CN101643796A - Method for utilizing straw biomass by grades - Google Patents
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Abstract
The invention discloses a method for utilizing straw biomass by grades, comprising the following steps: carrying out steam explosion to straw biomass; extracting and separating water soluble constituents and water insoluble constituents in steam exploded straw by water, wherein the water soluble constituents are purified and concentrated to obtain active low polyxylose and xylose and the water insoluble constituents are used for further fermentation to generate ethanol; and extracting lignin from the fermentation residue. The invention realizes the maximization of utilization of biomass and overcomes the disadvantages of high production cost, low efficiency and environmental pollution and the like in the prior art.
Description
Technical field
The invention belongs to biomass and utilize technical field, specifically, be that classification about a kind of stalk biomass utilizes method, more specifically, be about realizing its three big main ingredient Mierocrystalline cellulose, hemicellulose and lignin conversion and isolating method by physico-chemical process by stalk biomass.
Background technology
Because the worsening shortages of traditional energy, make the utilization of the renewable energy source comprise biomass (comprise account for 40% Mierocrystalline cellulose, account for 30% hemicellulose and account for 30% xylogen) rise, be expected in the energy structure in future, play an important role.The most representative in the recovery energy technology of biomass at present is biomass biochemical conversion and thermochemistry transformation technology, wherein the biochemical conversion technology is low because of its energy expenditure, reaction conditions is gentle and transformation efficiency than characteristics such as height, be considered to industrialization potential always and utilize technology preferably.
In recent years, be raw material with various biomass, the most noticeable by the cellulose hydrolysis preparing ethanol by fermentation, scientific research institution and enterprise have also carried out a series of pilot scale and commercialization demonstration in succession both at home and abroad.Utilize cellulose fermentation in the biomass such as stalk to produce alcoholic acid technology and mainly comprise hydrolysis and two steps of fermentation, wherein hydrolysis is divided into acid hydrolysis and two kinds of methods of enzymic hydrolysis again, promptly by under the differential responses condition, under the catalysis of mineral acid (strength sulfuric acid as 70% or dilute sulphuric acid) or enzyme (as cellulase), Mierocrystalline cellulose resolves into the hexose based on glucose in water.These products can be with the different ethanol of hexose fermentation generation concentration by the zymotechnique of routine in fermentor tank or reactor.Because above-mentioned technology can only realize that Mierocrystalline cellulose transforms to alcoholic acid, and more a large amount of hemicelluloses and xylogen are used and burn or modes such as compost are utilized, economic worth is not high, causes this technology can't reach the commercialization requirement, causes the wasting of resources and environmental pollution simultaneously yet.
Hemicellulose is an important intermediate raw material of producing oligose such as xylo-oligosaccharide.Oligose has caused the attention of academia and industrial community because of having significant propagation bifidus bacillus and improving GI effect.The SANZHU KOUFUYE of home sale, ANGLI No.1 etc. are the ecological microbial agents based on bifidus bacillus, and active oligose is compared with ecological microbial agent as the bifid somatomedin, have oxytolerant acidproof, can together take, be difficult for advantage (Sakai such as inactivation, production cost be low with microbiotic, K., et al., Agric.Biol.Chem., 1987,51 (2): 315-322).Be widely used in food-processing, healthcare products and the medicine at the active oligose of Japan, the sales volume of 19 kinds of active oligose reaches 4.7 ten thousand tons, the output value surpass 10,000,000,000 yen (in happiness brightness husband for a long time, use the saccharic science, 1995,42 (3): 275-283).Production method mainly contains 4 kinds, and (build etc. in horizontal field, makes association, 1994,89 (8): 626-683): (1) natural matter extraction method---extract from sugar beet juice as raffinose, soybean oligosaccharide extracts from soybean is clear, because content is low in the natural matter, extraction method is subjected to the restriction of raw material; (2) acid hydrolysis natural polysaccharide method---because acid-hydrolyzed poor selectivity, carbohydrate complexity in hydrolyzed solution is difficult to obtain specific oligose; (3) chemical synthesis---owing to the production cost height, only limit to the functional study of oligose at present; (4) enzyme engineering method---utilize the shift reaction or the lytic enzyme hydrolysis natural polysaccharide of the functional group of transferring enzymes, because the selectivity of enzyme is strong, easily obtain specific oligose, pollution-free, production cost is low, so become the method for industrial practicality.Current China food configuration is reasonable inadequately, only malto-oligosaccharide, dextrinosan and stachyose have been carried out research and produced (Quan Qirong, foodstuffs industry, 1995, (3): 5-6), the raw materials for production of xylo-oligosaccharide are mainly corn cob in the oligose, exist the raw materials for production kind single, there are problems such as bigger pollution in production process, is badly in need of environmental protection more, the suitability for industrialized production technology of active oligomeric xylose efficiently.
