CN1324788A - Recovery and utilization method of high and middle boiling point residue from ethyl acetate producing by acetaldehyde condensation - Google Patents
Recovery and utilization method of high and middle boiling point residue from ethyl acetate producing by acetaldehyde condensation Download PDFInfo
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- CN1324788A CN1324788A CN 00117835 CN00117835A CN1324788A CN 1324788 A CN1324788 A CN 1324788A CN 00117835 CN00117835 CN 00117835 CN 00117835 A CN00117835 A CN 00117835A CN 1324788 A CN1324788 A CN 1324788A
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- acetaldehyde
- ethyl acetate
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Abstract
A method for recovering and utilizing high-boiling point residual liquor produced in the course of production of ethyl acetate by using the acetaldehyde condensation method, belonging to the field of organic chemical industry, is characterized by adding small quantity of water to the residual liquor with high boiling point, selecting and using a proper catalyst, decomposing most of aldehyde acetal under the condition of heating to obtain ethyl alcohol and acetaldehyde, then returning them to the production system so as to implement a method for reutilizing and treating waste liquor.
Description
The invention provides a method for recycling high-boiling-point residual liquid discharged as waste liquid in a refining process of an industrial device for producing ethyl acetate by an acetaldehyde condensation method, belonging to the field of organic chemical industry.
The process for producing ethyl acetate by condensation of acetaldehyde (patent application No. 98116923.6) produces a high boiling point residue during the product purification in an industrial plant. The residual liquid contains ethyl acetate, and contains acetal as the main component generated in condensation reaction, and small amount of high boiling point compounds such as crotonaldehyde, paraldehyde, acetic acid, etc. from raw materials. The residual liquid can only be treated by burning, and the treatment method wastes production raw materials and causes secondary pollution to the environment due to burning.
The invention provides a waste liquid treatment method which adds a proper amount of water into a high boiling point residual liquid to decompose acetal in the residual liquid and then returns the decomposed acetal to a reaction system to be reused.
The specific implementation method of the invention is as follows:
since acetal is formed by the reaction of ethanol and acetaldehyde, this reaction is a reversible reaction, and acetal and water can in turn form ethanol and acetaldehyde when conditions are appropriate. The reaction equation is as follows:
the specific implementation method is that a small amount of water is added into the high boiling point residual liquid, and a proper catalyst is selected, most of acetal is decomposed under the heating condition, so that ethanol and acetaldehyde are obtained, and the ethanol and the acetaldehyde are the production raw materials for preparing ethyl acetate by acetaldehyde condensation, so that the ethanol and the ethyl acetate in the residual liquid can be directly returned to a production system for recycling, and the environmental pollution caused by the discharge of the high boiling point residual liquid is fundamentally eliminated.
The catalyst used in the present invention can be selected from various acidic and basic substances. The acidic substances are: inorganic acids, organic acids, solid acids, acidic inorganic salts, acidic organic salts, acidic oxides, and the like; the alkaline substances are: inorganic bases, organic bases, basic inorganic salts, basic organic salts, basic oxides, and the like. Wherein the addition amount of the acid and alkali catalyst is 0.1-10%, preferably 1-5% of the reaction liquid amount.
The amount of water used in the present invention is usually 1: 100, preferably 1: 10, in terms of the molar ratio of acetal to water contained in the reaction solution. The decomposition reaction temperature is 50-100 deg.C, preferably 80-90 deg.C. The decomposition reaction time is usually not more than 8 hours, preferably 2 to 5 hours.
The implementation of the invention can reduce the unit consumption of raw materials for producing the ethyl acetate and the environmental pollution, and is an effective way for changing waste into valuable.
Example 1
A500 ml three-necked flask equipped with a reflux condenser, a thermometer and a stirring device was charged with 210g of ethyl acetate, 90g of acetal and 20ml of distilled water, and then 0.3g of a solid phosphomolybdic acid catalyst was added thereto, followed by heating and refluxing for 4 hours. The decomposition rate of acetal by gas chromatography can reach 92.5%.
Example 2
5.0g of hydrochloric acid was used as a catalyst in place of solid phosphomolybdic acid, and the procedure of example 1 was repeated under reflux for 4 hours. The decomposition rate of acetal by gas chromatography analysis can reach 99.3%.
Claims (4)
1. A process for recovering the high-boiling-point residual liquid from ethyl acetate production by acetaldehyde condensation method features that a small amount of water is added to said high-boiling-point residual liquid, and a proper catalyst is used to decompose most of acetal under heating condition to obtain alcohol and acetaldehyde, which are then returned to production system for reuse.
2. The process for recovering high-boiling-point residual liquid in the production of ethyl acetate by acetaldehyde condensation as claimed in claim 1, wherein the catalyst used in the decomposition reaction may be an acidic substance: inorganic acids, organic acids, solid acids, acidic inorganic salts, acidic organic salts, acidic oxides, and the like; the alkaline substances are: inorganic base, organic base, alkaline inorganic salt, alkaline organic salt, alkaline oxide and the like, wherein the adding amount of the acid and the alkaline catalyst is 0.1 to 10 percent of the reaction liquid amount.
3. The process for recovering a high-boiling residue from the production of ethyl acetate by the condensation of acetaldehyde as claimed in claim 1, wherein the amount of water used for the decomposition reaction is 1: 100 by mole ratio of acetal to water.
4. The process for recovering high-boiling residue from the production of ethyl acetate by the condensation of acetaldehyde as claimed in claim 1, wherein the decomposition reaction temperature is 50 to 100 ℃ and the reaction time is not more than 8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00117835A CN1115322C (en) | 2000-05-23 | 2000-05-23 | Recovery and utilization method of high and middle boiling point residue from ethyl acetate producing by acetaldehyde condensation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00117835A CN1115322C (en) | 2000-05-23 | 2000-05-23 | Recovery and utilization method of high and middle boiling point residue from ethyl acetate producing by acetaldehyde condensation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1324788A true CN1324788A (en) | 2001-12-05 |
| CN1115322C CN1115322C (en) | 2003-07-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00117835A Expired - Fee Related CN1115322C (en) | 2000-05-23 | 2000-05-23 | Recovery and utilization method of high and middle boiling point residue from ethyl acetate producing by acetaldehyde condensation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1115322C (en) |
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2000
- 2000-05-23 CN CN00117835A patent/CN1115322C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1115322C (en) | 2003-07-23 |
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