CN107814778B - α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process - Google Patents
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Abstract
The invention discloses a α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process, which comprises the steps of taking acetoacetate and ethylene oxide as raw materials, adding alkali metal components into an alcohol solvent, reacting at 10-80 ℃, keeping the reaction time for 1 second-5 hours and the reaction pressure for 0.1-2Mpa, carrying out continuous condensation reaction by a continuous flow microchannel reactor to generate acetylbutyrolactone, obtaining a condensation reaction liquid, neutralizing the condensation reaction liquid by an acid solution, controlling the pH value to be 5-8, continuously evaporating at 40-80 ℃ under the pressure of 10-50kPa after neutralization, cooling to 20-40 ℃, extracting and layering by an organic solvent with the mass ratio of 0.1-1:1, removing the solvent from an organic layer obtained by extraction by a solvent removal tower, rectifying under the pressure of 0.1-1kPa to α -gamma-butyrolactone, and greatly improving the comprehensive production cost due to the adoption of the continuous distillation process.
Description
Technical Field
The invention belongs to the field of chemical synthesis, and particularly relates to a production method of α -acetyl-gamma-butyrolactone.
Background
α -acetyl-gamma-butyrolactone
The English name is 2-Acetylbutyrolactone, which is called Acetylbutyrolactone for short, and the English name is ABL for short.
The molecular formula is as follows: C6H8O3
Appearance: a colorless transparent liquid.
Solubility: the solubility in water was 20%.
Molecular weight: 128.13
Boiling point: 253 deg.C
Density: 1.191g/cm3
Flash point: 128 deg.C
Relative density 1.17
The application is as follows:
α -acetyl-gamma-butyrolactone (ABL) is a raw material for preparing vitamins (mainly used for synthesizing vitamin B1) and a main intermediate of chlorophyll, and can also be used for preparing medicines for treating angina pectoris, such as angina pectoris, and the like in the pharmaceutical industry.
The synthesis process in the prior art comprises the following steps:
α -acetyl-gamma-butyrolactone has two main methods for its industrial synthesis route:
one is the condensation reaction of gamma-butyrolactone in inert solvent and ethyl acetate under the action of sodium alkoxide. The process is a method commonly used in domestic industrial production at present. However, in the production process, toluene is used as a solvent, and a mixture of ethyl acetate and gamma-butyrolactone is added dropwise in a molten state of metal sodium, so that a large amount of acetate which is very easy to gasify and by-products of ethanol and hydrogen generated by reaction are generated at the reaction initiation stage, and accidents such as material flushing, combustion, even explosion and the like are easy to occur.
The other is a method of condensing and then closing the ring by the reaction of the acetoacetate and the ethylene oxide with sodium alkoxide or sodium hydroxide in methanol or ethanol, but the method adopts an intermittent method for production, has long reaction time, more side reactions, low yield and higher production cost compared with the former method.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a continuous flow microchannel reaction production process of α -acetyl-gamma-butyrolactone, which has simple process and high reaction efficiency.
The technical scheme of the invention is that an α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process takes acetoacetate and ethylene oxide as raw materials, under the action of adding alkali metal components into an alcohol solvent, the reaction temperature is 10-80 ℃, the reaction residence time is 1 second-5 hours, the reaction pressure is 0.1-2Mpa, continuous condensation reaction is carried out by a continuous flow microchannel reactor to generate the acetylbutyrolactone, and condensation reaction liquid is obtained, wherein the molar ratio of the ethylene oxide to the acetoacetate is 1-1.1, the molar ratio of the alkali metal components to the acetoacetate is 0.9-1.1, and the mass ratio of an alcohol solvent to the acetoacetate is 1-4.
Neutralizing the condensation reaction liquid obtained by the condensation reaction with an acid solution, controlling the pH value to be 5-8, continuously evaporating at 40-80 ℃ under the pressure of 10-50kPa after neutralization, cooling to 20-40 ℃ after evaporation, extracting and layering with an organic solvent in a mass ratio of 0.1-1:1, removing the solvent from the organic layer obtained by extraction through a solvent removal tower, and rectifying under the pressure of 0.1-1kPa to obtain the α -acetyl-gamma-butyrolactone product.
Preferably, the residence time of the reaction is from 0.5 hours to 5 hours.
According to the α -acetyl-gamma-butyrolactone continuous flow micro-channel reaction production process, the acetoacetate is preferably alkyl acetoacetate selected from methyl acetoacetate, ethyl acetoacetate, butyl acetoacetate and tert-butyl acetoacetate.
Further, the acetoacetate ester is methyl acetoacetate.