Xylogen is a kind of natural polymer, in industries such as macromolecule chemical industry, building materials industry, light industry and agriculturals extensive use is arranged.Produce " black liquor " by traditional paper industry at present, obtain sulfonated lignin or alkali lignin through separation and Extraction.Because the chemical functional group of xylogen is damaged in papermaking process, poor-performing is difficult to prepare high value-added product, and the effect of these lignin derivatives is greatly affected.
Therefore, be necessary that attempting developing new reasonable in technology efficiently utilizes biomass resources such as stalk,, obtain the function sugar of high added value, and make full use of fermentation residue, extract xylogen, avoid environmental pollution, improve economic worth transforming the acquisition alcoholic acid simultaneously.
Summary of the invention
Purpose of the present invention just is to utilize stalk biomass fully efficiently, thereby provides a kind of classification of stalk biomass to utilize method.
The classification of stalk biomass of the present invention utilizes method may further comprise the steps:
A, that stalk biomass is carried out vapour is quick-fried;
B, separate water soluble ingredient and water-msoluble ingredients in the steam puffed stalk by the water extracting, water soluble ingredient wherein is purified, concentrate and obtain active oligomeric xylose and wood sugar, and water-msoluble ingredients then is further used for fermentative production of ethanol;
Xylogen in C, the extraction fermentation residue.
According to a preferred embodiment of the present invention, described stalk biomass is selected from one or more in the following material: straw, wheat straw, beanstalk, sorghum stalks, corn cob, cornstalk and cotton bar.
According to a further advantageous embodiment of the invention, attach most importance to compound extracting or continous way extracting of the extractive method of described water.
According to the present invention, described water soluble ingredient is based on hemicellulose; Concrete, described water miscible hemicellulose is wood sugar and xylo-oligosaccharide.
According to the present invention, the purifying of described water soluble ingredient can adopt the method for gac, macroporous resin or sephadex chromatography.
According to the present invention, the concentrated method that can adopt reduction vaporization or thin film evaporation of described water soluble ingredient; After reduction vaporization or thin film evaporation, also comprise the step of product being carried out nanometer filter or ultrafiltration.
According to the present invention, described water-msoluble ingredients is based on Mierocrystalline cellulose and xylogen.
According to a preferred embodiment of the present invention, described water-msoluble ingredients is used for fermentative production of ethanol and is meant after wherein Mierocrystalline cellulose resolves into glucose by cellulase and is used for fermentative production of ethanol.
According to a further advantageous embodiment of the invention, extracting xylogen from fermentation residue is to adopt organic solvent or inorganic base aqueous solution to extract.
According to a preferred embodiment of the present invention, before vapour was quick-fried, stalk biomass was ground into suitable size.
According to a further advantageous embodiment of the invention, the fermentation residue behind the extraction xylogen is further made fuel.
