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Preparation process and equipment of n-amyl acetate

A technology for the preparation of n-pentyl acetate, which is applied in the preparation of carboxylic acid esters, carboxylic acid salts, and organic compounds, and can solve the problems of many side reactions, cumbersome production, and reduced yield and quality, so as to ensure safety The effect of stability, storage time prolongation, and environmental pollution is small

Pending Publication Date: 2021-06-29
JIANGSU YIDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional preparation process of n-pentyl acetate is to use concentrated sulfuric acid as a catalyst, using glacial acetic acid and n-amyl alcohol as raw materials, through esterification, dehydration, lightening, and rectification. Although the reaction rate is faster with concentrated sulfuric acid as a catalyst, the There are also many side reactions, especially in the subsequent light removal and rectification process, due to the decomposition of n-pentyl acetate, the yield and quality will decrease. In addition, the existence of concentrated sulfuric acid will corrode the equipment, and a large amount of acid will be generated in the follow-up. waste water, seriously polluting the environment
With the continuous improvement of technology and production level, the production process of n-pentyl acetate is also constantly improved, but usually by selecting different catalysts to try, the common reports are modified molecular sieves, resins, solid superacids, hetero Polyacids, composite metal oxides, and acid-loaded activated carbon, etc., these catalysts have the advantage of not participating in the reaction system, belonging to heterogeneous catalysts, and easy to separate; but the disadvantages are that most of them are cumbersome to make, the price is high, the yield is average, and the service life It is not long and the follow-up processing is complicated, and it is impossible to realize industrialized mass production
The Chinese patent publication number is CN 105251538B and the invention name is a kind of catalyst H 6 P 2 W 15 Mo 3 o 62 / TiO 2 And the preparation method of n-pentyl acetate, although the productive rate of n-pentyl acetate has been improved under mild reaction conditions by improving the catalyzer, can not pollute the environment, but the synthetic steps of catalyzer are complicated, and increase production cost

Method used

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  • Preparation process and equipment of n-amyl acetate
  • Preparation process and equipment of n-amyl acetate

Examples

Experimental program
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Embodiment 1

[0044] A kind of preparation technology of n-pentyl acetate, such as figure 1 Shown, comprise the following steps: S1, esterification reaction

[0045] Add 300kg of n-amyl alcohol, 250kg of acetic acid, 1.5kg of p-toluenesulfonic acid, and 25kg of sec-butyl acetate into the reaction kettle, stir and heat to boiling reaction, reflux for 1.5h, and the esterification reaction is completed.

[0046] S2, dehydration

[0047] Open the phase separator, normal pressure dehydration, when the n-amyl alcohol content is lower than 0.1%, stop dehydration.

[0048] The main components of the reaction solution here are: 90% n-pentyl acetate, 2% acetic acid, and 0.1% n-amyl alcohol.

[0049] S3, weight loss

[0050] Send the reaction liquid into a thin film evaporator for distillation. The vacuum degree of the thin film evaporator is 50KPa, and the distillation temperature is 130°C. The intermediate product of n-pentyl acetate is collected from the gas phase outlet of the thin film evapora...

Embodiment 2

[0056] In order to support the preparation process of the above-mentioned n-pentyl acetate, the present invention also provides the equipment of n-pentyl acetate, such as figure 2 Shown, comprise reactor, be provided with raw material inlet on the side wall of the reaction section of reactor, be provided with gaseous phase outlet at the still top of reactor, and gaseous phase outlet is provided with three-way valve (not shown in the figure), reactor The bottom of the kettle is provided with a reaction liquid outlet;

[0057] a condenser, including a condensation inlet and a condensation outlet, the condensation inlet and the gas phase outlet are connected through a three-way valve;

[0058] A phase separator, including a phase separator inlet, a first outlet of the phase separator and a second outlet of the phase separator, the inlet of the phase separator is connected to the condensation outlet through a pipeline, and the first outlet of the phase separator is connected to t...

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Abstract

The invention relates to a preparation process of n-amyl acetate. The preparation process comprises the following steps: esterification reaction, dehydration, heavy component removal, light component removal and rectification. A homogeneous catalyst is adopted, and the catalyst is separated by combining a film evaporator, so that side reactions in the subsequent light component removal and rectification processes are greatly reduced, and meanwhile, the efficient conversion rate of the reaction part is ensured; and the prepared product is high in purity, can be stored for a long time, can neglect corrosion to equipment, and is extremely small in environmental pollution. In addition, the invention also provides equipment for the preparation process of n-amyl acetate. The equipment comprises a reaction kettle, a condenser, a phase splitter, the film evaporator, a heavy component collecting tank, a light component removal tower, a rectifying tower and a finished product tank to be matched with the preparation process.

Description

technical field [0001] The invention relates to the technical field of synthesis of acetate compounds, in particular to a preparation process and equipment for n-pentyl acetate. Background technique [0002] N-pentyl acetate, also known as "banana water", is a colorless and transparent liquid with banana and fruit aromas, slightly soluble in water, and miscible with alcohol and ether. N-pentyl acetate is widely used in cosmetics, spices, gunpowder, film, medicine, chemical industry, plastics and textiles and other industries. [0003] The traditional preparation process of n-pentyl acetate is to use concentrated sulfuric acid as a catalyst, using glacial acetic acid and n-amyl alcohol as raw materials, through esterification, dehydration, lightening, and rectification. Although the reaction rate is faster with concentrated sulfuric acid as a catalyst, the There are also many side reactions, especially in the subsequent light removal and rectification process, due to the dec...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/48C07C69/14C07C67/00C07C69/22C07C69/54C07C51/00C07C57/04
CPCC07C67/08C07C67/48C07C67/00C07C51/00C07C69/14C07C69/22C07C69/54C07C57/04
Inventor 黄飞龙刘涌张虎袁坚周凯戴祖红刘晓雯袁纪贤
Owner JIANGSU YIDA CHEM
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