CN105154986A - Comprehensive cotton stalk base utilization method through combinations of alkali pretreatment, low pressure steam explosion and bio-enzyme treatment - Google Patents
Comprehensive cotton stalk base utilization method through combinations of alkali pretreatment, low pressure steam explosion and bio-enzyme treatment Download PDFInfo
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Abstract
The invention relates to a comprehensive cotton stalk base utilization method through combinations of alkali pretreatment, low pressure steam explosion and bio-enzyme treatment. After alkali pretreatment to the cotton stalk base, low steam explosion with alkali liquid is conducted to reduce furfural and other substance preventing follow-up diastatic fermentation. Crude fibers and hydrolysate are both collected after steam explosion, washed, filtered and centrifugally separated to acquire clean crude fibers and supernate and residuals. The crude fibers are further processed via laccase to acquire fine and soft cotton stalk base fibers. The supernate and the residuals are hydrolyzed and saccharified via bio-enzyme to achieve monosaccharide and then the monosaccharide is fermented to achieve biological ethyl alcohol. The steam explosion condition is reduced via alkali pretreatment; the fibers are achieved via steam explosion and then the residuals and hydrolysis achieved via steam explosion are prepared to be biological ethyl alcohol, so cellulosic fibers in the cotton stalk base and hemicellulose, polysaccharide and monosaccharide can be achieved via comprehensive utilization; and cotton stalk base utilization rate can be improved.
Description
Technical field
The present invention relates to a kind of biomass resource utilization method, especially relate to a kind of oxygenation pretreatment, method that low pressure vapor dodges the cotton stalk skin of quick-fried and Bio-enzyme Combined Pre-treatment treatment and comprehensive utilization, belong to biomass resource utilization field.
Background technology
Cotton stalk, as the byproduct of cotton planting, contains cellulose and the non-cellulosic material such as lignin, hemicellulose in its surperficial bast.Cotton stalk skin belongs to renewable resource, its content of cellulose about 40%, and extract from cotton stalk skin and be suitable for weaving, cotton stalk hide fiber prepared by composite, contributes to the value improving cotton crop.At present, most of cotton stalk is treated as waste combustion, causes the significant wastage of living resources.So, develop particularly important better to cotton stalk bast.
At present, the patent relating to the utilization of cotton stalk skin mainly contains: (1) stalk biomass utilization of resources, as patent of invention " biomass straw many mouthfuls dodges quick-fried preliminary treatment production system and production technology thereof " (publication number: CN104474975A), utilize biomass straw raw material to dodge quick-fried technology, produce inhomogeneous product by biomass straw fodder production line, edible powder production line, pulping production line, production alcohol fuel production line and wood plastics composite production of construction materials line; (2) steam explosion legal system is for cotton stalk hide fiber, as patent of invention " a kind of cotton stalk hide fiber cleans Degumming method " (publication number: CN101008108A), adopts the quick-fried method combined with High Temperature High Pressure post processing of sudden strain of a muscle to prepare cotton stalk hide fiber; Patent of invention " a kind of steam explosion and alkali treatment combine and prepare the method for the cotton stalk hide fiber of weaving " (publication number: CN104047063A), steam explosion is first adopted to be separated cotton stalk skin, then process further with potassium hydroxide, finally use hydrogen peroxide bleaching.After steam explosion, fiber yield is about 50%, and about 30% to be separated, the hemicellulose of degrading is left in the basket.Patent utilization oxygenation pretreatment of the present invention, reduces and dodges detonation pressure power, and while utilizing cellulose fibre, after utilizing sudden strain of a muscle quick-fried, except fiber, about 30% material diastatic fermentation prepares Ethanol, improves cotton stalk skin utilization rate.