The classification of stalk biomass of the present invention utilizes method to have following beneficial effect:
1, adopts the thinking of Poly-generation to design and inherit, three kinds of main ingredients (hemicellulose, Mierocrystalline cellulose and xylogen) of stalk biomass are carried out fractional separation conversion fully and extracted the maximization that the realization biomass are utilized.
2, use the quick-fried technology of vapour to make the hydrolysis of hemicellulose in the stalk biomass become water miscible wood sugar and xylo-oligosaccharide, overcome shortcomings such as prior art production cost height, efficient are low, environmental pollution.
3, become glucose to be used for the technology of fermentative production of ethanol cellulose hydrolysis by cellulase, not only can overcome the feedback inhibition of grape sugar mutual-cellulose enzyme, and can reduce the consumption of cellulase, improve the efficient of cellulase.
Description of drawings
Fig. 1 is the conversion of Mierocrystalline cellulose, hemicellulose and xylogen and extracts schema.
Fig. 2 is the quick-fried retort synoptic diagram of vapour.
Fig. 3 is the board-like evaporation current journey of a triple effect vacuum synoptic diagram.
Fig. 4 separates Coupling device for airlift fermentation.
Embodiment
Stalk biomass comprises straw, wheat straw, beanstalk, sorghum stalks, corn cob, cornstalk, cotton bar etc., contains three kinds of important component: Mierocrystalline cellulose (accounting for 40%), hemicellulose (accounting for 30%) and xylogen (accounting for 30%).
The classification of stalk biomass of the present invention utilizes method, its technical process as shown in Figure 1, with the stalk biomass is raw material, at first the polyxylose degraded of hemicellulose contained in the stalk biomass is separated by the quick-fried technology of vapour, it is water-soluble that hemicellulose is had, pass through the extractive method of water then with water miscible hemicellulose and water-insoluble Mierocrystalline cellulose and lignin separation, wherein water miscible hemicellulose (main component is wood sugar and xylo-oligosaccharide) is further purified, obtain purified wood sugar and xylo-oligosaccharide after concentrating, and water-insoluble Mierocrystalline cellulose and xylogen are further used for fermentative production of ethanol, Mierocrystalline cellulose wherein produces the synchronous fermentative production of ethanol of glucose through enzymolysis, the lignin component that can not be used to ferment then further adopts organic solvent or inorganic base aqueous solution to extract, last fermentation residue can also further be used as fuel after drying, thereby realizes the maximization that biomass are utilized.
Below in conjunction with specific embodiment, the present invention will be further described.Should be understood that following examples only are used to the present invention to be described but not to be used to limits the scope of the invention.
Embodiment 1, steam explosion (vapour is quick-fried)
Use the quick-fried retort of vapour that straw-like materials is carried out steam-explosion in the present embodiment, the quick-fried retort of described vapour can be that for example the patent No. is a disclosed steam-explosion jar in 01218677.6 the Chinese utility model patent, concrete structure as shown in Figure 2, comprise tank body 10, the top of tank body 10 is provided with opening for feed 11, the bottom is provided with discharge port 12 and slag-drip opening 13, in addition, the top of tank body 10 is provided with saturation steam floral tube 14, the bottom is provided with saturation steam jet pipe 15, and the middle part is provided with compressed mixed gas (air and saturated steam) jet pipe 16.
As shown in table 1, be raw material with straw-like materials such as beanstalk, corn cobs respectively, use the quick-fried retort of vapour to carry out steam explosion, actual conditions is as follows:
Stalk biomass is ground into the segment of the about 25mm of length, gets the 80kg 1m that packs into
3The quick-fried retort of vapour in, feed compressed mixed gas and saturated steam, under suitable temperature and pressure, react for some time, instant decompression discharges then, discharges steam puffed stalk by the pulp cutlet of retort.
