CN101024846B - Method and apparatus for preparing fuel alcohol by fermented liquid steam phase adsorption separation - Google Patents
Method and apparatus for preparing fuel alcohol by fermented liquid steam phase adsorption separation Download PDFInfo
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- CN101024846B CN101024846B CN2006101472522A CN200610147252A CN101024846B CN 101024846 B CN101024846 B CN 101024846B CN 2006101472522 A CN2006101472522 A CN 2006101472522A CN 200610147252 A CN200610147252 A CN 200610147252A CN 101024846 B CN101024846 B CN 101024846B
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Abstract
The invention belongs to the chemical technical field, concretely relating to a method and device for preparing fuel alcohol by fermented liquor steam-phase absorption separation, comprising the steps of: making 1%-30% thin alcohol steam pass through hydrophobic zeolite sorbent bed so that the alcohol is aborbed by the hydrophobic zeolite and the water is removed; guiding part of fuel alcohol steam into the sorbent bed to substitute for thin alcohol steam in the dead spaces between sorbent particles and between zeolite crystal grains in sorbent, and making intermediate blowing; the saturated sorbent is desorbed with CO2 or other gas, and the desorbed alcohol concentration is higher than 98% alcohol steam, drying by drier and obtaining the fuel alcohol. As compared with the traditional multi-action rectifying process, it saves energy by above 50%. And the method can implement continuous production, having features of simple equipment, less occupied land, high efficiency and low energy consumption. And it has a wide application prospect in absorption separation and recovery of small molecular organic solvent water solution.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of preparation method and device of fuel alcohol.
Background technology
Reserves is limited, is the non-renewable energy.International Crude Oil continues to rise violently, and national economy sustainable and healthy development, national security are constituted serious challenge.Opening up new renewable energy source, is the demand of national sustainable development strategy, also is the task of top priority.
Biological resources-plant (or animal) is sustainable generation, can be for the energy that continues to consume.The country of some petroleum resources shortage such as Brazil have successfully developed already with corn and sugarcane and have pressed sugared tankage fermentation, produce the technology of fuel with alcohol.At present, the automobile power of this state about 50% derives from fuel alcohol.
China has also developed the engineering of corn and grain fermentative production fuel alcohol before and after 2000.At present northeastward, the yearly capacity of the fuel alcohol on ground such as Henan has reached few hundred thousand tonnes of.Because the production cost height is had under the support of government finance subsidy, some places begin to promote fuel alcohol and are used for automobile power.
Therefore, with non-grain plant fermentation, the complex art of high efficiency separation, low cost production fuel alcohol is the core and the key of development bioenergy.
Plant (comprising grain) fermentation can only be obtained the Diluted Alcohol of content 8～10%.Usually, fuel will just can make by three distillations with alcohol (moisture 0.2～0.8%): 1, and simple distillation.The fermentation liquid distillation of the spirituosity 8～10% that produces by fermenting obtains the alcohol of 30-50% left and right sides concentration; 2, rectifying.Efficient distil process is concentrated into the concentration of 30%-50% the constant boiling point alcohol of 95% left and right sides concentration; 3, azeotropic distillation.Add entrainment agent (as organism such as benzene) destruction constant boiling point and distill these No. three distillation plant complexity, energy consumption height once more.Though, adopt novel process such as multitower multi-effect distilling and equipment can significantly reduce production energy consumption, but still quite high.Its each stage energy consumption calculation following (calculating) with the steam consumption quantity of producing 1 ton of raw spirit:
(mash-95% alcohol): 5.6 tons
Azeotropic distillation (95%-fuel alcohol): 2.22 tons
Add up to: 7.82 tons
General coal firing boiler, 1 ton of coal can produce 7 tons of steam.Produce 1 ton of fuel alcohol, need coal-fired 1.12 tons.Calorific value by 1 gram standard coal is 5,000 kilocalories of (～20.93KJ/g) calculating, calorific values 23.44 * 10 of 1.12 tons of standard coals
6KJ.
Calculate the calorific value 23.44 * 10 of this boiler thus for the used fuel of 1 ton of alcohol of production
6KJ, with the calorific value 29.71 * 10 of 1 ton of alcohol producing
6KJ compares, and has only increased by 6.27 * 10
6KJ, the amplitude of increase is 26.8%.As consider the energy that fermenting process consumes, the power consumption that tankage are handled and environmental protection is turned round, the energy consumption of raw material and fuel transport etc., we can say, producing fuel alcohol with multiple-effect distillation and just a kind of energy (as coal) is converted into the another kind of energy (fuel alcohol), is non-remunerative from the energy viewpoint.And the energy that actual biological product (as corn) should produce is steamed the energy counteracting that slide method separating alcohol and water are consumed by the Production of Fuel Ethanol process with multiple-effect.Thus, must create the energy-efficient novel method of fermentation alcohol alcohol/water sepn.