Summary of the invention
In order to improve the utilization rate of cotton stalk skin further, especially can utilize the material such as cellulose fibre and isolated hemicellulose, polysaccharide, monose in cotton stalk skin, the present invention reduces the pressure of steam explosion simultaneously.For guaranteeing that cotton stalk skin can obtain good separating effect under lower steam explosion condition, first use the cotton stalk skin of oxygenation pretreatment, pretreated cotton stalk belt alkali lye and is adopted the sudden strain of a muscle of the steam explosion technique testing desk of compole short (0.0875s) when dodging quick-fried quick-fried; Lower steam explosion condition can reduce the materials such as the furfural hindering follow-up diastatic fermentation and produce, and fully utilizes cotton stalk skin.
The technical solution adopted in the present invention is a kind of oxygenation pretreatment, low pressure vapor dodges method that is quick-fried and the cotton stalk skin of Bio-enzyme Combined Pre-treatment treatment and comprehensive utilization, specifically implements according to following steps:
(1) machine cuts: cotton stalk skin is cut into the section that 8 ~ 12cm is long;
(2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the aqueous slkali that solid-to-liquid ratio is 1: 10 ~ 1: 20, and alkali consumption is 2 ~ 20g/L;
(3) steam explosion: the cotton stalk skin after oxygenation pretreatment does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, saturated vapor pressure is made to reach 0.6 ~ 1.0Mpa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 60 ~ 300s, the crude fibre obtained and hydrolyzate are all collected, carry out following process respectively after steam explosion;
(4) wash: the crude fibre obtained after steam explosion is placed in the clear water cyclic washing that solid-to-liquid ratio is 1: 20 ~ 1: 40, with filter-cloth filtering, collect the crude fibre after cleaning and filtrate respectively, and crude fibre is at room temperature dried;
(5) laccase treatment: process crude fibre further by laccase mediator systems, is warming up to 90 ~ 100 DEG C and boils 1 ~ 2h after reaching the processing time;
(6) centrifugation: by filtrate and hydrolyzate centrifugation, collects supernatant and residue respectively, and the residue obtained is dried, pulverized;
(7) xylanase hydrolysis: add zytase and be hydrolyzed saccharification in supernatant, be warming up to 90 ~ 100 DEG C after reaching the processing time and boil 1 ~ 2h;
(8) cellulase treatment: with cellulase and hemicellulase complex treatment residue, hydrolysis and saccharification, is warming up to 90 ~ 100 DEG C and boils 1 ~ 2h after reaching the processing time;
(9) ferment: after enzymolysis liquid step (7) and (8) obtained is centrifugal, get supernatant collection together, fermenting and preparing biological alcohol.
2, oxygenation pretreatment according to claim 1, it is characterized in that, described alkali is NaOH or potassium hydroxide, and pretreatment temperature can be normal temperature, soaks 10 ~ 24h, also can be 60 ~ 100 DEG C, soda boiling 1 ~ 5h.
3, wash according to claim 1, it is characterized in that, first cotton stalk skin crude fibre being placed in solid-to-liquid ratio is 1: 20 ~ 1: 30,90 ~ 100 DEG C of hot water poach 1 ~ 2h, after in normal-temperature water wash 0.5 ~ 1.5h.
4, laccase mediator systems according to claim 1 processes crude fibre further, it is characterized in that, described laccase is from white-rot fungi or rainbow conk, treatment temperature is 25 ~ 55 DEG C, solid-to-liquid ratio is 1: 10 ~ 1: 25, pH value is 3.0 ~ 6.0, laccase consumption is the cotton stalk hide fiber of 20 ~ 600U/g, described amboceptor is ABTS or HBT, consumption is 0.5 ~ 6% of cotton stalk hide fiber dry weight, processing time is 5 ~ 25h, fiber after process clear water is cleaned, dry at ambient temperature, fiber pin tooth density after drying is the stainless steel comb combing of 10 ~ 15 teeth/cm, obtain cotton stalk skin fine fibre.
