CN101041835A - Method for preparing ethyl alcohol by cellulose waste double thin acid hydrolysis - Google Patents
Method for preparing ethyl alcohol by cellulose waste double thin acid hydrolysis Download PDFInfo
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- CN101041835A CN101041835A CNA2007100400589A CN200710040058A CN101041835A CN 101041835 A CN101041835 A CN 101041835A CN A2007100400589 A CNA2007100400589 A CN A2007100400589A CN 200710040058 A CN200710040058 A CN 200710040058A CN 101041835 A CN101041835 A CN 101041835A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a preparing method of flue alcohol with cellulose waste material double diluted acid hydrolysis, which comprises the following steps: choosing cellulose waste material as raw material; choosing dilute hydrochloric acid as accelerant; hydrolyzing the cellulose waste material under the craft condition of proper reacting temperature and acid density; producing monosaccharide with deacidizing property; yeasting and finestilling; getting the flue alcohol; utilizing active sludge method to dispose the waste liquid; using as water to produce complex acid. This method can cycle utilize the water, which can protect environment and decrease the cost.
Description
Technical field
The present invention relates to a kind of preparation method of alcohol fuel, relating to a kind of specifically is the method for raw material through dilute acid hydrolysis, alcohol prepared by fermenting with the cellulose castoff.
Background technology
Energy industry is the basis of national economy, and is all very important to society, Economic development and raising people's living standard.Along with human living standard's raising, people are more and more higher to the degree of dependence of the energy, but because the finiteness of non-renewable and its reserves of fossil oil, fossil energy is exhausted day by day, and ecocrisis is obvious day by day.Now, seek the renewable energy source little, caused showing great attention to of the whole world with the development of new energy, particularly environmental pollution.
Biomass energy is a kind of important renewable energy in the future source of energy field, as unique renewable energy source that is converted into liquid fuel, comes into one's own just day by day.Biomass typically refer to terrestrial plant (timber, yule logs, stalk etc.) and waterplant, are a kind of stable renewable energy source resources, and the source is abundant.China is large agricultural country, and large number of biological matter generation of waste materials is arranged every year.Only China's agricultural crop straw output is about 700,000,000 tons every year, and the stock number that can be used as the energy is hundred million tons of 2.8-3.5; The year rational exploitation amount of yule logs is about 1.58 hundred million tons, also has a large amount of waterplant in addition.But these resources are not fully utilized so far, and often because of the on-site incineration contaminate environment, this has become nationwide problem.Biomass have aboundresources, renewable, eco-friendly characteristics, and can realize clean CO
2Zero release, research, the development and utilization of biomass energy caused domestic and international common concern.China's Oil resource-constrained on the other hand, the demand of oil product but in continuous increase, is produced liquid fuel with the cellulose castoff hydrolysed ferment---ethanol is one of method of effectively utilizing biomass energy, and China is had bigger realistic meaning.The development and use cellulose castoff is produced alcohol fuel to setting up continuable energy resource system, solves human energy dilemma and the ecocrisis that is faced, and promoting national economic development and preserving the ecological environment has great importance.
Be that the principle that raw material is produced alcohol fuel obtains reductive monosaccharide to cellulose castoff through hydrolysis exactly with the cellulose castoff, as wood sugar, glucose etc., by fermentation, can obtain alcohol fuel after the rectifying with reductive monosaccharide.Wherein, cellulose castoff prepares reductive monosaccharide and cycling utilization of wastewater is two committed steps through hydrolysis, because they will directly influence the quality of alcohol fuel, the economy of process and the commercial application of technology.At present the method for producing alcohol fuel for the raw material hydrolysis with the cellulose castoff can be divided into two big classes: enzyme hydrolysis method and acid-hydrolysis method, and it is as follows to show division:
1. enzyme hydrolysis method
Enzymic hydrolysis is that the katalysis by the cellulase of microorganisms is a reductive monosaccharide with cellulose hydrolysis, and fermenting makes alcohol fuel again.This process energy consumption is low, and only generates by product seldom, but this arts demand carries out pre-treatment to raw material, and the hydrolysis cycle is long, the production cost height of high active enzyme, thus cause this technological operation expense too high.
