Separation method for equatic mixture of formic acid and acetic acid

A separation method and mixture technology, applied in the separation/purification of carboxylic acid compounds, etc., can solve the problems of limited application range, low price, low isolation agent, etc., and achieve the effects of obvious social benefits, simple equipment and low energy consumption

Inactive Publication Date: 2006-02-01
中国石化集团扬子石油化工有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the mixture is in the stage of direct use, mainly used in the manufacture of waterproofing agents, low release agents, etc., the application range is not wide, and the price is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add the aqueous mixture of formic acid and acetic acid (7 batches of mixed acids with different water contents were selected as raw materials during the test) and the entrainer ethyl acetate in the dehydration tower kettle, heat, and when the vapor-liquid in the tower reaches equilibrium, fully reflux for 2-3 hours , when the temperature at the top of the tower is controlled at t≤70.4°C, the distillate is separated from the water phase and the ester phase by a water separator, the water phase is collected, and the ester phase is returned to the bottom of the tank. Carry water about 9% each time, dehydrate repeatedly like this, till the water in the kettle liquid can not be taken out. The residual ester was distilled off. After the kettle liquid is collected, formic acid and acetic acid are separated. The dehydration results are shown in Table 1.

[0017] The dehydration results show that: the water content in the feed mixed acid is different. After azeotropic dehydrat...

Embodiment 2

[0019] Add the still liquid of the dehydrating distillation tower to the still of the separation and rectification tower, heat it, and when the vapor-liquid in the tower reaches equilibrium, reflux for 2-3 hours, control the temperature at the top of the tower to 97.0-101.8°C to collect light components, and control the temperature at the top of the tower The transition fraction was collected at 101.9-116.0°C, and the separation results are shown in Table 2.

[0020] serial number

[0021] serial number

[0022] The results show that: due to the large change in the content of formic acid and acetic acid components in the transition fraction, the content of formic acid components increases, which is greater than 38%. The content of acetic acid component is reduced, less than 45%, and the content of water and impurities is reduced. The transition fraction is added to the next batch of mixed acids for treatment. When the formic acid content in the transition ...

Embodiment 3

[0024] After the light components and transition fractions are separated on the separation tower, the temperature at the top of the tower is 116.1-118.0°C, and the finished product of acetic acid is separated and collected. The purity and yield of separated acetic acid finished products are shown in Table 3.

[0025]

[0026] The results show that the separated product acetic acid has a purity greater than 99% and an average single-pass yield of 78.1%.

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Abstract

A process for separating acetic acid from the aqueous mixture of formic acid and acetic acid includes such steps as adding azeotrpic agent to the said mixture, then rectification, azeotropic dewatering (until water content less than 2%), rectifying to obtain light component, transition fraction and acetic acid, separating water from the water phase generated by dewatering step, recovering azeotropic agent, and adding said light component and transition fraction to the said mixture as raw material. Its advantage is high purity of acetic acid (more than 99%).

Description

technical field [0001] The present invention relates to the separation method of formic acid and acetic acid. Background technique [0002] Organic mixed acid (aqueous mixture of formic acid and acetic acid) is a by-product of direct oxidation of acetaldehyde to produce acetic acid. At present, the mixture is in the stage of direct use, and is mainly used in the manufacture of waterproofing agents, low-release agents, etc., and the application range is not wide, and the price is low. A set of 70,000 tons of acetic acid plant produces about 1,140 tons of formic acid and acetic acid aqueous mixture every year during the production process. The formic acid content is about 5-17%, and the acetic acid content is about 62-80%. If formic acid and acetic acid are separated to obtain basic chemical raw materials Acetic and formic acids will be of great benefit. Contents of the invention [0003] The purpose of this invention is to provide a kind of formic acid, the separation of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/02C07C53/08C07C51/44
Inventor 黄秋明李明亮周鹏朱家德朱桂莲王珩姝霍玉林邵学华甘秋填徐盛谨阙子龙许红林
Owner 中国石化集团扬子石油化工有限责任公司
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