CN102658095A - Alcohol adsorption material and application and using method thereof - Google Patents
Alcohol adsorption material and application and using method thereof Download PDFInfo
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- CN102658095A CN102658095A CN2012101635811A CN201210163581A CN102658095A CN 102658095 A CN102658095 A CN 102658095A CN 2012101635811 A CN2012101635811 A CN 2012101635811A CN 201210163581 A CN201210163581 A CN 201210163581A CN 102658095 A CN102658095 A CN 102658095A
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Abstract
The invention relates to an alcohol adsorption material and application and a using method thereof. The material is prepared by performing free radical polymerization reaction on a polymeric monomer under the action of a polymerization initiator, wherein the polymeric monomer consists of 60 to 80 volume percent of butyl acrylate monomer or methyl methacrylate monomer or a mixture of the monomers and 20 to 40 volume percent of hydroxyethyl acrylate monomer; and the addition amount of the initiator is 0.1 to 0.8 percent based on the weight of the polymeric monomer. The alcohol adsorption material can selectively adsorb alcohol in an alcohol aqueous solution at room temperature, and can be applied to the low-temperature extraction of the alcohol; continuous fermentation can be realized, and the work period of yeast is prolonged; the degree of wine can be reduced in short time; and in addition, the alcohol adsorption material is easy to prepare and low in cost.
Description
Technical field
The present invention relates to a kind of purposes and usage with alcohol sorbing material and this material of selective absorption alcohol functionality.
Background technology
With the fuel alcohol of fermentative Production, have the fuel performance similar, but its raw materials for production are biogenic with fossil fuel, be a kind of regenerative resource.Theoretically; Carbon dioxide that is discharged in the ethanol combustion process and the carbon dioxide that growth is consumed as the bioenergy of raw material quantitatively maintain an equal level; This is significant to reducing atmosphere pollution and suppressing greenhouse effects, and therefore fuel alcohol also is called as clean fuel.Since 20th century, energy crisis took place in the end of the year 70; People begin to pay close attention to the utilization of regenerative resource; Adopt crops fermentative Production absolute alcohol to substitute or partly substitute gasoline and put on schedule,, can add the absolute alcohol of 10-15% in the gasoline according to the new fuel oil in the world.Four big fermentation alcohol producing countries are Brazil in the world, and the U.S. is Chinese and Russian.Brazil's annual production reaches 1,200 ten thousand tons, almost all is used for gasoline replacing, as the fuel of automobile.The U.S. produces fermentation alcohol per year and exceedes 2,000,000 tons, and is most of as the preparation gasohol.Russia produces nearly ten thousand tons of alcohol per year, is mainly used in alcoholic beverages such as preparation vodka.Fuel alcohol is in the U.S., national successful application such as Brazil more than 20 year, be defined in 37 used gasoline of metropolitan automobile like the U.S. and must add 5 kinds of fuel alcohols.In recent decades, through introducing the advanced technology of Alcohol Production and the autonomous research and development of China in the world, China is in the Alcohol Production technology, and the level of aspects such as equipment manufacturing technology is greatly improved, and the improvement of environmental pollution has obtained very big improvement.But in industry generally, also has a segment distance from especially cleaner production target of modern alcohol industry system.Therefore, need to strengthen the dynamics and the input of scientific and technological development, constantly bring forth new ideas, improve constantly, strengthening the market competition strength of enterprise, thereby improve the production technology level and the strength of whole industry.
Utilize the fermentation of agricultural crop straw to produce alcohol, the concentration of alcohol reaches about 15% in fermentation tank, and mushrooms such as yeast are stopped action; And by cereal crops (cereal, potato class, molasses) through boiling; Saccharification, the alcohol content volume fraction in the zymotic fluid that obtains after the processing such as fermentation very low (10%), and also impurity content is high; Often need carry out post processing, make it reach quality requirement it.The purification of alcohol mainly is to be main with high temperature rectifying, but this method needs huge investment, complex equipments, and also energy consumption is high, and expensive and responsive yeast are had mortality.In general, the alcohol in the zymotic fluid is processed the 50-80% that absolute alcohol will occupy energy consumption in the whole absolute alcohol production process.When adopting benzene sequence of constant boiling and rectification method, the added value of one ton of absolute alcohol of every production is about 2000 yuan, has lost the competitiveness with gasoline greatly, and the dewatering process of therefore seeking low energy consumption is imperative.