According to the α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process, preferably, the alcohol solvent is selected from one of methanol, ethanol, propanol, butanol and ethylene glycol.
According to the α -acetyl-gamma-butyrolactone continuous flow micro-channel reaction production process, the alkali metal component is preferably selected from alkali metal hydroxide or alkali metal alkoxide.
Further, the alkali metal is selected from sodium and potassium.
Further, the alkali metal component is preferably sodium hydroxide or sodium methoxide. That is, the alkali metal hydroxide is more preferably sodium hydroxide, and the alkali metal alkoxide is more preferably sodium methoxide.
According to the α -acetyl-gamma-butyrolactone continuous flow micro-channel reaction production process, the organic solvent is preferably one of an aromatic hydrocarbon solvent, an ester solvent and a halogen solvent.
According to the α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process, the acid solution is preferably one or more of hydrochloric acid solution, dilute sulfuric acid solution, dilute phosphoric acid and dilute acetic acid, and more preferably, the dilute sulfuric acid solution is 20-65% sulfuric acid solution.
According to the α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process, preferably, after continuous evaporation, recovered alcohol is dehydrated for recycling, the recovered solvent can be recycled for extraction, and acetoacetate obtained from rectification is recycled for condensation reaction.
The invention mainly aims at the problems of long time, more side reactions and low yield of the prior production process of adopting the intermittent condensation method under the action of alkali metal components in alcohol solvent of acetoacetate and ethylene oxide, and develops a new continuous production process.
The invention has the beneficial effects that:
the invention applies the process technology and the reaction equipment which take the continuous flow high flux microchannel reaction system as the core to the condensation reaction of the acetoacetate and the ethylene oxide, strengthens the process conditions, improves the reaction efficiency, realizes the continuous, safe, high-efficiency and stable production of the product, obviously improves the purity and the quality of the product, compared with the traditional intermittent process, the controllability of the reaction process is greatly improved, the efficiency of the reaction device is obviously enhanced, the danger of the process is obviously reduced due to continuous operation and greatly reduced material quantity of the reaction area, the productivity of the unit volume production device is multiplied, the method has reliable guarantee in the aspects of enhanced heat transfer, mass transfer, environmental protection and safety, and greatly reduces the generation of side reaction by technical means of enhanced process, accurate temperature control, short reaction time, reduction of reaction liquid holdup and the like, thereby avoiding the defects of low boiling point, flammability and explosiveness of the ethylene oxide. The process enables the conversion per pass of raw material acetoacetic ester to reach more than 84%, the yield per pass of ABL to reach more than 68%, and the total yield to reach more than 80%. The methanol, the toluene and the unreacted acetoacetate can be recycled, the process has high yield, and the comprehensive production cost is lower than that of the butyrolactone method. Meanwhile, the safety is greatly improved due to the adoption of a continuous synthesis process. The project integration technology fills up the domestic blank and reaches the international advanced level.
By adopting a batch process, the condensation reaction of the acetoacetate and the ethylene oxide under the action of alkali metal components in an alcohol solvent has the problems of long reaction time, more side reactions, low yield and the like, and the continuous condensation reaction of a novel continuous flow microchannel reactor generates the acetylbutyrolactone, so that the reaction time is short, the safety is high, the operation is stable and reliable, and the yield is obviously improved.
Detailed Description
Example 1:
a α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process comprises the following steps:
adding solid sodium hydroxide into methanol to prepare 20% methanol solution, pumping the methanol solution into a microchannel reactor at the same time of 400g/h, 232g/h methyl acetoacetate and 92g/h ethylene oxide (n methyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1.05:1), reacting at 50 ℃, 0.5Mpa and a retention time of 1 hour, adding 30% sulfuric acid into the reaction solution at the outlet at a speed of 360g/h, adjusting the pH to 5.5, continuously evaporating the methanol in an evaporator at an operating pressure of 20kpa, dehydrating the evaporated methanol at a temperature of 70 ℃, cooling the kettle liquid to 35 ℃, sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction with toluene simultaneously entering the bottom of the extraction tower at a speed of 150g/h, sending the extracted organic phase into a desolventizing tower at an operating pressure of 15kpa, recycling the evaporated toluene to extraction, sending the kettle liquid after removing the toluene into a reduced pressure rectifying tower at an operating pressure of 0.65kpa, using 36g/h of the obtained methyl acetoacetate for condensation reaction, carrying out a butyrolactone condensation reaction at a yield of α -84%, and converting the total yield of GC content of between 35.4% and 8.84% and a yield of between GC.