Attempt to substitute traditional rectifying concentrated broth to reduce the existing some bibliographical informations of the energy consumption of producing fuel alcohol with the method for fractionation by adsorption.Utilize 3A (KA) zeolite molecular sieve to carry out alcohol/water transformation fractionation by adsorption and can effectively reduce energy consumption (Adsorption-Journal of the InternationalAdsorption Society 8 (3) by the azeotropic ethanol distillation of the 95% concentration fuel alcohol to＞99.2%; LatinAmerican Applied Research 31 (4): 333-357, OCT 2001); American Institute of Chemical Engineers, National Meeting, 1987,27p).With high silica ZSM-5 or silicon zeolite (Silicalite-1) low-concentration ethanol (2%～4%) is carried through liquid phase adsorption separation and densely certain energy-saving effect (J.ofChemical Technology and Biotechnology also to be arranged to 35%, V31, n12, Dec, 1981, p732-736; Petrochemical complex 1994,23 (6), 356-8).But aforesaid method just has part energy efficient effect in fermented liquid (containing ethanol 8-10%) the concentrated production fuel alcohol part stage, and is limited to reducing total production energy consumption effect.A kind of novel method provided by the invention, adopt hydrophobic silicalite (Silicalite-1) sorbent material or high silica ZSM-5 molecular sieve with low-concentration ethanol (1%～30%), directly carry through the vapor phase fractionation by adsorption dense to fuel alcohol, compare with traditional distillating method, energy-conservation more than 30%.
Summary of the invention
The objective of the invention is to propose a kind of consuming little energy, separation efficiency high prepare the method and apparatus of fuel alcohol from fermented liquid.
The method for preparing the alcohol that burns that the present invention proposes, concrete steps are as follows:
(1) at first be that the fermenting raw materials liquid (mash) of 1%-10% obtains the alcohol steam that ethanol content is 1%-30% (its plateau temperature is 90-100 ℃, sees accompanying drawing 1 (B)) through simple distillation with ethanol content;
(2) after the alcohol steam that step (1) is obtained is heated to 100-110 ℃, feed first adsorption bed, carry out adsorption treatment, wherein, first adsorption bed uses the hydrophobic silex sorbent material, the inlet amount of alcohol steam is 80-250g ethanol/h, and the dynamic adsorption amount of sorbent material is 20-30 gram ethanol/kilogram sorbent material, adsorption time 3-15 minute; The by product carbonic acid gas that produces with fermenting process is a desorbing agent, perhaps uses nitrogen (N
2), hydrogen (H
2) wait gas to make desorbing agent, the ethanol content that hydrophobic silicon zeolite adsorbent is adsorbed is the alcohol in high concentration desorption of 91%-95%, desorption time is 6-15 minute, normal pressure; Here desorption temperature is identical with adsorption temp;
(3) alcohol in high concentration steam and the desorption gas that step (2) is obtained together enters second adsorption bed, and to remove a spot of moisture in the alcohol, second adsorption bed uses the 3A adsorbent of molecular sieve, and obtaining ethanol content at last is the burning alcohol of 99.2%-99.9%.
It is the main factor of rectifying energy consumption that alcohol concn is increased to 88% by 50%.Because in this scope, in liquid phase and the vapor phase alcohol, relatively near (seeing Fig. 1 (A)), rectification efficiency is lower for amount of moisture.
Therefore, the Diluted Alcohol with concentration 1%-30% be concentrated into the azeotropic alcohol stage adopt the vapor phase absorption/desorption separation of hydrophobic adsorbent, in conjunction with this new economic benefits and social benefits separation principle of 3A type molecular sieve vapor phase absorption/dehydration, production energy consumption is significantly reduced.
The sorbent material that first adsorption bed uses among the present invention is hydrophobic silicon zeolite adsorbent, and its chemical ingredients is SiO
2, heat and chemical stability are high, and work-ing life is very long, (seeing Chinese invention patent ZL 94 1 12035.X).It is to water saturation loading capacity＜1%, under differing temps, to different and different according to adsorption temp and vapour pressure of the Static Adsorption capacity of alcohol steam, (sees accompanying drawing 2 (A)) in 2～12% scopes.This zeolite is faint physisorption to the absorption of alcohol, and its heat of adsorption is 0.82KJ/g only, far below the vaporization heat (2.26KJ/g) of water, also be lower than alcoholic acid vaporization heat (0.90KJ/g) (petrochemical complex 1994,23 (6), 356-8).Therefore the alcohol absorption/desorption rate that is adsorbed by this hydrophobic adsorbent is very fast, and heat effect is little, and energy consumption is very low.