The nontraditional technology method that absolute alcohol is purified can operate at normal temperatures and energy consumption low.Such technology mainly comprises liquid-liquid technique, overcritical and subcritical abstraction technology, molecular sieve adsorbing and dewatering technology and pervaporation technology etc.
The principle of liquid-liquid technique is to utilize the difference of extractant to the solubility of second alcohol and water; Extractant is joined in the solution of second alcohol and water; Under suitable operating condition, a certain component in the solution evenly is diffused in the extractant, thereby reaches the purpose that improves alcohol concentration.Extraction phase is easy to separate, can recycling.This method equipment investment is few, easy and simple to handle, and labour intensity is low, and separation accuracy is high, can make the ethanol of different purity as required.
The key of adsorption dewatering technology is to select suitable adsorbent.Adsorbent commonly used has lime, active carbon, ion exchange resin, molecular sieve, silica gel etc.The effect of adsorbent is moisture and the small amount of ethanol in the adsorbent solution, thereby the volume fraction of ethanol is reached more than 99.5%, and adsorbent itself can obtain regeneration.Generally acknowledge molecular sieve adsorbing and dewatering method good energy-conserving effect at present in the world, it is the most frequently used to produce absolute alcohol with the molecular sieve adsorbing and dewatering method.Molecular sieve is one type of silicate crystal with skeleton structure, can carry out cation exchange and reversible dehydration.Compare with adsorbents such as silica gel and activated aluminas, molecular sieve has strong water sorption, and its reason is that the aperture of molecular sieve is less, and size is suitable with hydrone, superposes thereby produce ultra hole wall field, strong especially absorption affinity occurs; And except the adsorption of hole wall field, molecular sieve also has bigger electrostatic force.The existence of two kinds of active forces makes that the absorption affinity of adsorbent of molecular sieve is strong especially.
The character of active carbon mainly shows as adsorptivity, chemical, catalytic and mechanicalness.The critical process of making active carbon is activation, according to the difference of used activator, can be divided into two types of chemicals activation method and gas activation methods.The contained mineral matter of raw material focuses in activation becomes ash content in the active carbon, the main component of ash content is the salt of alkali metal and alkaline-earth metal, like phosphate etc.Other organic matters or the inorganic matter that will contain more water soluble or ethanol in such active carbon make wine body band look, solid content exceeds standard or produce the shelf life deposited phenomenon, brings the abominable influence that can't retrieve to vinosity.Make a general survey of in recent years kind, use amount and action time about active carbon, the document to the aspects such as influence of fragrance component reservation amounts such as the acid of product, ester generally lays particular emphasis on the physical absorption of active carbon, and has ignored the influence of its chemisorbed to vinosity.The adsorptivity of active carbon had both depended on pore structure, depended on chemical composition again.Increase along with amount of activated; The equal decrease to some degree of content of higher fatty acid ethyl esterses such as ethyl hexanoate, ethyl lactate, ethyl acetate, ethyl butyrate isochromatic spectrum framework ingredient and ethyl palmitate, ethyl linoleate, ethyl oleate in the wine; To adsorbing consumption is 2.0% o'clock, and the high-grade aliphatic ester composition in the wine is then by absorption fully.Different activity charcoal product to trace flavor component in the wine and turbidity removal effect to influence difference little.
Summary of the invention
Technical problem to be solved by this invention provides a kind of alcohol sorbing material simple, that cost is low, alternative is adsorbed alcohol for preparing.
The present invention also relates to the purposes and the usage of alcohol sorbing material simultaneously.
For solving above technical problem, a kind of technical scheme that the present invention takes is:
A kind of alcohol sorbing material; It issues living Raolical polymerizable by polymerization single polymerization monomer in the effect of polymerization initiator and obtains; Cumulative volume with polymerization single polymerization monomer is a benchmark; Polymerization single polymerization monomer is made up of with hydroxy-ethyl acrylate monomer 20% ~ 40% Butyl Acrylate Monomer or methyl methacrylate monomer or the mixing of the two 60% ~ 80%, and the adding weight of said initator is 0.1% ~ 0.8% of polymerization single polymerization monomer weight.