2. acid-hydrolysis method
Acid hydrolysis comprises two kinds of concentrated acid hydrolysis and dilute acid hydrolysis, and used catalyzer is mainly hydrochloric acid and two kinds of mineral acids of sulfuric acid.
The concentrated acid hydrolysis
The concentrated acid hydrolysis is a catalyzer with the concentrated hydrochloric acid or the vitriol oil mainly, under 80-100 ℃, condition of normal pressure, be hydrolyzed, best acid solution and solid weight ratio are 1.25: 1 (is benchmark with bright sulfur acid), reaction times is depended on the content of Mierocrystalline cellulose and hemicellulose in hydrolysis temperature and the raw material, changes between 40-480 minute.The advantage of concentrated acid hydrolysis is the productive rate height (can reach more than 90%) of sugar, but required time is long, and acid must be reclaimed.
Dilute acid hydrolysis
Hydrolysis is to be catalyzer with dilute hydrochloric acid or dilute sulphuric acid, carries out at a certain temperature.In order to improve the yield of monose, adopt the hydrolysis of two-part percolation process, this technological advantage is to have improved monose yield and concentration, has reduced the progressive of monose and has decomposed.
In sum, dilute acid hydrolysis is considered to present stage and can realizes one of technology of industrialization.Disclosed dilute acid hydrolysis technology is to use dilute hydrochloric acid or dilute sulphuric acid as catalyzer separately, under the identical situation of acid concentration, hydrolysis temperature is lower when using dilute hydrochloric acid as catalyzer, with the dilute sulphuric acid be catalyzer then hydrolysis temperature is higher, but if in when being catalyzer with dilute hydrochloric acid and after hydrolyzed solution in a large amount of CaCl will be arranged
2This had not only made the waste water can't reuse but also bring great difficulty to discharge of wastewater, had also increased the production cost of whole technological process.
Summary of the invention
The technical issues that need to address of the present invention are the methods that disclose a kind of cellulose castoff dilute acid hydrolysis ethanol production, to solve high and waste water recycling or emission problem of energy consumption in the existing dilute acid hydrolysis technology.
Design of the present invention:
Be degraded to the process of glucose and wood sugar under the katalysis of Mierocrystalline cellulose and hemicellulose hydrogen ion (actual is oxonium ion) in water just of cellulose castoff dilute acid hydrolysis process, this technology is more clearly on principle, but need to reduce process cost, could promote the industrialized development of this technology.Reduce process cost mainly on three links: improve monosaccharide concentration, reduce hydrolysis energy consumption and discharge costs and waste water recycling.Doing a lot of work, the combined method of having developed percolation process, two-stage method and hydrolyzed solution partial recycle process and several method being combined aspect the raising monosaccharide concentration at present.When improving the reduction monosaccharide concentration if hydrolysis reaction is carried out under lower temperature, reduce the hydrolysis energy consumption, and most of waste water recycling can be reduced the waste water cost can reduce consumption to water again, thereby reduction cellulose castoff that just can be bigger is produced the alcohol fuel process cost.
The present invention's imagination adopts dilute hydrochloric acid as catalyzer when hydrolysis reaction.
The contriver finds, compare dilute sulphuric acid, with dilute hydrochloric acid is that catalyzer can obtain corresponding reductive monosaccharide under lower temperature, as acid concentration is 1% o'clock, dilute hydrochloric acid is the wood sugar of catalyzer at 100-130 ℃ of product, obtain glucose at 130-170 ℃, dilute sulphuric acid is that catalyzer makes wood sugar and glucose respectively when 140-170 ℃ and 190-220 ℃, with be that catalyzer is compared and used dilute sulphuric acid to be catalyzer with dilute hydrochloric acid, requirement to boiler and hydrolysis kettle operating pressure has improved, and has significantly increased the energy consumption of hydrolytic process simultaneously.
