CN101092407B - Method for preparing alpha - acetyl - gamma - butyrolactone - Google Patents
Method for preparing alpha - acetyl - gamma - butyrolactone Download PDFInfo
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- CN101092407B CN101092407B CN200710025378A CN200710025378A CN101092407B CN 101092407 B CN101092407 B CN 101092407B CN 200710025378 A CN200710025378 A CN 200710025378A CN 200710025378 A CN200710025378 A CN 200710025378A CN 101092407 B CN101092407 B CN 101092407B
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Abstract
This invention discloses a method for preparing alpha-acetyl-gamma-butyrolactone, which comprises a reaction process and a distillation process. The reaction process comprises: pumping gasified gamma-butyrolactone and ethyl acetate into a reaction loaded with catalyst, and reacting. The method utilizes gamma-butyrolactone and ethyl acetate to react, thus can avoid potential safety hazard caused by using ethylene oxide. The method utilizes supported solid catalyst and fixed bed reactor, and continuous gasification reaction mode to change previous intermittent reaction to continuous reaction, which can realzie uniform distribution of the reactants, prolonged service life of the catalyst, and shortened reaction time, and eliminate the deficiencies of slow heat dissipation and difficult temperature control of reaction kettle. The method has such advantages as stable and safe production, and high product yield and purity. The content of alpha-acetyl-gamma-butyrolactone is greater than or equal to 99.4%, the content of water is less than or equal to 0.15%, and the yield is greater than or equal to 92%.
Description
Technical field
The present invention relates to the intermediates preparation of a kind of pharmaceuticals and organic industry medicine, more specifically to the preparation method of a kind of α-ethanoyl-gamma-butyrolactone.
Background technology
α-ethanoyl-gamma-butyrolactone is at medicine, proposed various preparation methods as the raw material of medicine or intermediate etc. in the organic chemical industry field.At present, the method for preparing α-ethanoyl-gamma-butyrolactone mainly contains two kinds of routes, and the first is the technology of starting raw material with oxyethane, and it two is to be the technology of starting raw material with the gamma-butyrolactone.Adopt oxyethane as first kind of operational path reaction raw materials, and oxyethane belongs to the inflammable and explosive chemical substance of one-level, exists serious security hidden danger in reaction, also be difficult to make simultaneously high-purity α-ethanoyl-gamma-butyrolactone; Adopting gamma-butyrolactone as second kind of operational path is the technology of the synthetic α-ethanoyl of starting raw material-gamma-butyrolactone; generally all with gamma-butyrolactone directly and sodium Metal 99.5 carry out rhythmic reaction at the enamel glass reactor; because it is too fierce to exist reaction; the reactor heat radiation is slow; problems such as the difficult control of temperature; often occur in the production process towards material, burning and explosive incident, causing both at home and abroad, many enterprises stop using this product of this explained hereafter.
In Chinese patent ZL03128773.5, mention and adopt the solvent of toluene as the sodium Metal 99.5 catalyzer in addition, toluene, sodium Metal 99.5 all belong to the inflammable and explosive chemical substance of one-level in fact, all exist serious potential safety hazard in transportation, storage, use; Though catalyst metal sodium is stirred in reactor as solvent by toluene, and adopt the special stainless steel material to make reactor, also have the rubbing effect of material and reactor eventually, still wall thickness attenuate causes unsafe factor in the use; Owing to adopt in the reaction process toluene to make solvent, in the phosphoric acid and etc. technological process, even last by distillation, the purity, yield and the elimination environmental pollution that also do not improve α-ethanoyl-gamma-butyrolactone; Last because intermittently tank reactor is still adopted in this invention, though improve, also exist heat radiation slow, the difficult control of temperature, problems such as long reaction time at aspects such as structures.
Summary of the invention
The objective of the invention is to solve the shortcoming that exists in the above-mentioned prior art, the preparation method of a kind of α-ethanoyl-gamma-butyrolactone is provided, this preparation method produces stable, safety, product yield and purity height.
The present invention is achieved by the following technical solutions:
The preparation method of α-ethanoyl of the present invention-gamma-butyrolactone comprises reaction workshop section and distillation workshop section, and described reaction workshop section is in the reactor of catalyzer is housed, and squeezes into the gamma-butyrolactone and the ethyl acetate of gasification continuously and reacts.
Among the preparation method of α-ethanoyl of the present invention-gamma-butyrolactone, the reactor described in the reaction workshop section is preferably fixed-bed reactor.
The preparation method of α-ethanoyl of the present invention-gamma-butyrolactone more further technical scheme be that its described reaction workshop section may further comprise the steps:
A) fixed-bed reactor that catalyzer will be housed earlier heat, and make bed temperature be raised to 160～270 ℃;
B) again will be squeeze into gamma-butyrolactone and the ethyl acetate that static mixer and gasifier gasified continuously reacts by fixed-bed reactor.