According to the present invention, described Raolical polymerizable can carry out according to mode known in the art.According to a concrete aspect of the present invention; Said Raolical polymerizable is implemented as follows: with Butyl Acrylate Monomer or methyl methacrylate monomer or the mixing of the two, and the hydroxy-ethyl acrylate monomer joins in the solvent in proportion, and the formation total volume concentration is 5 ~ 30% solution; Add polymerization initiator then; Use the inert gas deoxygenation, maintain under the initiation temperature of polymerization initiator and react, reaction finishes promptly to get said alcohol sorbing material.
Preferably, described polymerization initiator is middle temperature initator, and its initiation temperature is 30 ℃ ~ 100 ℃.In a representational embodiment, for example said polymerization initiator is an azo-bis-isobutyl cyanide, and solvent is an oxolane, is reflected under 50 ~ 60 ℃ of the temperature to carry out.The adding weight of azo-bis-isobutyl cyanide is preferably 0.3% ~ 0.6% for example 0.5% of polymerization single polymerization monomer weight.
According to alcohol sorbing material of the present invention, wherein butyl acrylate and methyl methacrylate are hydrophobic monomer, have given material certain hydrophobicity; And hydroxy-ethyl acrylate is a hydrophilic monomer.Through hydrophobic monomer and hydrophilic monomer are controlled within the proportion of the present invention, make that the polarity of polarity and ethanol and hydrate thereof of material is suitable.The existence of alcoholic extract hydroxyl group provides material and alcohol hydrate to form the chance of hydrogen bond.These hydrogen bonds be formed with the active force that helps reinforcing material and ethanol and hydrate thereof; Make the ethanol of moving in the sorbing material and hydrate thereof no longer freely again diffusion go back; Thereby guaranteed the irreversible diffusion in sorbing material from mixed solution of ethanol and hydrate thereof, finally having reached has the purpose of selecting absorption alcohol.
For this reason, the present invention especially also relates to the purposes that above-mentioned alcohol sorbing material is used for adsorbing from the mixed solution that contains alcohol alcohol.
The said mixed solution that contains alcohol is preferably the mixed solution of alcohol and water especially.
The present invention also will provide the method for the content of alcohol in a kind of mixed solution that reduces alcohol and water simultaneously; This method is in the mixed solution of alcohol and water, to add above-mentioned alcohol sorbing material; Under 20 ℃ ~ 40 ℃ of temperature; Insulated and stirred 30min ~ 2 hour remove by filter the alcohol sorbing material at last.
The present invention also provide a kind of from the mixed solution of alcohol and water the method for purification alcohol; This method utilizes above-mentioned alcohol sorbing material from the mixed solution of alcohol and water, alcohol to be adsorbed, and through heating the alcohol that is adsorbed is parsed from the alcohol sorbing material then.
In the method for above-mentioned purification alcohol, parse, generally need be heated to 65 ℃ ~ 80 ℃ of temperature for making alcohol.
Because the enforcement of above technical scheme, the present invention compared with prior art has following advantage:
Alcohol sorbing material of the present invention can at room temperature selectively adsorb alcohol from the aqueous solution of alcohol, can be applied to the low-temperature extraction of alcohol; Can realize continuously fermenting, improve the work period of yeast; Can also reduce the number of degrees of wine in the short period of time.In addition, the preparation of alcohol sorbing material is simple, and cost is low.
The specific embodiment
Below in conjunction with specific embodiment such scheme is further specified.Should be understood that these embodiment are used to explain basic principle of the present invention, principal character and advantage, and the present invention is not limited by the scope of following examples.The implementation condition that adopts among the embodiment can be done further adjustment according to specific requirement, and not marked implementation condition is generally the condition in the normal experiment.