Method of the present invention comprises the steps:
(1) the cellulose castoff raw material is added second hydrolysis reactor and the 3rd hydrolysis reactor, second hydrolysis reactor is heated to 100-130 ℃, with temperature is that 100～130 ℃ weight concentration is that the aqueous hydrochloric acid of 0.05-5% pumps into second hydrolysis reactor, reacted 1～60 minute, this time hydrolyzed solution is bled off as waste water, obtain Mierocrystalline cellulose and xylogen;
(2) again second hydrolysis reactor is heated to 130～170 ℃, with temperature is that 130～170 ℃ weight concentration is that the aqueous hydrochloric acid of 0.05-5% pumps in second hydrolysis reactor, reacted 1～60 minute, then the hydrolyzed solution product in second hydrolysis reactor is put into the 3rd hydrolysis reactor that the cellulose castoff raw material is housed, 100-130 ℃ of reaction 1～60 minute, obtain hydrolysis prods, sugared concentration is 4～12wt%;
The material of remnants in the 3rd hydrolysis reactor is the Mierocrystalline cellulose and the xylogen that can be used in second hydrolysis reactor;
Then the residue in second hydrolysis reactor is discharged, new cellulose castoff raw material is added in second hydrolysis reactor, continue the process of step (2), can obtain hydrolysis prods continuously;
The 3-15 that said aqueous hydrochloric acid add-on is the cellulose castoff raw material weight doubly;
Said cellulose castoff comprises agricultural wastes, as: stalk, shell, fruit stone, the waste of agricultural byproducts such as corn cob; Forestry waste, as: fuel wood, fallen leaves, bark, tree root and forestry processing waste; Waterplant, as: algae, duckweed, Herba Eichhorniae, jacinthe etc.; Energy crop is as: oil crops be rich in the plant of hydrocarbon polymer and other growth of biomass;
Cellulose castoff preferably is crushed to the particle less than 2cm;
According to preferable methods of the present invention, after reaction finishes, be incorporated as the 0.5-4 water washing hydrolytic residue doubly of raw material weight to the hydrolysis reactor after pyroreaction, collect the hydrolysis water of productive use that water lotion participates in the cellulose castoff raw material;
(3) unslaked lime is added step (2) gained hydrolysis prods, control pH is 3.5-6.0, static 3-12 hour, collect supernatant liquor and send into fermentor tank, add zymocyte liquid in fermentor tank, the add-on of zymocyte liquid is the 4-15% of hydrolysis prods volume, at 28-40 ℃ of bottom fermentation 24-56h, obtain tunning, wherein, the alcoholic acid volumetric concentration is 2～4.8%;
Bacterial classification in the said zymocyte liquid is selected from the wood chip yeast after the domestication and manages the composite bacteria of two kinds of bacterium of capsule yeast;
Described wood chip barms is managed the product that the capsule yeast adopts Chinese microbial preservation center to provide available from the Shanghai City Industry Wei Biological Research Institute;
The acclimation method of used bacterial classification comprises the steps:
A with two kinds of bacterial classifications respectively in nutrient solution separately, 22-30 ℃ of breeding 24-48h down;
The saccharomycetic nutrient solution of wood chip is the wort of 2 degree;
The component and the content of pipe capsule zymic nutrient solution are as follows:
1000 milliliters of malt extract 3 grams, glucose 10 grams, yeast extract 3 grams, peptone 5 grams, agar 20 grams, water;
B gets the hydrolyzed solution of step (2), and it is 4.0 that adding unslaked lime is neutralized to pH, mixes (1: 1, volume ratio) with the worts of 2 degree, and two kinds of bacterial classifications of step breeding are bred 24-56h in the adding under 22-30 ℃ condition.Wherein, the volume percent of two kinds of bacterial classifications is 4-15%, and the wood chip yeast accounts for 60%, pipe capsule yeast accounts for 40%;
The bacterial classification that c takes out the b breeding is put in the wort of 2 degree, breeds 24-48h down for 22-30 ℃;
D increases the volume percent of hydrolyzed solution with 10%, other condition constant repetition b and c are hydrolyzed liquid fully to wort and substitute.
