtain n-butyl acetate. Using the method of the present invention to produce n-butyl acetate has the characteristics of high conversion rate, simple and fast post-processing, no need to use catalysts and the like.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for preparing n-butyl acetate using a microwave pipeline reactor. Background technique [0002] N-butyl acetate is an important organic solvent, which is widely used as an extraction agent in petroleum processing and pharmaceutical processes, and can also be used in the fields of compounding spices, etc. Its structural formula is: [0003] [0004] The traditional synthesis method of n-butyl acetate is mainly obtained by the esterification of acetic acid and n-butanol under the catalysis of sulfuric acid. This method has poor selectivity, many side reactions, dark product color and easy to cause equipment corrosion. In recent years, many new catalysts have appeared, such as: zeolite molecular sieve, solid superacid, solid heteropolyacid, strong acid cation exchange resin, etc. These catalysts have good catalytic activity, do not corrode equipment, and have certain practi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/14C07C67/08B01J19/12
Inventor 冯烈陈云斌陈新志钱超
Owner ZHEJIANG JIANYE CHEM
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