7, xylanase treatment supernatant according to claim 1, is characterized in that, zytase consumption is 50 ~ 300U/mL supernatant, and treatment temperature is 30 ~ 50 DEG C, and pH value is 4.0 ~ 6.0, and the processing time is 24 ~ 72h;
6, residue biology enzyme saccharification processing procedure according to claim 1, it is characterized in that, hemicellulase and cellulase amount ratio are 1: 1 ~ 1: 4, treatment temperature is 30 ~ 50 DEG C, solid-to-liquid ratio is 1: 10 ~ 1: 25, and pH value is 4.0 ~ 6.0, and the processing time is 24 ~ 72h;
7, fermentation according to claim 1, it is characterized in that, cultivate 24 ~ 48h to accessing after the supernatant sterilizing obtained after enzymolysis, thermotolerant yeast cell liquid that concentration reaches 1 ~ 5g/L, cell liquid consumption is 0.5 ~ 2% of supernatant weight, anaerobic fermentation 24 ~ 48h under 35 ~ 45 DEG C of conditions.
In above each operation:
(1) oxygenation pretreatment not only can moisten the cellulose that rises, and can also make hemicellulose generation deacetylation simultaneously, between cell membrane and intercellular layer, form hole, thus is conducive to saturated vapor and water infiltration internal batch, is beneficial to Steam explosion treatment.
(2) the cotton stalk skin after oxygenation pretreatment does not wash, directly dodge quick-fried with alkali lye, in the dwell time, alkali and hemicellulose, lignin etc. react, more excellent fiber can be obtained on the one hand, steam explosion condition can be reduced on the other hand, reduce furfural etc. and hinder the material of follow-up diastatic fermentation to produce.
(3), before steam explosion, dodging quick-fried after being extruded by circulating water, is the uniformity in order to improve reaction.
(4) effect of hot water poach is on the one hand that the lignin that prevents from having deviate from and hemicellulose are again again agglomerated together, is the sugar and the stripping of part soluble sugar that make hemicellulose degradation after steam explosion on the other hand.
(5) process of laccase mediator systems removes lignin emphatically, the mechanism of its lignin degrading: in the presence of oxygen, amboceptor is oxidized to active high and have the intermediate of certain stability by laccase, these reactive intermediates can obtain electronics from oxygen molecule, and give lignin molecule electron transmission, thus lignin oxidation is degraded, oxygen is reduced into water.
(6) deactivation is to prevent enzyme liquid from remaining.
(7) fiber dries at ambient temperature and does not dry and mainly prevents fiber adhesion, be convenient to combing, and the fiber that the fabric hand naturally dried comparatively is dried is good.
(8) sterilizing is to go out except the bacterium carried in supernatant after enzyme hydrolysis.
The invention has the beneficial effects as follows, dodge quick-fried with Bio-enzyme Combined Pre-treatment process by oxygenation pretreatment, low pressure vapor, while obtaining thin, soft cotton stalk hide fiber, utilize the hydrolyzate after steam explosion and residue to prepare Ethanol, fully utilize cotton stalk skin.
Accompanying drawing explanation
Fig. 1 is cotton stalk skin comprehensive utilization flow chart.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described.
The present invention first uses the cotton stalk skin of oxygenation pretreatment, after with alkali lye adopt blasting time extremely short (0.0875s) steam explosion technique testing desk steam explosion, reduce steam explosion condition, obtain cellulose fibre on the one hand, low-pressure can reduce the material generations such as the furfural hindering follow-up diastatic fermentation on the other hand, improves cotton stalk skin utilization rate.