(4) with the acquisition tunning of step (3), adopt conventional rectificating method, so Kaitian. the alcohol distillation technology. Beijing: light industry press, 1990 (first version) document disclosed method, after rectifying tower 5 rectifying, the alcoholic acid volume percent can reach 85-95%.Further can make dehydrated alcohol;
According to preferable methods of the present invention, also comprise:
(5) will separate the alcoholic acid fermented waste fluid, adopt the supernatant after conventional anaerobic and aerobic are handled to pump into the complex acid groove, add sulfuric acid and carry out complex acid, the mole number of the calcium ion in vitriolic mole number and the fermented waste fluid equates, generate calcium sulfate precipitation and hydrochloric acid behind the complex acid, if the acid concentration of solution does not reach preset value, replenish behind the adding sulfuric acid with hydrochloric acid, the calcium sulfate precipitation thing that generates behind the complex acid is used for material of construction, and what play katalysis is hydrochloric acid.
The method that the present invention utilizes the double thin acid hydrolysis cellulose castoff to produce alcohol fuel is compared with the method that present biomass by hydrolyzation is produced alcohol fuel, the waste water that not only reduced energy consumption but also reuse, has reduced the discharge of wastewater expense, has alleviated the dependency to water resources.Protected environment; reduced cellulose castoff hydrolysis cost; improved the economy that the alcohol fuel process is produced in the cellulose castoff hydrolysis; promoted the industrialized development that alcohol fuel is produced in the cellulose castoff hydrolysis, had great importance setting up continuable energy resource system and preserving the ecological environment.
Description of drawings
Fig. 1 cellulose castoff hydrolysis schematic flow sheet.
Embodiment
The invention will be further described below by embodiment, but do not influence protection scope of the present invention:
Embodiment 1
Adopt flow process shown in Figure 1.
(1) the maize straw raw material of 150g granularity less than 1cm added in second and the 3rd liang of hydrolysis reactor, with the high pressure saturated steam hydrolysis reactor 2 is heated to 100 ℃, with temperature is that 100 ℃ weight concentration is that 1% aqueous hydrochloric acid pumps into hydrolysis reactor 2, in 1 minute reaction times, this time hydrolyzed solution is bled off as waste water;
(2) second hydrolysis reactor 2 is heated to 160 ℃, with the 1200ml temperature is that 160 ℃ weight concentration is that 1% aqueous hydrochloric acid pumps in the hydrolysis reactor 2, reacted 1 minute, then the hydrolyzed solution product in the hydrolysis reactor 2 is put into the 3rd hydrolysis reactor 3,1 minute 100 ℃ of reaction times, obtain hydrolysis prods 1200ml, sugared concentration is 6.5wt%;
The material of remnants in the hydrolysis reactor 3 is and is used for hydrolysis reactor 2 Mierocrystalline celluloses and xylogen;
After reaction finishes, be incorporated as 2 times water washing hydrolytic residue of raw material weight, collect the hydrolysis water that water lotion participates in following batch of cellulose castoff raw material to hydrolysis reactor 3;
Water is neutrality with the washing of the hydrolytic residue in the reactor 2 in batches, and washings is as next bath water and additional complex acid water.
The hydrolysis prods that embodiment 1 is produced, adopting the unslaked lime pH value that neutralizes is 4.0, static 3h pumps into supernatant liquor in the fermentor tank 4.
Bacterial classification in the zymocyte liquid is selected from the wood chip yeast after the domestication and manages the composite bacteria of two kinds of bacterium of capsule yeast;
The acclimation method of used bacterial classification comprises the steps:
A with two kinds of bacterial classifications respectively in nutrient solution separately, 26 ℃ of breeding 36h down;
The saccharomycetic nutrient solution of wood chip is the wort of 2 degree;
The component and the content of pipe capsule zymic nutrient solution are as follows:
1000 milliliters of malt extract 3 grams, glucose 10 grams, yeast extract 3 grams, peptone 5 grams, agar 20 grams, water;
B gets the hydrolyzed solution of step (2), and it is 4.0 that adding unslaked lime is neutralized to pH, mixes (1: 1, volume ratio) with the worts of 2 degree, and two kinds of bacterial classifications of step breeding are bred 24-56h in the adding under 30 ℃ condition.Wherein, the volume percent of two kinds of bacterial classifications is 10%;
The wood chip yeast accounts for 60% pipe capsule yeast and accounts for 40%;
The bacterial classification that c takes out the b breeding is put in the wort of 2 degree, breeds 36h down for 30 ℃;
D increases the volume percent of hydrolyzed solution with 10%, other condition constant repetition b and c are hydrolyzed liquid fully to wort and substitute.