Example 2:
adding solid sodium hydroxide into methanol to prepare 20% methanol solution, pumping 232g/h methyl acetoacetate and 96g/h ethylene oxide (n methyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1.1:1.1) into a microchannel reactor by a pump at the same time, reacting at 50 ℃ and 0.5Mpa for 1 hour, adding 30% sulfuric acid into the reaction solution at the outlet at the speed of 393g/h, adjusting the pH value to 5.5, continuously evaporating the methanol in an evaporator at the operating pressure of 20kpa, dehydrating and recycling the evaporated methanol at the temperature of 70 ℃, cooling the kettle liquid to 35 ℃ and sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the toluene simultaneously entering the bottom of the extraction tower at the speed of 150g/h, sending the extracted organic phase into a desolventizing tower at the operating pressure of 15kpa, recycling the evaporated toluene to an extraction tower, sending the kettle liquid after removing the toluene into a reduced pressure rectifying tower at the operating pressure of 0.65kpa, using 35g/h of the obtained methyl acetoacetate for condensation reaction, carrying out the condensation reaction on the butyrolactone product with the content of 3580-84% of gamma-0.80%, and obtaining the total yield of 0.80% conversion rate of GC (GC-0.3-80%).
Example 3:
adding solid sodium hydroxide into methanol to prepare 20% methanol solution, pumping 232g/h methyl acetoacetate and 88g/h ethylene oxide (n methyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1:0.9) into a microchannel reactor by a pump at the same time, reacting at 50 ℃, 0.5Mpa for 1 hour, adding 30% sulfuric acid into the reaction solution at the outlet at a speed of 328g/h, adjusting the pH to 5.5, continuously evaporating methanol in an evaporator at an operating pressure of 20kpa, dehydrating the evaporated methanol at a temperature of 70 ℃, cooling the kettle liquid to 35 ℃, sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the kettle liquid and toluene simultaneously entering the bottom of the extraction tower at a speed of 150g/h, entering an extraction tower for an extracted organic phase, entering an extraction solvent tower at an operating pressure of 15kpa, recycling the evaporated toluene to an extraction tower, entering a reduced-pressure rectifying tower for an operating pressure of 0.65kpa, recycling 37g/h of the obtained methyl acetoacetate for condensation reaction, obtaining a butyrolactone product with a yield of α -84% of gamma-80%, and converting the total yield of 0.80% by GC (GC-80%).
Example 4:
adding solid sodium hydroxide into methanol to prepare 20% methanol solution, pumping the methanol solution into a microchannel reactor at the same time of 400g/h, 232g/h methyl acetoacetate and 92g/h ethylene oxide (n methyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1.05:1), reacting at 40 ℃, 0.4Mpa and a retention time of 2 hours, adding 30% sulfuric acid into the reaction solution at the outlet at a speed of 360g/h, adjusting the pH to 5.5, continuously evaporating the methanol in an evaporator at an operating pressure of 20kpa, dehydrating the evaporated methanol at a temperature of 70 ℃, cooling the kettle liquid to 35 ℃, sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the kettle liquid and toluene simultaneously entering the bottom of the extraction tower at a speed of 150g/h, entering an extraction tower from an extracted organic phase, recycling the distilled toluene to the extraction tower at an operating pressure of 15kpa, recycling the extracted toluene, entering a reduced pressure rectification tower from the kettle liquid after toluene removal, carrying out countercurrent extraction at an operating pressure of 0.65kpa, recycling 36g/h of the obtained methyl acetoacetate for condensation reaction, carrying out a butyrolactone condensation reaction at a yield of α -84%, and converting the total yield of GC content of 4.5-84% by GC (GC-80%).
Example 5:
adding solid sodium hydroxide into methanol to prepare 20% methanol solution, pumping the methanol solution into a microchannel reactor at the same time of 400g/h, 232g/h methyl acetoacetate and 92g/h ethylene oxide (n methyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1.05:1), reacting at 40 ℃, 0.4Mpa and a retention time of 2 hours, adding 40% sulfuric acid into the reaction solution at the outlet at a speed of 270g/h, adjusting the pH to 5.5, continuously evaporating the methanol in an evaporator at an operating pressure of 20kpa, dehydrating the evaporated methanol at a temperature of 70 ℃, cooling the kettle liquid to 35 ℃, sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the kettle liquid and toluene simultaneously entering the bottom of the extraction tower at a speed of 150g/h, entering an extraction tower from an extracted organic phase, recycling the distilled toluene to the extraction tower at an operating pressure of 15kpa, recycling the extracted toluene, entering a reduced pressure rectification tower from the kettle liquid after toluene removal, carrying out countercurrent extraction at an operating pressure of 0.65kpa, recycling 36g/h of the obtained methyl acetoacetate for condensation reaction, carrying out a butyrolactone condensation reaction at a yield of α -84%, and converting the total yield of GC content of 4.5-84% by GC (GC-80%).