Embodiment 1
(1) machine cuts: cotton stalk skin is cut into the section that 8cm is long;
(2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the sodium hydroxide solution soak at room temperature 20h that solid-to-liquid ratio is 1: 10, and sodium hydroxide concentration is 14g/L;
(3) steam explosion: the cotton stalk skin after oxygenation pretreatment does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, saturated vapor pressure is made to reach 0.6Mpa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 300s, the crude fibre obtained and hydrolyzate are all collected, carry out following process respectively after steam explosion;
(4) wash: first the cotton stalk skin crude fibre obtained after steam explosion is placed in solid-to-liquid ratio be 1: 20 90 DEG C of hot water wash 2h, being placed on solid-to-liquid ratio is wash 0.5h in the normal-temperature water of 1: 40, with filter-cloth filtering, collect the crude fibre after cleaning and filtrate respectively, and crude fibre is at room temperature dried;
(5) laccase treatment: process crude fibre further by laccase mediator systems, laccase is from white-rot fungi, treatment temperature is 50 DEG C, solid-to-liquid ratio is 1: 15, pH value is 3.0, laccase consumption is the cotton stalk hide fiber of 150U/g, amboceptor ABTS, consumption is 2% of cotton stalk skin crude fibre dry weight, and the processing time is 10h, is warming up to 90 DEG C and boils 2h after reaching the processing time, fiber clear water is cleaned, dry at ambient temperature, the fiber pin tooth density after drying is the stainless steel comb combing of 10 teeth/cm, obtains cotton stalk skin fine fibre;
(6) centrifugation: by filtrate and hydrolyzate centrifugation, collects supernatant and residue respectively, and the residue obtained is dried, pulverized;
(7) xylanase hydrolysis: add zytase and be hydrolyzed saccharification in supernatant, zytase consumption is 100U/mL supernatant, and treatment temperature is 35 DEG C, and pH value is 5.0, and the processing time is 48h, is warming up to 90 DEG C and boils 2h after reaching the processing time;
(8) cellulase treatment: with cellulase and hemicellulase complex treatment residue, hydrolysis and saccharification, hemicellulase and cellulase amount ratio are 1: 4, treatment temperature is 45 DEG C, solid-to-liquid ratio is 1: 20, pH value is 5.0, and the processing time is 24h, is warming up to 90 DEG C and boils 2h after reaching the processing time;
(9) ferment: enzymolysis liquid centrifuging and taking supernatant collection step (7) and (8) obtained together, access after sterilizing and cultivated 48h, thermotolerant yeast cell liquid that concentration is 5g/L, cell liquid consumption is 0.5% of supernatant weight, at 35 DEG C, anaerobic fermentation 24h, prepares Ethanol.
Embodiment 2
(1) machine cuts: cotton stalk skin is cut into the section that 10cm is long;
(2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in sodium hydroxide solution 70 DEG C of soda boiling 4h that solid-to-liquid ratio is 1: 15, and sodium hydroxide concentration is 10g/L;
(3) steam explosion: the cotton stalk skin after oxygenation pretreatment does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, saturated vapor pressure is made to reach 0.8Mpa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 180s, the crude fibre obtained and hydrolyzate are all collected, carry out following process respectively after steam explosion;
(4) wash: first the cotton stalk skin crude fibre obtained after steam explosion is placed in solid-to-liquid ratio be 1: 30 100 DEG C of hot water wash 1h, being placed on solid-to-liquid ratio is wash 1h in the normal-temperature water of 1: 30, with filter-cloth filtering, collect the crude fibre after cleaning and filtrate respectively, crude fibre is at room temperature dried;
(5) laccase treatment: process crude fibre further by laccase mediator systems, laccase is from white-rot fungi, treatment temperature is 55 DEG C, solid-to-liquid ratio is 1: 20, pH value is 3.5, laccase consumption is the cotton stalk hide fiber of 300U/g, amboceptor ABTS, consumption is 1% of cotton stalk skin crude fibre dry weight, and the processing time is 15h, is warming up to 95 DEG C and boils 1.5h after reaching the processing time, fiber clear water is cleaned, dry at ambient temperature, the fiber pin tooth density after drying is the stainless steel comb combing of 15 teeth/cm, obtains cotton stalk skin fine fibre;
(6) centrifugation: by filtrate and hydrolyzate centrifugation, collects supernatant and residue respectively, and the residue obtained is dried, pulverized;
(7) xylanase hydrolysis: add zytase and be hydrolyzed saccharification in supernatant, zytase consumption is 150U/mL supernatant, and treatment temperature is 40 DEG C, solid-to-liquid ratio is 1: 25, pH value is 4.0, and the processing time is 36h, is warming up to 95 DEG C and boils 1.5h after reaching the processing time;
(8) cellulase treatment: with cellulase and hemicellulase complex treatment residue, hemicellulase and cellulase amount ratio are 1: 3, treatment temperature is 40 DEG C, solid-to-liquid ratio is 1: 25, pH value is 4.0, processing time is 48h, hydrolysis and saccharification, is warming up to 95 DEG C and boils 1.5h after reaching the processing time;
(9) ferment: enzymolysis liquid centrifuging and taking supernatant collection step (7) and (8) obtained together, access after sterilizing and cultivated 36h, thermotolerant yeast cell liquid that concentration is 3g/L, cell liquid consumption is 1% of supernatant weight, at 40 DEG C, anaerobic fermentation 36h, prepares Ethanol.