The composite zymocyte liquid of the back two kinds of bacterium of domestication is dropped in the fermentor tank, input amount be said supernatant liquor volume 5%, 33 ℃ of leavening temperatures, fermentation time 48h obtains tunning, wherein, the alcoholic acid volumetric concentration is 2.4%;
Alcoholic acid rectifying is a kind of prior art, its method referring to: permitted Kaitian. the alcohol distillation technology. Beijing: light industry press, 1990 (first versions), after rectifying tower 5 rectifying, collecting alcoholic acid purity is 95%;
Fermented waste fluid after the rectifying pumps in the anaerobic reactor earlier with constant flow pump, the anaerobic reactor upper liquid is pumped in the aerobic reactor with identical flow velocity by an other constant flow pump simultaneously, the residence time of fermented waste fluid in the anaerobic and aerobic reactor all is 24h.
Waste water after handling is pumped into the complex acid groove, carrying out complex acid with sulfuric acid uses for next hydrolysis, the mole number of calcium ion equates in vitriolic mole number that uses and the liquid, generate calcium sulfate precipitation and hydrochloric acid behind the complex acid, add behind the sulfuric acid if the acid concentration of solution does not reach preset value, replenish with hydrochloric acid, what play katalysis is hydrochloric acid.
Is raw material with granularity less than the duckweed of 1cm, and other hydrolysis process condition is identical with embodiment 1, and sugared concentration is 6.7wt% in the gained hydrolysis prods.
Divided by high-pressure saturated steam reactor 2 is preheating to 170 ℃, to be preheating to 170 ℃ 1200ml 1wt%HCl by high-pressure saturated steam is that catalytic liquid pumps into reactor 2 China and foreign countries, other processing condition are identical with embodiment 1, and sugared concentration is 5.6wt% in the gained hydrolysis prods.
Above result as can be seen, producing alcohol fuel with cellulose waste double thin acid hydrolysis is a kind of preparation method of alcohol fuel preferably.
Claims (7)
1. prepare the alcoholic acid method by cellulose waste double thin acid hydrolysis, it is characterized in that, comprise the steps:
(1) the cellulose castoff raw material is added in second hydrolysis reactor (2) and the 3rd hydrolysis reactor (3), hydrolysis reactor (2) is heated to 100-130 ℃, with temperature is that 100～130 ℃ weight concentration is that the aqueous hydrochloric acid of 0.05-5% pumps into hydrolysis reactor (2), reacted 1～60 minute, this time hydrolyzed solution is bled off as waste water;
(2) second hydrolysis reactor (2) is heated to 130～170 ℃, with temperature is that 130～170 ℃ weight concentration is that the aqueous hydrochloric acid of 0.05-5% pumps in second hydrolysis reactor (2), reacted 1～60 minute, then the hydrolyzed solution product in the hydrolysis reactor 2 is put into the 3rd hydrolysis reactor (3) that the cellulose castoff raw material is housed, 100-130 ℃ of reaction 1～60 minute, obtain hydrolysis prods, sugared concentration is 4～12wt%;
The material of remnants in the 3rd hydrolysis reactor (3) is the Mierocrystalline cellulose and the xylogen that are used for second hydrolysis reactor (2);
Then the residue in second hydrolysis reactor (2) is discharged, new cellulose castoff raw material is added in second hydrolysis reactor (2), continue the process of step (2), can obtain hydrolysis prods continuously;
(3) unslaked lime is added step (2) gained hydrolysis prods, control pH is 3.5-6.0, static 3-12 hour, collect supernatant liquor and send into fermentor tank (4), in fermentor tank (4), add zymocyte liquid, the add-on of zymocyte liquid is the 4-15% of hydrolysis prods volume, at 28-40 ℃ of bottom fermentation 24-56h, obtains tunning;
Bacterial classification in the said zymocyte liquid is selected from the wood chip yeast after the domestication and manages the composite bacteria of two kinds of bacterium of capsule yeast;
(4) with the acquisition tunning of step (3), adopt rectificating method, carry out rectifying, collect ethanol wherein.