Among the preparation method of α-ethanoyl of the present invention-gamma-butyrolactone, its described catalyzer is preferred load type solid body base catalyst, further is preferably the load type solid body base catalyst that contains sodium or potash metal ingredient; Described load type solid body base catalyst preferably is made up of the Sodium Fluoride of the 30-50% of weight part or the silicon-dioxide of Potassium monofluoride and 50-70% and the composite oxides of aluminium sesquioxide, and wherein the weight proportion of silicon-dioxide and aluminium sesquioxide is 1: 1; Described load type solid body base catalyst or be made up of the Sodium Fluoride of the 30-50% of weight part or the silicon-dioxide of Potassium monofluoride and 50-70% and the composite oxides of zinc oxide, wherein the weight proportion of silicon-dioxide and zinc oxide is 1: 1.
Each raw material consumption proportion is preferably the mol ratio 1.05～1.10: 1 of ethyl acetate and gamma-butyrolactone in its reaction workshop section; The mol ratio of catalyzer and gamma-butyrolactone is preferably 0.15～0.20: 1.
Compared with prior art the invention has the beneficial effects as follows:
1, adopts gamma-butyrolactone and acetic acid ethyl reaction, avoided the potential safety hazard of using oxyethane to bring.
2, owing to used supported solid catalyzer and fixed-bed reactor, adopt the continuous gasification reactive mode, make original intermittent reaction become continuous reaction, material is evenly distributed, improved the work-ing life of catalyzer; And shortened the reaction times, eliminated defectives such as the tank reactor heat radiation is slow, the difficult control of temperature.
3, owing to adopted solid catalyst; do not need the benzene class to do solvent and acid neutralization,, significantly reduced pollution environment so not only eliminated the generation of source of pollution from the source; but also the creation good economic benefits is the novel environment-friendly process of a kind of α of production-ethanoyl-gamma-butyrolactone.
4, the present invention adopts the continuous reaction of solid catalyst, fixed-bed reactor; not only processing safety is protected, and has improved the quality and the yield of product, its α-ethanoyl-gamma-butyrolactone content 〉=99.4%; water-content≤0.15%, yield 〉=92%.
Embodiment
Below by specific embodiment explanation the present invention, but the present invention not merely is defined in these embodiment.
Embodiment 1
The present embodiment flow that feeds intake is that gamma-butyrolactone 500g/h, ethyl acetate are 537g/h, and the mol ratio of comprehensive evaluation catalyzer and gamma-butyrolactone is 0.16: 1, and whole process is divided into reaction workshop section and distillation workshop section, and concrete operations are as follows:
Step of reaction is carried out in the fixed-bed reactor that the supported solid catalyzer that the composite oxides that contain 40% Sodium Fluoride and 60% silicon-dioxide and aluminium sesquioxide form is housed; wherein the weight proportion of silicon-dioxide and aluminium sesquioxide is 1: 1; make bed temperature in the time of 170 ℃, begin charging; by volume pump with gamma-butyrolactone 500g/h; the flow of ethyl acetate 537g/h is squeezed into static mixer and gasifier continuously; make its gasification and react by fixed-bed reactor; reaction solution enters distillation tower after heat exchange; after the amount of being accumulated to; control the distillation tower temperature rise rate well; steam light constituent; thereafter carry out underpressure distillation again; configure reflux ratio by automatic adjusting reflux ratio device, online sampling analysis cuts and heavily steams after the head material is accumulated; content switches the finished product jar greater than 99%, obtains highly purified α-ethanoyl-gamma-butyrolactone.By the one-period continuous production, the mol ratio of comprehensive evaluation depletion load type solid catalyst and gamma-butyrolactone is 0.16: 1, total recovery 89.8%.
Actual conditions and the results are shown in Table 1.
Embodiment 2
The present embodiment catalyzer is made up of the composite oxides of 40% Potassium monofluoride and 60% silicon-dioxide and zinc oxide; wherein silicon-dioxide and zinc oxide weight proportion are 1: 1; the flow that feeds intake is that gamma-butyrolactone 500g/h, ethyl acetate 562g/h drop into continuously; other all operates this reaction similarly to Example 1, distill α-ethanoyl-gamma-butyrolactone; its total recovery is 91.2%, actual conditions and the results are shown in Table 1.
Embodiment 3
The present embodiment catalyzer is made up of the composite oxides that contain 40% Potassium monofluoride and 60% silicon-dioxide and aluminium sesquioxide; wherein the weight proportion of silicon-dioxide and aluminium sesquioxide is 1: 1; the flow that feeds intake is that gamma-butyrolactone 500g/h, ethyl acetate 547g/h drop into continuously; other all operates this reaction similarly to Example 1, distill α-ethanoyl-gamma-butyrolactone; its total recovery is 92.2%, actual conditions and the results are shown in Table 1.