Table 1, steam explosion condition
| Sample | Straw-like materials | Temperature of reaction (℃) | Reaction pressure (Mpa) | Reaction times (min) |
| ??1 | Beanstalk | ??180 | ??1.3 | ??6 |
| ??2 | Corn cob+corn stalk | ??180 | ??1.5 | ??4 |
| ??3 | Straw | ??180 | ??1.0 | ??2 |
| ??4 | Wheat straw | ??190 | ??1.5 | ??4 |
| ??5 | Sorghum stalks | ??190 | ??1.8 | ??2 |
| ??6 | The cotton bar | ??200 | ??1.3 | ??6 |
Under the effect of the High Temperature High Pressure of straw-like materials such as beanstalk in the quick-fried retort of vapour, hemicellulose is wherein separated through vapour outburst unboiled water, generates wood sugar and xylo-oligosaccharide.
Embodiment 2, separate hemicellulose, Mierocrystalline cellulose and xylogen by steam puffed stalk
The steam puffed stalk (hemicellulose, Mierocrystalline cellulose and xylogen) that embodiment 1 is obtained is immersed in the concentration of 15wt% in 75 ℃ the hot water, carry out extracting after 4 hours, to isolate water miscible hemicellulose (wood sugar and xylo-oligosaccharide), water-insoluble Mierocrystalline cellulose and xylogen then still are retained in the stalk, and concrete method for extracting is as follows:
A) repeat formula extracting (sample 1～3)
Adopt and repeat the formula extracting 4 times, the filtrate of each extracting gained is used further to the new steam puffed stalk of extracting, and the sugared concentration of hemicellulose is respectively 92.6g/l, 85.3g/l and 83.9g/l (counter sample 1～3) in the extract that obtains;
B) continous way extracting (sample 4～6)
Adopt 4 continous way extractings, the continuous reverse input of material and water in operating process, the sugared concentration of hemicellulose is 35.12g/l, 38.21g/l and 28.63g/l (counter sample 4～6) in the extract that obtains.
Embodiment 3, purifying, concentrate xylo-oligosaccharide
Get the extract that embodiment 2 obtains, heating is concentrated into 1/4th of its volume, activated carbon chromatography post on the concentrated solution (aspect ratio is 5～10) is used 60% ethanol elution then, collects elutriant, with 3, the calibrating of 5-dinitrosalicylic acid method promptly stops to collect to no longer containing reducing sugar, merges the elutriant of collecting, adopt HPLC to analyze, analytical results shows that the reducing sugar that obtains is an active oligomeric xylose.
Under 40 ℃ of temperature condition, the active oligomeric xylose of collecting is carried out reduction vaporization to remove wherein contained ethanol (recyclable repeated use), promptly obtain active oligomeric xylose content through the nanometer filter again and be about 50% syrup.This syrup is water white thickness pulpous state, light sweet taste, does not have other peculiar smell, and with respect to the raw material dry weight, the yield of active oligomeric xylose is 10～15%.
Embodiment 4, concentrate wood sugar
Adopt triple effect vacuum plate-type evaporator to concentrate wood sugar.As shown in Figure 3, get among the embodiment 3 and hold back the filtered liquid that obtains behind the low xylan through the nanometer filter, wherein contained wood sugar mass percent concentration is about 6%, join in first single-effect evaporator 1 by charging opening 6, heating steam enters into the well heater of first single-effect evaporator 1 by steam-in 7, feed liquid after 1 distillation of first single-effect evaporator enters second single-effect evaporator 2, and the secondary steam of first single-effect evaporator, 1 vaporization continues to do the heating use as the heating chamber that thermal source feeds second single-effect evaporator 2, after second distillation finishes, feed liquid enters in the third effect evaporator 3, the steam of second single-effect evaporator, 2 vaporizations continues on for heating as the heating chamber that thermal source feeds third effect evaporator 3, after three distillations finish, steam feeds condensing equipment 5, feed liquid is collected by holding tank 4, the xylose concentration that finally obtains is about 80%, and with respect to the raw material dry weight, the yield of wood sugar is 15～20%.