Embodiment 1
A kind of alcohol sorbing material; Its preparation process is following: with joining in the oxolane after butyl acrylate and 6: 4 by volume the mixed of hydroxy-ethyl acrylate, the organizator volume concentrations is 5% solution, continues in solution to add consumption again and be 0.5% initator azo-bis-isobutyl cyanide of monomer weight; With nitrogen or argon gas solution was carried out deoxygenation 30 minutes; Be warming up to 60 ℃, reacted 24 hours, promptly get.
Embodiment 2
A kind of alcohol sorbing material; Its preparation process is following: with joining in the oxolane after methyl methacrylate and 7: 3 by volume the mixed of hydroxy-ethyl acrylate, the organizator volume concentrations is 15% solution, continues in solution to add consumption again and be 0.5% initator azo-bis-isobutyl cyanide of monomer weight; With nitrogen or argon gas solution was carried out deoxygenation 30 minutes; Be warming up to 60 ℃, reacted 24 hours, promptly get.
Embodiment 3
A kind of alcohol sorbing material; Its preparation process is following: butyl acrylate and hydroxy-ethyl acrylate are joined in the oxolane after the mixed of 8:2 by volume, and the organizator volume concentrations is 30% solution, continues in solution, to add consumption again and be 0.5% initator azo-bis-isobutyl cyanide of monomer weight; With nitrogen or argon gas solution was carried out deoxygenation 30 minutes; Be warming up to 60 ℃, reacted 24 hours, promptly get.
Variable density through test wine is tested the alcohol absorption property of the alcohol sorbing material of the foregoing description 1 ~ 3, and is specific as follows:
(1), draw density-wine number of degrees curve: the density of alcohol is 0.7892g/cm under the room temperature
3, the density of water is 1g/cm
3At first prepared the wine of a plurality of different number of degrees, and in the time of 38 ℃, adopted the densitometer bottle test density of 50ml, the density of wine when the different number of degrees is as shown in table 1:
Table 1
| Wine (number of degrees) | Density (g/cm 3） |
| 2.5° | ?0.9889 |
| 5° | ?0.9854 |
| 10° | ?0.9782 |
| 12.5° | ?0.9751 |
| 15° | ?0.9716 |
| 20° | ?0.9651 |
| 25° | ?0.9583 |
| 30° | ?0.9507 |
| 35° | ?0.9422 |
| 40° | ?0.9346 |
| 45° | ?0.9223 |
According to the resulting density of last table, draw density-wine number of degrees curve.
(2), take by weighing the alcohol sorbing material of a certain amount of embodiment 1 ~ 3, join respectively in the wine of 16ml, then with seal of vessel, be placed in 38 ℃ the water bath with thermostatic control, under the magneton condition of stirring, heated 30 minutes.At last, get an amount of wine and carry out density measurement.Density measurement also is in 38 ℃ of water-baths, earlier the densitometer bottle heating that fills wine is made the temperature constant of wine in 10 minutes, weighs then.Because the weight of empty densitometer bottle is known and constant, volume also is known.Knowing under the situation of weight, calculating the density of wine.
(3), record density, from density-wine number of degrees curve that step (1) is drawn, draw the number of degrees through the alcohol after the sorbing material absorption according to step (2).
(4), the test result of embodiment 1 ~ 3 is referring to table 2.
Table 2
Above-mentioned test result shows, according to alcohol sorbing material of the present invention in the short period of time, can effectively reduce the number of degrees of wine, shows that alcohol is had extraordinary adsorption effect.
The foregoing description only is explanation technical conceive of the present invention; Its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this; Can not limit protection scope of the present invention with this; All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (10)
1. alcohol sorbing material; It is characterized in that: said alcohol sorbing material issues living Raolical polymerizable by polymerization single polymerization monomer in the effect of polymerization initiator and obtains; Cumulative volume with described polymerization single polymerization monomer is a benchmark; Said polymerization single polymerization monomer is made up of with hydroxy-ethyl acrylate monomer 20% ~ 40% Butyl Acrylate Monomer or methyl methacrylate monomer or the mixing of the two 60% ~ 80%, and the adding weight of described initator is 0.1% ~ 0.8% of said polymerization single polymerization monomer weight.