Embodiment 3
(1) machine cuts: cotton stalk skin is cut into the section that 12cm is long;
(2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in potassium hydroxide solution 80 DEG C of soda boiling 3h that solid-to-liquid ratio is 1: 20, and alkali consumption is 8g/L;
(3) steam explosion: the cotton stalk skin after oxygenation pretreatment does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, saturated vapor pressure is made to reach 1.0Mpa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 120s, the crude fibre obtained and hydrolyzate are all collected, carry out following process respectively after steam explosion;
(4) wash: first by dodge quick-fried after the cotton stalk skin crude fibre that obtains be placed in solid-to-liquid ratio be 1: 25 85 DEG C of hot water boil 1.5h, being placed on solid-to-liquid ratio is cyclic washing 1.5h in the normal-temperature water of 1: 20, with filter-cloth filtering, collect the crude fibre after cleaning and filtrate, crude fibre is at room temperature dried;
(5) laccase treatment: process crude fibre further by laccase mediator systems, laccase is from rainbow conk, treatment temperature is 45 DEG C, solid-to-liquid ratio is 1: 25, pH value is 4.0, laccase consumption is the cotton stalk hide fiber of 100U/g, amboceptor HBT, consumption is 5% of cotton stalk hide fiber dry weight, and the processing time is 25h, is warming up to 100 DEG C and boils 1h after reaching the processing time, fiber clear water is cleaned, dry at ambient temperature, the fiber pin tooth density after drying is the stainless steel comb combing of 12.5 teeth/cm, obtains cotton stalk skin fine fibre;
(6) centrifugation: by filtrate and hydrolyzate centrifugation, collects supernatant and residue, and the residue obtained is dried, pulverized;
(7) xylanase hydrolysis: add zytase and be hydrolyzed saccharification in supernatant, zytase consumption is 300U/mL supernatant, and treatment temperature is 50 DEG C, and pH value is 6.0, and the processing time is 24h, is warming up to 100 DEG C and boils 1h after reaching the processing time;
(8) cellulase treatment: with cellulase and hemicellulase complex treatment residue, hemicellulase and cellulase amount ratio are 1: 1, and treatment temperature is 50 DEG C, solid-to-liquid ratio is 1: 15, pH value is 6.0, and the processing time is 72h, is warming up to 100 DEG C and boils 1h after reaching the processing time;
(9) ferment: enzymolysis liquid centrifuging and taking supernatant collection step (7) and (8) obtained together, access after sterilizing and cultivated 24h, thermotolerant yeast cell liquid that concentration is 2g/L, cell liquid consumption is 2% of supernatant weight, at 45 DEG C, anaerobic fermentation 48h, prepares Ethanol.
Above-mentioned explanation fully discloses the specific embodiment of the present invention.It is pointed out that the scope be familiar with person skilled in art and any change that the specific embodiment of the present invention is done all do not departed to claims of the present invention.Correspondingly, the scope of claim of the present invention is also not limited only to previous embodiment.