Embodiment 5, the steam puffed stalk of fermentation after the water extracting produce ethanol
In the present embodiment, steam puffed stalk after the water extracting (water-insoluble Mierocrystalline cellulose and xylogen) is further used in fermentative production of ethanol, the employed fermentation reactor for example patent No. is 01131184.3 the disclosed airlift bioreactor of Chinese invention patent, concrete structure comprises retort 20 and activated carbon adsorption desorption apparatus 30 as shown in Figure 4; An internal recycle diversing bucket 21 is placed in the inside of retort 20, and the bottom of diversing bucket 21 is provided with gas distribution tube 22; Activated carbon adsorption desorption apparatus 30 comprises the activated carbon absorption tower 32 of condenser 31 and two parallel connections; CO is passed through at the top of retort 20
2Gas recycle pump 25 is connected with activated carbon absorption tower 32, and the below of condenser 31 is provided with collector 40.
Get the steam puffed stalk after the water extracting among the embodiment 2, be hybridly prepared into mixing solutions with 10IU FPA (filter paper enzyme activity international unit) cellulase preparation/g Mierocrystalline cellulose, join in the gas-lift fermentation reactor as fermention medium, wherein the content of steam puffed stalk is 15% (W/V), and loading amount is 70% of a reactor volume.Temperature is elevated to 120 ℃ to fermention medium sterilization 20 minutes, is cooled to 40 ℃ then, insert the yeast saccharomyces cerevisiae seed liquor of relative fermention medium weight about 5%, cool to 35～37 ℃ of fermentations.
After fermenting about 24～30 hours, concentration of ethanol reaches about 3wt% in the fermented liquid, opens CO this moment
2Gas recycle pump is with water vapor, the CO at airlift reactor top
2Extract out with the ethanol gas mixture, make the vacuum tightness of reactor head remain on 5000～8000Pa.
The gas mixture of extracting out enters one of them of two activated carbon adsorption towers in parallel, switches to another activated carbon adsorption tower after ethanol to be adsorbed reaches capacity and continues absorption, so hockets; Gac in the adsorption tower that the absorption of electrically heated simultaneously reaches capacity is with desorb ethanol, and desorption temperature is controlled at about 140 ℃; The ethanol that desorb is got off is collected in the product collector after the condenser desorb, obtains the coarse ethanol product, and its alcohol concn is about 65% after measured.
The CO that comes out from adsorption tower
2Gas sprays in the bio-reactor by the gas distribution tube of pipeline by the airlift reactor bottom, and fermented liquid is promoted in the internal recycle sleeve, and fermented liquid forms internal recycling in reactor, and is entrained with the ethanol in the fermented liquid.CO
2Gas circulation speed is 0.8～1.5vvm (per minute round-robin CO
2Gas volume and fermentating liquid volume ratio).
When glucose concn in the fermented liquid is reduced to lower level or zero, show that the Mierocrystalline cellulose in the stalk is converted into ethanol, fermentation ends substantially or all.
Get the stalk residue after fermentation among the embodiment 5, adopt further extraction xylogen wherein of following two kinds of methods respectively:
A) organic solvent extraction
Take by weighing in the mass percent of fermentation back, be heated to 90 ℃ then, kept 1.5 hours under pressure 0.3MPa, by filtering enzymolysis xylogen solution is separated with the impurity of other insoluble organic solvents, solution obtains enzymolysis xylogen 40.20 grams after solvent is sloughed in distillation.
B) inorganic base aqueous solution extracts
Take by weighing residue 100 grams after the fermentation, put into 1500 milliliters there-necked flask, add 500 ml concns and be 10% sodium hydroxide solution, stir and promoted enzymolysis art quality to be dissolved in the alkali aqueous solution in 15 minutes, be heated to 95 ℃ and be forced into 0.3MPa then, kept 1 hour, by filtering the insoluble impurity of enzymolysis xylogen solution and other is separated, after the hydrochloric acid of 152 milliliter 30% of solution adding is neutralized to neutrality (PH=7), stir on one side, add the water of 4 times of volumes of this solution on one side, left standstill 30 minutes, the enzymolysis xylogen precipitation is separated out filtering separation, water washing and precipitating and precipitation oven dry obtains enzymolysis xylogen 45.31 grams.
