CN1115322C - 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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- CN1115322C CN1115322C CN00117835A CN00117835A CN1115322C CN 1115322 C CN1115322 C CN 1115322C CN 00117835 A CN00117835 A CN 00117835A CN 00117835 A CN00117835 A CN 00117835A CN 1115322 C CN1115322 C CN 1115322C
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- acetaldehyde
- ethyl acetate
- acetal
- residual liquid
- boiling
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Abstract
The present invention relates to a recovery and utilization method of a high boiling point residue from ethyl acetate produced by an acetaldehyde condensation method, which belongs to the organic chemical industry field. The present invention is a residue processing method that most of acetal is decomposed under the heating condition to obtain alcohol and acetaldehyde by adding little water in the high boiling point residue and using proper catalyst, and the alcohol and the acetaldehyde return to a production system to be recycled. Using the method can make almost all acetal generated in the condensation reaction decomposed and recovered. Thereby, the unit consumption of raw materials for producing the ethyl acetate is reduced, and the environment pollution is decreased.
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.
In the process for producing ethyl acetate by condensing acetaldehyde (patent application No. 98116923.6), a high-boiling residue is produced in the product refining process of an industrial plant. The residual liquid contains ethyl acetate, and its main component is acetal as by-product produced in condensation reaction, and in addition, it contains a small amount of high-boiling-point compounds of crotonaldehyde, paraldehyde and acetic acid, etc. brought by production raw material. 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 acetal to a production 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; the alkaline substances are: inorganic base, organic base, basic inorganic salt, basic organic salt, basic oxide. 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: 1.5 to 100, preferably 1: 1.5 to 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 refluxing at 80 to 90 ℃ for 4 hours. The decomposition rate of the acetal can reach 92.5 percent through gas chromatography analysis.
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. The decomposition rate of the acetal can reach 99.3 percent through gas chromatography analysis.
Claims (4)
1. The method for recycling the high-boiling-point residual liquid in the production of the ethyl acetate by the acetaldehyde condensation method is characterized by comprising the following steps of: adding water into the high boiling point residual liquid according to the molar ratio of acetal to water contained in the high boiling point residual liquid of 1: 1.5-100, selecting acid or alkaline substances as catalysts, wherein the adding amount of the catalysts is 0.1% -10% of the reaction liquid amount, decomposing most of acetal at the reaction temperature of 50-100 ℃ for not more than 8 hours to obtain ethanol and acetaldehyde, and returning the ethanol and acetaldehyde to a production system for reutilization.
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 any one of the following acidic substances: inorganic acids, organic acids, solid acids, acidic inorganic salts, acidic organic salts, acidic oxides; the alkaline substances are: inorganic base, organic base, alkaline inorganic salt, alkaline organic salt and alkaline oxide, wherein the addition amount of the acid and alkali catalyst is 1-5% 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: 1.5 to 10 in terms of the molar ratio of acetal to water.
4. 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 decomposition reaction temperature is 80-90 ℃ and the reaction time is 2-5 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 CN1324788A (en) | 2001-12-05 |
| CN1115322C true 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
Non-Patent Citations (3)
| Title |
|---|
| 化学与粘合，第3期 1993-01-01 刘业成等 ，乙醛缩合制乙酸乙酯 * |
| 化学与粘合，第3期 1993-01-01 刘业成等 ，乙醛缩合制乙酸乙酯;精细化工，15(4) 1998-01-01 张俊华，陈永生，乙醛法合成乙酸乙酯 * |
| 精细化工，15(4) 1998-01-01 张俊华，陈永生，乙醛法合成乙酸乙酯 * |
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| Publication number | Publication date |
|---|---|
| CN1324788A (en) | 2001-12-05 |
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