Claims (7)
1. oxygenation pretreatment, low pressure vapor dodge a method that is quick-fried and the cotton stalk skin of Bio-enzyme Combined Pre-treatment treatment and comprehensive utilization, and it is characterized in that, the method comprises following processing step:
(1) machine cuts: cotton stalk skin is cut into the section that 8 ~ 12cm is long;
(2) oxygenation pretreatment: cotton stalk skin step (1) obtained is placed in the aqueous slkali that solid-to-liquid ratio is 1:10 ~ 1:20, and alkali consumption is 2 ~ 20g/L;
(3) steam explosion: the cotton stalk skin after oxygenation pretreatment does not wash, after circulating water is extruded, load and dodge in quick-fried tank, pass into saturated vapor, saturated vapor pressure is made to reach 0.6 ~ 1.0MPa, dodge quick-fried instantaneously with 0.0875s after maintaining saturated vapor pressure 60 ~ 300s, the crude fibre obtained and hydrolyzate are all collected, carry out following process respectively after steam explosion;
(4) wash: the crude fibre obtained after steam explosion is placed in the clear water cyclic washing that solid-to-liquid ratio is 1:20 ~ 1:40, with filter-cloth filtering, collect the crude fibre after cleaning and filtrate respectively, and crude fibre is at room temperature dried;
(5) laccase treatment: process crude fibre further by laccase mediator systems, is warming up to 90 ~ 100 DEG C and boils 1 ~ 2h after reaching the processing time;
(6) centrifugation: by filtrate and hydrolyzate centrifugation, collects supernatant and residue respectively, and the residue obtained is dried, pulverized;
(7) xylanase hydrolysis: add zytase and be hydrolyzed saccharification in supernatant, be warming up to 90 ~ 100 DEG C after reaching the processing time and boil 1 ~ 2h;
(8) cellulase treatment: with cellulase and hemicellulase complex treatment residue, hydrolysis and saccharification, is warming up to 90 ~ 100 DEG C and boils 1 ~ 2h after reaching the processing time;
(9) ferment: after enzymolysis liquid step (7) and (8) obtained is centrifugal, get supernatant collection together, fermenting and preparing biological alcohol.
2. oxygenation pretreatment according to claim 1, it is characterized in that, described alkali is NaOH or potassium hydroxide, and pretreatment temperature can be normal temperature, soaks 10 ~ 24h, also can be 60 ~ 100 DEG C, soda boiling 1 ~ 5h.
3. wash according to claim 1, it is characterized in that, first cotton stalk skin crude fibre being placed in solid-to-liquid ratio is 1: 20 ~ 1:30,90 ~ 100 DEG C of hot water poach 1 ~ 2h, after in normal-temperature water wash 0.5 ~ 1.5h.
4. laccase mediator systems process crude fibre according to claim 1, it is characterized in that, described laccase is from white-rot fungi or rainbow conk, treatment temperature is 25 ~ 55 DEG C, solid-to-liquid ratio is 1:10 ~ 1:25, pH value is 3.0 ~ 6.0, laccase consumption is the cotton stalk hide fiber of 20 ~ 600U/g, described amboceptor is ABTS or HBT, consumption is 0.5 ~ 6% of cotton stalk hide fiber dry weight, processing time is 5 ~ 25h, fiber after process clear water is cleaned, dry at ambient temperature, fiber pin tooth density after drying is the stainless steel comb combing of 10 ~ 15 teeth/cm, obtain cotton stalk skin fine fibre.
5. xylanase treatment supernatant according to claim 1, is characterized in that, zytase consumption is 50 ~ 300U/mL supernatant, and treatment temperature is 30 ~ 50 DEG C, and pH value is 4.0 ~ 6.0, and the processing time is 24 ~ 72h.
6. residue biology enzyme saccharification processing procedure according to claim 1, it is characterized in that, hemicellulase and cellulase amount ratio are 1:1 ~ 1:4, treatment temperature is 30 ~ 50 DEG C, solid-to-liquid ratio is 1:10 ~ 1:25, and pH value is 4.0 ~ 6.0, and the processing time is 24 ~ 72h.
7. fermentation according to claim 1, it is characterized in that, cultivate 24 ~ 48h to accessing after the supernatant sterilizing obtained after enzymolysis, thermotolerant yeast cell liquid that concentration reaches 1 ~ 5g/L, cell liquid consumption is 0.5 ~ 2% of supernatant weight, anaerobic fermentation 24 ~ 48h under 35 ~ 45 DEG C of conditions.
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