Residue behind the extracting xylogen can further be made fuel, and is specific as follows:
Residue among the embodiment 6 after extracting xylogen, water ratio is about 80%, carries out centrifuge dehydration earlier, and it is about 60% that dehydration back water ratio is reduced to, and further carries out drying (for example by tube bank moisture eliminator etc.) then, makes the water ratio in the residue be lower than 40%.Empirical tests, the residue of this moment can act as a fuel and be used for burning.
The present invention adopts the thinking of Poly-generation to design and inherit, it is water-soluble at first by the quick-fried technology of vapour hemicellulose to be had, realize the separation of biomass three big components through the water extracting, then according to the physicochemical property of different components, carry out classification and transform and extract and handle, realize the maximization that raw material is worth.Technical matters of the present invention has the advantage that adaptability to raw material is strong, the production process pollution is little, pattern is reproducible and added value of product is high, the component of stalk biomass is fully used, can also obtain the product such as ethanol, wood sugar, xylo-oligosaccharide, xylogen of high added value, thereby be with a wide range of applications.
Those skilled in the art will readily understand, that more than enumerates just implements a special case of the present invention, equipment such as quick-fried retort of wherein employed vapour and airlift bioreactor, all can adopt known other similar devices of prior art to replace, can not influence enforcement of the present invention, this is conspicuous.
Claims (13)
1, a kind of classification of stalk biomass utilizes method, it is characterized in that may further comprise the steps:
A, that stalk biomass is carried out vapour is quick-fried;
B, separate water soluble ingredient and water-msoluble ingredients in the steam puffed stalk by the water extracting, water soluble ingredient wherein is purified, concentrate and obtain active oligomeric xylose and wood sugar, and water-msoluble ingredients then is further used for fermentative production of ethanol;
Xylogen in C, the extraction fermentation residue.
2, method according to claim 1 is characterized in that: described stalk biomass is selected from one or more in the following material: straw, wheat straw, beanstalk, sorghum stalks, corn cob, cornstalk and cotton bar.
3, method according to claim 1 is characterized in that: the extractive method of described water attach most importance to compound extracting or continous way extracting.
4, method according to claim 1 is characterized in that: described water soluble ingredient is based on hemicellulose.
5, method according to claim 4 is characterized in that: described water miscible hemicellulose is wood sugar and xylo-oligosaccharide.
6, method according to claim 1 is characterized in that: the purifying of described water soluble ingredient is the method that adopts gac, macroporous resin or sephadex chromatography.
7, method according to claim 1 is characterized in that: the concentrated of described water soluble ingredient is the method that adopts reduction vaporization or thin film evaporation.
8, method according to claim 7 is characterized in that: described water soluble ingredient also comprises the step of nanometer filter or ultrafiltration after reduction vaporization or thin film evaporation.
9, method according to claim 1 is characterized in that: described water-msoluble ingredients is based on Mierocrystalline cellulose and xylogen.
10, method according to claim 9 is characterized in that: described water-msoluble ingredients is used for fermentative production of ethanol and is meant after wherein Mierocrystalline cellulose resolves into glucose by cellulase and is used for fermentative production of ethanol.
11, method according to claim 1 is characterized in that: extracting xylogen from fermentation residue is to adopt organic solvent or inorganic base aqueous solution to extract.
12, method according to claim 1 is characterized in that: before vapour was quick-fried, stalk biomass was ground into suitable size.
13, method according to claim 1 is characterized in that: the fermentation residue behind the extraction xylogen is further made fuel.
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