2. alcohol sorbing material according to claim 1; It is characterized in that: described Raolical polymerizable is implemented as follows: with Butyl Acrylate Monomer or methyl methacrylate monomer or the mixing of the two, and the hydroxy-ethyl acrylate monomer joins in the solvent in proportion, and the formation total volume concentration is 5 ~ 30% solution; Add polymerization initiator then; Use the inert gas deoxygenation, maintain under the initiation temperature of polymerization initiator and react, reaction finishes promptly to get said alcohol sorbing material.
3. alcohol sorbing material according to claim 2 is characterized in that: described polymerization initiator is middle temperature initator, and its initiation temperature is 30 ℃ ~ 100 ℃.
4. alcohol sorbing material according to claim 3 is characterized in that: described polymerization initiator is an azo-bis-isobutyl cyanide.
5. alcohol sorbing material according to claim 4 is characterized in that: described solvent is an oxolane, and said being reflected under 50 ~ 60 ℃ of the temperature carried out.
6. alcohol sorbing material according to claim 4 is characterized in that: the adding weight of azo-bis-isobutyl cyanide is 0.3% ~ 0.6% of said polymerization single polymerization monomer weight.
7. the described alcohol sorbing material of each claim is used for from the purposes of the mixed solution absorption alcohol that contains alcohol in the claim 1 to 6.
8. purposes according to claim 7 is characterized in that: the said mixed solution that contains alcohol is the mixed solution of alcohol and water.
9. the method for the content of alcohol in the mixed solution that reduces alcohol and water; It is characterized in that: this method is in the mixed solution of alcohol and water, to add the described alcohol sorbing material of each claim in the claim 1 to 6; Under 20 ℃ ~ 40 ℃ of temperature; Insulated and stirred 30min ~ 2 hour remove by filter said alcohol sorbing material at last.
10. the method for a purification alcohol from the mixed solution of alcohol and water; It is characterized in that: this method utilize in the claim 1 to 6 the described alcohol sorbing material of each claim from the mixed solution of alcohol and water with alcohol absorption, through heating the alcohol that is adsorbed is parsed from the alcohol sorbing material then.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014161998A1 (en) | 2013-04-05 | 2014-10-09 | D'alcante B.V. | Improved process for reducing the alcohol and/or sugar content of a beverage |
| CN107626289A (en) * | 2017-10-31 | 2018-01-26 | 北京百漾酒业科技股份有限公司 | The desorption process for regenerating and device of wine liquid impurity absorption agent |
| CN109182063A (en) * | 2018-11-09 | 2019-01-11 | 湖北工业大学 | A kind of filter medium and its filter method of high efficiency filter fen-flavor type white spirit |
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| CN1895772A (en) * | 2006-06-02 | 2007-01-17 | 郑州大学生化工程中心 | Adsorbent for dewatering alcohol |
| CN101279241A (en) * | 2007-12-28 | 2008-10-08 | 广西大学 | Adsorbing agent for gas-phase dehydration of alcohol and method of producing the same |
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Patent Citations (3)
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| CN1895772A (en) * | 2006-06-02 | 2007-01-17 | 郑州大学生化工程中心 | Adsorbent for dewatering alcohol |
| CN101279241A (en) * | 2007-12-28 | 2008-10-08 | 广西大学 | Adsorbing agent for gas-phase dehydration of alcohol and method of producing the same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014161998A1 (en) | 2013-04-05 | 2014-10-09 | D'alcante B.V. | Improved process for reducing the alcohol and/or sugar content of a beverage |
| CN107626289A (en) * | 2017-10-31 | 2018-01-26 | 北京百漾酒业科技股份有限公司 | The desorption process for regenerating and device of wine liquid impurity absorption agent |
| CN109182063A (en) * | 2018-11-09 | 2019-01-11 | 湖北工业大学 | A kind of filter medium and its filter method of high efficiency filter fen-flavor type white spirit |
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Effective date of registration: 20160128 Address after: 361022, building 903, unit 2, building 2052, 904 West Weng Road, Haicang District, Fujian, Xiamen Patentee after: XIAMEN JIAYAN POLYMER MATERIALS CO., LTD. Address before: 215600, room 205, building A, 1 Cathay Pacific Road, Zhangjiagang, Jiangsu, Suzhou Patentee before: Suzhou Easent Biological Technology Co., Ltd. |