The present invention uses aperture that the energy-conservation basic reason of hydrophobic silicon zeolite adsorbent adsorption separation process is that this separation is based on molecular sieve to the weak interaction between crystal field/adsorption molecule on the bore surface huge in the type of the selecting adsorption selectivity effect of molecule and the adsorbent solids, to split between water and the alcohol with the mutual association of hydrogen bond.This crystal field splits required energy to associating adsorption molecule and distills the heat energy that the associated molecule of carrying out splits consumption well below simple dependence.
Based on above-mentioned principle process flow system figure of the present invention as shown in Figure 3, appended separating technology unit only shows single hydrophobic adsorption bed and 3A zeolite adsorption bed among the figure.With fermenting raw materials liquid (mash, contain ethanol 1-10%) to obtain ethanol content through the simple distillation process be steam (90～100 ℃ of its equilibrium temperatures of 1%～30%, see Fig. 1 (B)), after being heated to 100～110 ℃, feed first adsorption bed (interior dress hydrophobic silicon zeolite adsorbent) and carry out adsorption operations.Alcohol in the steam is adsorbed by hydrophobic adsorbent, and water is discharged from.The adsorption operations time is 3-15 minute.Later operation is all carried out in 100～110 ℃ vapor phase.Because of heat of adsorption and desorptive activation can be very low, need the heat that replenishes seldom.By product carbonic acid gas with the fermenting process association is alcohol in high concentration (contain ethanol 91～95%) desorption of desorbing agent with hydrophobic silicon zeolite adsorbent absorption.The desorption manipulation time is 6～15 minutes (seeing Fig. 2 (B)).The alcohol steam of this high density and carbonic acid gas together enter second adsorption bed-3A sieve adsorpting bed and remove a spot of water in the alcohol, can obtain alcohol concn and be higher than 99.2% fuel alcohol.Molecular dimension is not discharged from adsorption bed, recyclable recycling by the 3A molecular sieve adsorption greater than the carbonic acid gas of 3A molecular sieve bore diameter.The 3A sorbent material that planar water reaches capacity, available pressure swing regeneration (PSR) technology, the negative pressure that produces with vacuum pump are the power desorption and regeneration that reduces pressure, and make it recover dehydrating function.Look the different of absorption and desorption time, hydrophobic adsorption bed (first adsorption bed) can adopt two or three to unite operation in turn.As when the first hydrophobic adsorption bed desorption begins, the second hydrophobic adsorption bed (Fig. 3 is not shown) carries out adsorption operations, switches to desorption manipulation after finishing absorption.Simultaneously, the 3rd hydrophobic adsorption bed (Fig. 3 is not shown) enters adsorption operations.With this order, 3 co-operations, a whole set of adsorption unit can be realized under computer control continuously and automatic production.Production equipment is in (100～110 ℃) operation down.Equally, A type zeolite adsorbent dehydration adsorption bed (second adsorption bed) also can adopt 2 or 3 through transports (ratio on absorption/desorption time is decided), can adopt sophisticated pressure swing regeneration (PSR) technology to realize continuous adsorption and desorption.The 3A zeolite adsorbents does not adsorb alcohol and CO
2, and the water saturation loading capacity is 18～22%.Therefore, with its from hydrophobic adsorption bed, obtain neutral spirits steam remove in contained 5%～8% water, the 3A zeolite loadings of adsorption bed is not more than the hydrophobic silicalite adsorption bed.
Energy consumption calculation
The alcoholic acid heat of adsorption is 49.4KJ/mol (1.07KJ/g) on the hydrophobic silicalite; Desorptive activation energy 19.4KJ/mol (0.82KJ/g) adds up to 1.89KJ/g.Produce the energy consumption 1.89 * 10 of one ton of fuel alcohol with this method
6KJ, the vaporization heat 2.26KJ/g calculating with water needs 0.836 ton of steam.Heat by the Diluted Alcohol process consumption of fermented liquid (1～10% alcohol) simple distillation to 30% is approximately 1/3 of multi-effect distilling total energy consumption, i.e. 5.6/3=1.87 ton steam.The power consumption of ethanol/water fractionation by adsorption is 0.863 ton on the first step hydrophobic silicalite; 2.22 tons of second stage A zeolite dehydration fractionation by adsorption (its energy consumption and azeotropic distillation remain basically stable) power consumptions add up to 4.95 tons.The 4.95/7.86=63.0% that is equivalent to multiple-effect distillation energy-conservationly reaches 37%.
