CN102731250A - Method for synthesizing sec-butyl alcohol - Google Patents
Method for synthesizing sec-butyl alcohol Download PDFInfo
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- CN102731250A CN102731250A CN2012102309129A CN201210230912A CN102731250A CN 102731250 A CN102731250 A CN 102731250A CN 2012102309129 A CN2012102309129 A CN 2012102309129A CN 201210230912 A CN201210230912 A CN 201210230912A CN 102731250 A CN102731250 A CN 102731250A
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- butyl alcohol
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- alcohol
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Abstract
The invention discloses a method for synthesizing sec-butyl alcohol. In the method, sec-butyl acetate and methyl alcohol are used as raw materials, sec-butyl alcohol is produced by ester exchange, and the by-product is methyl acetate. The yield of sec-butyl alcohol is 50-90%. Compared with the method for preparing sec-butyl alcohol by n-butene hydration, the method is high in reaction speed, high in conversion rate and selectivity, mild in reaction conditions and less in corrosion for equipment; and the by-product methyl acetate is also an important industrial raw material.
Description
Technical field
The invention belongs to the organic synthesis field, be specifically related to a kind of method of synthetic sec-butyl alcohol.
Background technology
Sec-butyl alcohol has another name called the 2-butanols, is the liquid of no colour band fragrance, 99.5 ° of C of boiling point.Be mainly used in the manufacturing methyl ethyl ketone, account for 90% of total flow.Also can be used as the raw material of making softening agent, tensio-active agent, dressing agent, weedicide etc., also can replace propyl carbinol, or use as flotation agent, inhibitor as solvent.
The method of traditional mode of production sec-butyl alcohol is to be generated by n-butylene hydration, mainly contains the indirect hydration of sulfuric acid, resin catalysis direct hydration and three kinds of modes of heteropoly acid catalysis direct hydration.
(1) the indirect hydration of sulfuric acid: contain the hybrid C 4 cut of n-butene with concentration 50% sulfuric acid absorption, generate butyl sulfuric acid vinegar, hydrolysis obtains the sec-butyl alcohol aqueous solution again.Owing to use sulfuric acid to make reactant, cause equipment corrosion serious, plant investment is big, and consumes a large amount of sulphur bronsted lowry acids and bases bronsted lowries, and the three wastes of generation are many, and the n-butene unit consumption is higher.
(2) resin catalysis direct hydration: adopt the agent of solid sulfoacid type cation resin catalyzing, and it is high to the purity requirement of raw material n-butene to change synthetic route, but n-butene reaction per pass conversion is lower, generally is not higher than 10%.
(3) heteropoly acid catalysis direct hydration: adopt heteropolyacid catalyst, major ingredient is a molybdophosphate, and adds people's organometallic compound additive, 200～230 ℃ of temperature of reaction, reaction pressure 19.0MPa.N-butene per pass conversion 25%～30%.This synthetic route reaction pressure is high, and the transformation efficiency of n-butene is also lower.
Summary of the invention
The present invention is directed to the synthetic sec-butyl alcohol severe reaction conditions of hydration method, defective that the sec-butyl alcohol yield is lower, a kind of method of synthetic sec-butyl alcohol is provided.The yield of sec-butyl alcohol of the present invention reaches 50%～90%; Being equipped with sec-butyl alcohol with the n-butylene hydration legal system compares; Speed of reaction is fast, transformation efficiency is high, selectivity is high, reaction conditions is gentle, little to corrosion on Equipment, and by-product methyl acetate also is a kind of important industrial raw material.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of method of synthetic sec-butyl alcohol is a raw material with 2-butyl acetate and methyl alcohol, produces sec-butyl alcohol through transesterify, and by product is a ritalin.
Catalyst for reaction is one or more the mixture in sodium methylate, sodium hydroxide, the salt of wormwood.
The mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:1～1:4.
The mass percent of catalyzer in liquid stock is 0.01%～2%.
Temperature of reaction is 20～60 ℃.
Reaction pressure is 0.8～1.2atm.
Beneficial effect of the present invention: the transformation efficiency of 2-butyl acetate of the present invention can reach 50%～90%, and the yield of sec-butyl alcohol can reach 50%～90%.Have that speed of reaction is fast, transformation efficiency is high, selectivity is high, reaction conditions is gentle, to remarkable advantage such as corrosion on Equipment is little.
Embodiment
Below in conjunction with embodiment the present invention is done to further describe, case study on implementation will help to understand the present invention better, but the present invention is not limited only to following embodiment.
Embodiment 1
At volume is 1m
3Tank reactor in, be catalyzer with the sodium methylate, the mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:1; The mass percent of catalyzer in liquid stock is 0.4%, and temperature of reaction is 50 ℃, and reaction pressure is 1atm; Earlier the 420.3kg 2-butyl acetate is added in the reaction kettle and be preheating to temperature of reaction; Again sodium methylate 2.1kg is dissolved among the methyl alcohol 116kg, is heated to temperature of reaction, methanol solution is added in the reaction kettle react then.The transformation efficiency of 2-butyl acetate is 60.8%, and the yield of sec-butyl alcohol is 60.4%.