Example 6:
adding methanol into sodium methoxide to prepare 27% methanol solution, pumping the methanol solution into a microchannel reactor at the same time of 400g/h, 232g/h of methyl acetoacetate and 92g/h of ethylene oxide (n-methyl acetoacetate: n-ethylene oxide: n-sodium methoxide is 1:1.05:1) to react at 50 ℃ under 0.5Mpa for 1 hour, adding 30% sulfuric acid into the reaction solution at the outlet at the speed of 360g/h, adjusting the pH to 5.5, continuously evaporating methanol in an evaporator at the operating pressure of 20kpa, dehydrating and recycling the distilled methanol at the temperature of 70 ℃, cooling the kettle liquid to 35 ℃ and sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the toluene entering the bottom of the extraction tower at the same time of 150g/h, entering an organic phase of a desolventizing tower at the operating pressure of 15kpa, recycling the distilled toluene to extraction, entering a reduced-pressure rectifying tower at the operating pressure of 0.65kpa, recycling 36g/h of the obtained methyl acetoacetate in a condensation reaction, obtaining α -84% of butyrolactone, converting the total yield of GC content of 4.5-80%, and converting the yield of GC.
Example 7:
adding solid sodium hydroxide into ethanol to prepare 20% ethanol solution, pumping the ethanol solution into a microchannel reactor at the same time of 400g/h, 260g/h of ethyl acetoacetate and 92g/h of ethylene oxide (n ethyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1.05:1), reacting at 50 ℃, 0.5Mpa and a retention time of 1 hour, adding 30% sulfuric acid into the reaction solution at the outlet at a speed of 360g/h, adjusting the pH to 5.5, continuously evaporating the ethanol in an evaporator at an operating pressure of 20kpa, dehydrating and recycling the evaporated ethanol at a temperature of 75 ℃, cooling the kettle liquid to 35 ℃, sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the kettle liquid and toluene simultaneously entering the bottom of the extraction tower at a speed of 150g/h, entering an extraction tower for an extracted organic phase, feeding the extracted organic phase into a desolventizer at an operating pressure of 15kpa, recycling the evaporated toluene to extraction, feeding the kettle liquid after toluene removal into a reduced pressure refining tower at an operating pressure of 0.65kpa, recycling 41g/h of the obtained ethyl acetoacetate for condensation reaction, obtaining a product with a yield of α -84%, and a total conversion yield of GC content of 0.80%, wherein GC is 0.7-80%, and the yield of gamma-80%.
Comparative example 1:
adding solid sodium hydroxide into methanol to prepare 20% methanol solution, 480g/h, 232g/h methyl acetoacetate and 106g/h ethylene oxide (n methyl acetoacetate: n ethylene oxide: n sodium hydroxide is 1:1.2:1.2), pumping the solution into a microchannel reactor by a pump at the same time, reacting at 50 ℃ and 0.5Mpa for 1 hour, adding 30% sulfuric acid into the solution at 426g/h in the reaction solution at an outlet, adjusting the pH value to 5.5, continuously evaporating the methanol in an evaporator at an operating pressure of 20kpa, dehydrating and recycling the evaporated methanol at a temperature of 70 ℃, cooling the kettle liquid to 35 ℃ and sending the kettle liquid to the top of an extraction tower, carrying out countercurrent extraction on the toluene simultaneously entering the bottom of the extraction tower at a speed of 150g/h, sending the extracted organic phase into a desolventizing tower at an operating pressure of 15kpa, recycling the evaporated toluene to an extraction tower, sending the kettle liquid after removing the toluene into a reduced pressure rectification tower at an operating pressure of 0.65kpa, using 26g/h of the obtained methyl acetoacetate for a condensation reaction, carrying out a condensation reaction on a butyrolactone product with a once-through conversion rate of 0.88-95% and a total conversion rate of GC (GC content of 0.8-95.8% and GC).
When the equivalent of ethylene oxide and sodium hydroxide was increased to 1.2, the reaction rate was increased, but the decomposition rate of α -acetyl- γ -butyrolactone produced was increased more than that of the main reaction, resulting in a decrease in yield of α -acetyl- γ -butyrolactone.
The present invention has been disclosed in terms of the preferred embodiment, but it is not intended to be limited to the embodiment, and all technical solutions obtained by substituting or converting the equivalent embodiments fall within the scope of the present invention.