2. method according to claim 1 is characterized in that, is that 130～170 ℃ weight concentration is that the aqueous hydrochloric acid of 0.05-5% pumps in second hydrolysis reactor 2 with temperature, the aqueous hydrochloric acid add-on be the cellulose castoff raw material weight 3-15 doubly.
3. method according to claim 1 is characterized in that, the add-on of zymocyte liquid is the 4-15%% of hydrolysis prods volume.
4. method according to claim 1 is characterized in that, after reaction finishes, to the 0.5-4 water washing hydrolytic residue doubly of the 3rd hydrolysis reactor (3) adding raw material weight, collects the hydrolysis water that water lotion participates in following batch of cellulose castoff raw material.
5. method according to claim 1 is characterized in that, also comprises:
(5) will separate the alcoholic acid fermented waste fluid, adopt the supernatant after anaerobic and aerobic are handled to pump into the complex acid groove, add sulfuric acid and carry out complex acid, the mole number of the calcium ion in vitriolic mole number and the fermented waste fluid equates, generate calcium sulfate precipitation and hydrochloric acid behind the complex acid, if the acid concentration of solution does not reach preset value, replenish with hydrochloric acid behind the adding sulfuric acid, what play katalysis is hydrochloric acid.
6. according to each described method of claim 1～5, it is characterized in that said cellulose castoff comprises other growth of agricultural wastes, forestry waste, forestry processing waste, waterplant, energy crop and biomass.
7. method according to claim 6 is characterized in that cellulose castoff is crushed to the particle less than 2cm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102010882A (en) * | 2010-09-21 | 2011-04-13 | 华东理工大学 | Method for performing lignocelluloses raw material high-temperature diluted acid pretreatment by using extremely small amount of water |
| CN102277389A (en) * | 2011-06-22 | 2011-12-14 | 中国科学院成都生物研究所 | Method for producing fuel ethanol by fermenting duckweed |
| CN103003435A (en) * | 2010-06-30 | 2013-03-27 | 欧内斯特·斯图尔特 | Universal biomass refinery |
| CN103814141A (en) * | 2011-09-21 | 2014-05-21 | 国际壳牌研究有限公司 | Process for conversion of xylan-containing feed |
| CN104903469A (en) * | 2012-10-13 | 2015-09-09 | 生物产品创新绿糖有限公司 | Method for hydrolysis of pelletizable biomasses using hydrohalic acids |
-
2007
- 2007-04-26 CN CNA2007100400589A patent/CN101041835A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103003435A (en) * | 2010-06-30 | 2013-03-27 | 欧内斯特·斯图尔特 | Universal biomass refinery |
| CN102010882A (en) * | 2010-09-21 | 2011-04-13 | 华东理工大学 | Method for performing lignocelluloses raw material high-temperature diluted acid pretreatment by using extremely small amount of water |
| CN102277389A (en) * | 2011-06-22 | 2011-12-14 | 中国科学院成都生物研究所 | Method for producing fuel ethanol by fermenting duckweed |
| CN102277389B (en) * | 2011-06-22 | 2014-04-30 | 中国科学院成都生物研究所 | Method for producing fuel ethanol by fermenting duckweed |
| CN103814141A (en) * | 2011-09-21 | 2014-05-21 | 国际壳牌研究有限公司 | Process for conversion of xylan-containing feed |
| CN104903469A (en) * | 2012-10-13 | 2015-09-09 | 生物产品创新绿糖有限公司 | Method for hydrolysis of pelletizable biomasses using hydrohalic acids |
| CN104903469B (en) * | 2012-10-13 | 2019-03-22 | 生物产品创新绿糖有限公司 | Method for biomass that can be pellet by halogen acids hydrolysis |
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Open date: 20070926 |