According to above-mentioned technical process, the device of preparation fuel alcohol of the present invention is constructed as follows:
It by a fermentor tank 1, slightly steam tower 2, hydrophobic adsorption bed (first adsorption bed) 3,3A sieve adsorpting bed (second adsorption bed) 4, first vapour/liquid/gas separator 5, vacuum pump 6, condenser 8, second vapour/liquid/gas separator 7 and well heater 9 and form through pipe connection.See shown in the accompanying drawing 3.Wherein, the ripe mash that fermentor tank 1 obtains enters thick steaming tower 2, the CO that fermentor tank 1 comes out through pipeline
2As desorbing agent, feed hydrophobic adsorption bed 3 by pipeline; The ethyl alcohol content that thick steaming tower 2 comes out is that the following process of 0-30% well heater 9 enters hydrophobic adsorption bed 3; Sorbent material in the hydrophobic adsorption bed 3 is with the alcohol occlusion in the mixing steam, and water vapor then is cooled to water by this adsorption bed and discharges in condenser 8.Desorption gas CO
2The CO that the alcohol desorption that hydrophobic adsorbent is adsorbed by this adsorption bed comes out to form
2The mixing steam that contains less water with neutral spirits enters 3A sieve adsorpting bed 4 by pipeline, and moisture wherein is by the 3A molecular sieve adsorption, and has removed the CO of moisture
2Cool off a little with the mixing steam of alcohol and to enter first vapour/liquid/gas separator 5, with CO
2Separate with alcohol, obtain fuel alcohol.Adsorbing water saturated 3A molecular sieve regenerates to recover dewatering by connected vacuum pump 6 decompression dehydrations.Water vapor in vacuum pump 6 expellant gas cools off a little after in the 2nd vapour/liquid/gas separator 7 water is discharged.
Among the present invention, the hydrophobic adsorbent that hydrophobic adsorption bed 3 uses is attached dose of hydrophobic silicalite.The sorbent material that the 3A sieve adsorpting bed uses is the 3A molecular sieve.
Among the present invention, described hydrophobic adsorption bed 3 can adopt 2 or 3 interlock forms.Equally, 3A sieve adsorpting bed 4 also can adopt 2 or 3 interlock modes.
Description of drawings
Fig. 1 is alcohol-water system liquid/vapour phase state diagram.Wherein (A) is alcohol-water system balancing figure, (B) is the graph of a relation of ethanol content and boiling point in solution and the steam.
Fig. 2 is adsorption isothermal line and the desorption rate curve of ethanol on hydrophobic silicalite under the differing temps.Wherein, (A) being adsorption isothermal line, (B) is the desorption rate curve.
Fig. 3 is device (flow process) diagram of economic benefits and social benefits fractionation by adsorption preparation burning alcohol.Number in the figure: 1 is fermentor tank, and 2 is the thick tower that steams, and 3 is hydrophobic adsorption bed, and 4 is the 3A sieve adsorpting bed, and 5 is first vapour/liquid/gas separator, and 6 is vacuum pump, and 7 is the 2nd vapour/liquid/gas separator, and 8 is condenser, and 9 is well heater.
Embodiment
Further specify the present invention below by embodiment, its condition and the results are shown in following table:
*Adsorption bed filling hydrophobic adsorbent (hydrophobic silicalite) 1000 grams;
*(gram ethanol/kilogram sorbent material);
* *Desorption gas pressure is normal pressure.
Claims (4)
1. a fermented liquid vapor phase is adsorbed the method for preparing fuel alcohol, it is characterized in that concrete steps are as follows:
(1) at first be that the fermenting raw materials liquid of 1%-10% obtains the alcohol steam that ethanol content is 1%-30% through simple distillation with ethanol content;
(2) after the alcohol steam that obtains of step (1) is heated to 100-110 ℃, feed first adsorption bed, carry out adsorption treatment; Wherein, first adsorption bed uses hydrophobic silicon zeolite adsorbent, and the inlet amount of alcohol steam is 80-250g ethanol/h, and the dynamic adsorption amount of sorbent material is 20-30 gram ethanol/kilogram sorbent material, adsorption time 3-15 minute; The by product carbonic acid gas that produces with fermenting process is a desorbing agent, perhaps use nitrogen, hydrogen to make desorbing agent, with the ethanol content of hydrophobic silicon zeolite adsorbent absorption is alcohol in high concentration desorption under normal pressure of 91%-95%, and desorption time is 6-15 minute, and desorption temperature is identical with adsorption temp;
(3) alcohol in high concentration steam and the desorption gas that step (2) is obtained together enters second adsorption bed, and to remove a spot of moisture in the alcohol, second adsorption bed uses the 3A adsorbent of molecular sieve, obtains the fuel alcohol that ethanol content is 99.2%-99.9% at last.