Claims (7)
1. An α -acetyl-gamma-butyrolactone continuous flow microchannel reaction production process is characterized in that acetoacetic ester and ethylene oxide are used as raw materials, under the action of adding alkali metal components into an alcohol solvent, the reaction temperature is 10-80 ℃, the reaction residence time is 1 second-5 hours, the reaction pressure is 0.1-2Mpa, continuous condensation reaction is carried out by a continuous flow microchannel reactor to generate acetylbutyrolactone, so as to obtain a condensation reaction liquid, wherein the molar ratio of ethylene oxide to acetoacetic ester is 1-1.1, the molar ratio of alkali metal components to acetoacetic ester is 0.9-1.1, and the mass ratio of alcohol solvent to acetoacetic ester is 1-4;
neutralizing the condensation reaction liquid with acid solution, controlling the pH value to be 5-8, continuously evaporating at 40-80 ℃ under the pressure of 10-50kPa after neutralization, cooling to 20-40 ℃ after evaporation, extracting and layering with organic solvent in a mass ratio of 0.1-1:1, removing the solvent from the organic layer obtained by extraction through a solvent removal tower, and rectifying under the pressure of 0.1-1kPa to obtain the product α -acetyl-gamma-butyrolactone.
2. The continuous flow microchannel reaction process of α -acetyl-gamma-butyrolactone according to claim 1, wherein the acetoacetate is alkyl acetoacetate selected from methyl acetoacetate, ethyl acetoacetate, butyl acetoacetate, and tert-butyl acetoacetate.
3. The continuous flow microchannel reaction process of α -acetyl-gamma-butyrolactone according to claim 2, wherein the acetoacetate is methyl acetoacetate.
4. The continuous flow microchannel reaction process of α -acetyl-gamma-butyrolactone according to claim 1, wherein the alcoholic solvent is selected from methanol, ethanol, propanol, butanol, and ethylene glycol.
5. The continuous flow microchannel reaction process of α -acetyl-gamma-butyrolactone according to claim 1, wherein the organic solvent is one of aromatic hydrocarbon solvent, ester solvent, and halogen solvent.
6. The continuous flow microchannel reaction process of α -acetyl-gamma-butyrolactone according to claim 1, wherein the acid solution is one or more of hydrochloric acid solution, dilute sulfuric acid solution, dilute phosphoric acid, and dilute acetic acid.
7. The continuous flow microchannel reaction production process of α -acetyl-gamma-butyrolactone according to claim 1, wherein the recovered alcohol is dehydrated for reuse after continuous evaporation, the recovered solvent can be recycled for extraction, and the acetoacetate ester obtained from rectification is recycled for condensation reaction.
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| CN110156621B (en) * | 2019-05-08 | 2022-07-26 | 重庆建峰工业集团有限公司 | Method for liquid-liquid homogeneous phase synthesis of N, N-dimethylacetamide in microchannel reactor |
| CN111018810B (en) * | 2019-12-13 | 2021-09-14 | 浙江联盛化学股份有限公司 | Device and method for continuously producing alpha-acetyl-gamma-butyrolactone |
| CN112979461B (en) | 2021-02-26 | 2022-03-18 | 复旦大学 | Full continuous flow preparation method of 3-chloro-4-oxoacetic acid amyl ester |
| CN114044763B (en) * | 2022-01-13 | 2022-11-15 | 山东国邦药业有限公司 | Method for synthesizing gamma-butyrolactone |
| CN117720487A (en) * | 2023-12-16 | 2024-03-19 | 深圳智微通科技有限公司 | Method for continuously synthesizing alpha-acetyl-gamma-butyrolactone |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357545A (en) * | 2000-12-05 | 2002-07-10 | 大赛璐化学工业株式会社 | Prepn of alpha-acetyl-gamma butyrolactone |
| CN101522654A (en) * | 2006-10-03 | 2009-09-02 | 隆萨股份公司 | Process for the preparation of gamma-butyrolactones |
| CN103304519A (en) * | 2013-07-09 | 2013-09-18 | 浙江海正化工股份有限公司 | Method for preparing alpha-acetyl-gamma-butyrolactone by using recycled reaction material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1357545A (en) * | 2000-12-05 | 2002-07-10 | 大赛璐化学工业株式会社 | Prepn of alpha-acetyl-gamma butyrolactone |
| CN101522654A (en) * | 2006-10-03 | 2009-09-02 | 隆萨股份公司 | Process for the preparation of gamma-butyrolactones |
| CN103304519A (en) * | 2013-07-09 | 2013-09-18 | 浙江海正化工股份有限公司 | Method for preparing alpha-acetyl-gamma-butyrolactone by using recycled reaction material |
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