Table 1:
Claims (4)
1. the preparation method of α-ethanoyl-gamma-butyrolactone; comprise reaction workshop section and distillation workshop section; it is characterized in that described reaction workshop section is in the fixed-bed reactor of load type solid body base catalyst are housed; squeezing into the gamma-butyrolactone and the ethyl acetate of vaporization continuously reacts; described load type solid body base catalyst is made up of the Sodium Fluoride of the 30-50% of weight part or the silicon-dioxide of Potassium monofluoride and 50-70% and the composite oxides of aluminium sesquioxide; wherein the weight proportion of silicon-dioxide and aluminium sesquioxide is 1: 1; or load type solid body base catalyst is made up of the Sodium Fluoride of the 30-50% of weight part or the silicon-dioxide of Potassium monofluoride and 50-70% and the composite oxides of zinc oxide, and wherein the weight proportion of silicon-dioxide and zinc oxide is 1: 1.
2. the preparation method of a kind of α-ethanoyl according to claim 1-gamma-butyrolactone is characterized in that described reaction workshop section may further comprise the steps:
A) fixed-bed reactor that catalyzer will be housed earlier heat, and make bed temperature be raised to 160～270 ℃;
B) again will be squeeze into gamma-butyrolactone and the ethyl acetate that static mixer and gasifier gasified continuously reacts by fixed-bed reactor.
3. the preparation method of a kind of α-ethanoyl according to claim 1 and 2-gamma-butyrolactone is characterized in that reacting that each raw material consumption proportion is the mol ratio 1.05～1.10: 1 of ethyl acetate and gamma-butyrolactone in the workshop section; The mol ratio of catalyzer and gamma-butyrolactone is 0.15～0.20: 1.
4. the preparation method of a kind of α-ethanoyl according to claim 2-gamma-butyrolactone is characterized in that described reaction workshop section may further comprise the steps:
A) the load type solid body base catalyst fixed-bed reactor that sodium or potash metal ingredient will be housed earlier heat, and make bed temperature be raised to 170 ℃;
B) gamma-butyrolactone is squeezed into static mixer and gasifier with flow, the ethyl acetate of 500g/h continuously with the flow of 547g/h, the gamma-butyrolactone and the ethyl acetate that gasified are reacted by fixed-bed reactor continuously.
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| CN200710025378A CN101092407B (en) | 2007-07-27 | 2007-07-27 | Method for preparing alpha - acetyl - gamma - butyrolactone |
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| CN200710025378A CN101092407B (en) | 2007-07-27 | 2007-07-27 | Method for preparing alpha - acetyl - gamma - butyrolactone |
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| CN101092407B true CN101092407B (en) | 2010-05-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107857745A (en) * | 2017-12-12 | 2018-03-30 | 安徽国星生物化学有限公司 | A kind of synthetic method of α acetyl group gamma butyrolactone |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102030728A (en) * | 2010-04-07 | 2011-04-27 | 上海南化科技发展有限公司 | Two-stage rectifying process for acetylbutyrolactone |
| CN102030729B (en) * | 2010-11-04 | 2012-05-23 | 山西大学 | Preparation method of alpha-acetyl-gamma-butyrolactone |
| CN102229586B (en) * | 2011-05-13 | 2012-12-19 | 山西三维集团股份有限公司 | Preparation method for alpha-acetyl-gamma-butyrolactone |
| CN103387557B (en) * | 2012-05-08 | 2015-03-11 | 江苏兄弟维生素有限公司 | Continuous synthesis process of alpha-chloro-alpha-acetyl-gamma-butyrolactone |
| CN108299345B (en) * | 2018-02-09 | 2021-06-11 | 东北制药集团股份有限公司 | Preparation method of alpha-acetyl-gamma-butyrolactone |
| 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 |
| CN117720487B (en) * | 2023-12-16 | 2024-08-06 | 深圳智微通科技有限公司 | Method for continuously synthesizing alpha-acetyl-gamma-butyrolactone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5789603A (en) * | 1996-02-24 | 1998-08-04 | Huels Aktiengesellschaft | Method for preparing 2-acetyl-γ-butyrolactone |
| CN1548427A (en) * | 2003-05-10 | 2004-11-24 | 浙江联盛化学工业有限公司 | Prepn process and apparatus for alpha-acetyl-gamma-butyrolactone |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5789603A (en) * | 1996-02-24 | 1998-08-04 | Huels Aktiengesellschaft | Method for preparing 2-acetyl-γ-butyrolactone |
| CN1548427A (en) * | 2003-05-10 | 2004-11-24 | 浙江联盛化学工业有限公司 | Prepn process and apparatus for alpha-acetyl-gamma-butyrolactone |
Non-Patent Citations (2)
| Title |
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| 张莉.α-乙酰基γ-丁内酯的合成及进展.湖北化工 4.1999,(4),23-24. |
| 张莉.α-乙酰基γ-丁内酯的合成及进展.湖北化工 4.1999,(4),23-24. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107857745A (en) * | 2017-12-12 | 2018-03-30 | 安徽国星生物化学有限公司 | A kind of synthetic method of α acetyl group gamma butyrolactone |
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