2. the device of fermented liquid vapor phase absorption preparation fuel alcohol, it is characterized in that it by a fermentor tank (1), slightly steam tower (2), hydrophobic adsorption bed (3), 3A sieve adsorpting bed (4), first vapour/liquid/gas separator (5), vacuum pump (6), condenser (8), second vapour/liquid/gas separator (7) and well heater (9) and form through pipe connection; Wherein, the ripe mash that fermentor tank (1) obtains enters thick steaming tower (2) through pipeline, the CO that fermentor tank (1) comes out
2Feed hydrophobic adsorption bed (3) as desorbing agent by pipeline; The alcohol steam that thick steaming tower (2) comes out enters hydrophobic adsorption bed (3) through well heater (9); Water vapor in the hydrophobic adsorption bed (3) enters condenser (8), CO by pipeline
2Enter 3A sieve adsorpting bed (4) with the neutral spirits mixing steam by pipeline, removed the CO of moisture
2Enter first vapour/liquid/gas separator (5) with the mixing steam of alcohol by pipeline, with CO
2Separate with alcohol, obtain fuel alcohol; Water vapor in vacuum pump (6) expellant gas enters the 2nd vapour/liquid/gas separator (7) by pipeline;
The hydrophobic adsorbent that hydrophobic adsorption bed (3) uses is the 3A molecular sieve as attached dose of hydrophobic silicalite, the sorbent material that the 3A sieve adsorpting bed uses.
3. the device of fermented liquid vapor phase absorption preparation fuel alcohol according to claim 2 is characterized in that described hydrophobic adsorption bed (3) adopts 2 or 3 interlock modes.
4. the device of fermented liquid vapor phase absorption preparation fuel alcohol according to claim 2 is characterized in that described 3A sieve adsorpting bed (4) adopts 2 or 3 interlock modes.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| IT1396424B1 (en) * | 2009-06-05 | 2012-11-23 | Hf Europ Srl | FOOD PRODUCTS INCLUDING ZEOLITI |
| PL2333092T3 (en) | 2009-12-08 | 2013-07-31 | Sued Chemie Ip Gmbh & Co Kg | Method for the recovery of ethanol during fermentation |
| CN102351646B (en) * | 2011-09-16 | 2014-05-21 | 南京工业大学 | Method for separating ethanol from fermentation liquor |
| CN104877714B (en) * | 2015-05-25 | 2016-06-08 | 李明阳 | A kind of biological combustion-supporting material and its preparation method and application |
| CN106237652B (en) * | 2015-06-11 | 2019-09-20 | 上海复榆新材料科技有限公司 | Method is selectively adsorbing and separating using molecular sieve as adsorbent |
| CN112169752B (en) * | 2020-10-15 | 2023-03-17 | 西安近代化学研究所 | Adsorbent for separating biological method to synthesize 1,2,4-butanetriol, preparation and separation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105906A (en) * | 1994-01-29 | 1995-08-02 | 复旦大学 | Hydrophobic silicon zeolite adsorbent without cohesive agent and its preparation |
| CN1403579A (en) * | 2001-09-05 | 2003-03-19 | 中国科学院过程工程研究所 | Alcohol preparing airlift fermentation and separation coupling technological process and special equipment |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105906A (en) * | 1994-01-29 | 1995-08-02 | 复旦大学 | Hydrophobic silicon zeolite adsorbent without cohesive agent and its preparation |
| CN1403579A (en) * | 2001-09-05 | 2003-03-19 | 中国科学院过程工程研究所 | Alcohol preparing airlift fermentation and separation coupling technological process and special equipment |
Non-Patent Citations (2)
| Title |
|---|
| 王秀道 等.分子筛吸附法生产无水酒精.酿酒科技 第1期（总第109期）.2002,(第1期（总第109期）),24-26. |
| 王秀道等.分子筛吸附法生产无水酒精.酿酒科技 第1期(总第109期).2002,(第1期(总第109期)),24-26. * |
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