Embodiment 2
At volume is 1m
3Tank reactor in, be catalyzer with the sodium methylate, the mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:1; The mass percent of catalyzer in liquid stock is 0.38%, and temperature of reaction is 60 ℃, and reaction pressure is 1atm; Earlier the 420.3kg 2-butyl acetate is added in the reaction kettle and be preheating to temperature of reaction; Again sodium methylate 2.1kg is dissolved among the methyl alcohol 116kg, is heated to temperature of reaction, methanol solution is added in the reaction kettle react then.The transformation efficiency of 2-butyl acetate is 55.7%, and the yield of sec-butyl alcohol is 55.3%.
Embodiment 3
At volume is 1m
3Tank reactor in, be catalyzer with salt of wormwood, the mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:1.5; The mass percent of catalyzer in liquid stock is 0.4%, and temperature of reaction is 40 ℃, and reaction pressure is 1atm; Earlier the 420.3kg 2-butyl acetate is added in the reaction kettle and be preheating to temperature of reaction; Again salt of wormwood 2.1kg is dissolved among the methyl alcohol 116kg, is heated to temperature of reaction, methanol solution is added in the reaction kettle react then.The transformation efficiency of 2-butyl acetate is 50.2%, and the yield of sec-butyl alcohol is 49.8%.
Embodiment 4
At volume is 1m
3Tank reactor in, be catalyzer with the sodium methylate, the mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:2; The mass percent of catalyzer in liquid stock is 0.4%, and temperature of reaction is 55 ℃, and reaction pressure is 1atm; Earlier the 420.3kg 2-butyl acetate is added in the reaction kettle and be preheating to temperature of reaction; Again sodium methylate 2.1kg is dissolved among the methyl alcohol 116kg, is heated to temperature of reaction, methanol solution is added in the reaction kettle react then.The transformation efficiency of 2-butyl acetate is 84.5%, and the yield of sec-butyl alcohol is 83.6%.
Embodiment 5
At volume is 1m
3Tank reactor in, be catalyzer with the sodium methylate, the mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:1.4; The mass percent of catalyzer in liquid stock is 0.4%, and temperature of reaction is 50 ℃, and reaction pressure is 1atm; Earlier the 420.3kg 2-butyl acetate is added in the reaction kettle and be preheating to temperature of reaction; Again sodium methylate 2.1kg is dissolved among the methyl alcohol 116kg, is heated to temperature of reaction, methanol solution is added in the reaction kettle react then.The transformation efficiency of 2-butyl acetate is 77.5%, and the yield of sec-butyl alcohol is 77.2%.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (6)
1. the method for a synthetic sec-butyl alcohol, it is characterized in that: with 2-butyl acetate and methyl alcohol is raw material, produces sec-butyl alcohol through transesterify, by product is a ritalin.
2. the method for synthetic sec-butyl alcohol according to claim 1 is characterized in that: catalyst for reaction is one or more the mixture in sodium methylate, sodium hydroxide, the salt of wormwood.
3. the method for synthetic sec-butyl alcohol according to claim 1, it is characterized in that: the mol ratio of raw material 2-butyl acetate and methyl alcohol is 1:1～1:4.
4. the method for synthetic sec-butyl alcohol according to claim 1, it is characterized in that: the mass percent of catalyzer in liquid stock is 0.01%～2%.
5. the method for synthetic sec-butyl alcohol according to claim 1, it is characterized in that: temperature of reaction is 20～60 ℃.
6. the method for synthetic sec-butyl alcohol according to claim 1, it is characterized in that: reaction pressure is 0.8～1.2atm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102309129A CN102731250A (en) | 2012-07-05 | 2012-07-05 | Method for synthesizing sec-butyl alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102309129A CN102731250A (en) | 2012-07-05 | 2012-07-05 | Method for synthesizing sec-butyl alcohol |
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| CN102731250A true CN102731250A (en) | 2012-10-17 |
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| CN2012102309129A Pending CN102731250A (en) | 2012-07-05 | 2012-07-05 | Method for synthesizing sec-butyl alcohol |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058822A (en) * | 2013-01-16 | 2013-04-24 | 福州大学 | Method for using ionic liquid as catalyst to prepare sec-butyl alcohol |
| CN104475109A (en) * | 2014-11-20 | 2015-04-01 | 北京恩泽福莱科技有限公司 | Catalyst for preparing sec-butyl alcohol and preparation method of catalyst |
| CN108821967A (en) * | 2018-08-07 | 2018-11-16 | 中国天辰工程有限公司 | A kind of synthesis technology of high-purity Ester |
-
2012
- 2012-07-05 CN CN2012102309129A patent/CN102731250A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| WOJCIECH KROSZCZYNSKI ET AL.: "Effective High-Pressure Cleavage of Sterically Hindered Steroid Esters.", 《HELVETICA CHIMICA ACTA》, vol. 87, 2004, pages 1488 - 1492 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058822A (en) * | 2013-01-16 | 2013-04-24 | 福州大学 | Method for using ionic liquid as catalyst to prepare sec-butyl alcohol |
| CN104475109A (en) * | 2014-11-20 | 2015-04-01 | 北京恩泽福莱科技有限公司 | Catalyst for preparing sec-butyl alcohol and preparation method of catalyst |
| CN108821967A (en) * | 2018-08-07 | 2018-11-16 | 中国天辰工程有限公司 | A kind of synthesis technology of high-purity Ester |
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Application publication date: 20121017 |