CN111518846A - Method for producing biogas by fermenting mild hydrothermal pretreatment corn straws - Google Patents
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- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
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- C12P5/023—Methane
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- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P2203/00—Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
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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 method for producing biogas by fermenting mild moist heat pretreated corn straws, which comprises the following steps: (1) crushing straws: drying and crushing the straws to obtain crushed straws; (2) pretreatment: mixing the crushed straws obtained in the step (1) with CaO2Mixing the solutions, treating at 75-85 ℃ for 12-24 h, and filtering to obtain straw paste; (3) anaerobic fermentation: adjusting the pH value of the straw paste obtained in the step (2) to 6.8-7.3, mixing the straw paste with biogas slurry, fermenting in a closed manner for 10-30 days, and collecting biogas generated by fermentation. The invention adopts CaO2As a pretreatment agent, the corn straw is treated under the mild damp and hot conditions, and an ideal methane generating effect is obtained. Compared with the conventional method, the method can obtain ideal treatment effect, increase treatment speed, reduce chemical use and generation of inhibitors, and has high utilization rate of the substrate. The invention is economic, efficient and environment-friendly, and is suitable for large-scale fermentation production of biogas by using the corn straws.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a method for producing biogas by fermenting mild moist heat pretreatment corn straws.
Background
Corn belongs to crops with wide planting areas and high yield, and has an economic coefficient of about 0.35, so that a large amount of agricultural wastes are generated in the production process of the corn. About 2.15 million tons of straws are not reasonably utilized every year nationwide. The straw treatment modes are various, wherein the energy output input ratio of the biogas produced by anaerobic fermentation reaches 28/1, the efficiency is high, the cost is low, and the economic benefit reaches more than twice of that of the biogas produced by briquettes. In addition, anaerobic fermentation is based on microorganisms, neither substrate sterilization nor special culture inoculation measures are required, and the requirements on technology and equipment are low.
In the process of carrying out anaerobic fermentation by taking corn straws as raw materials, the decomposition of complex organic matters in the corn straws by hydrolysis is the rate-limiting step of the anaerobic fermentation. In order to improve the hydrolysis efficiency of the straws, proper pretreatment measures are necessary. The commonly used pretreatment modes mainly include biological pretreatment, chemical pretreatment, physical pretreatment, combined pretreatment and the like. From the composition characteristics of the corn straws, the cellulose is insoluble in water and has strong resistance to depolymerization, the hemicellulose is very sensitive to biological, thermal and chemical hydrolysis, and the lignin has strong resistance to biological and chemical degradation. Alkali treatment is a well-established and convenient chemical pretreatment method. The alkali chemical reagent can saponify and break the connecting bond between lignin and carbohydrate, promote the hydrolysis of enzyme and increase the methane yield and methane content in anaerobic fermentation. However, the problem of steric hindrance of materials due to the single pretreatment with an alkali solution is solved, and the environmental and material costs are high, which is not favorable for environmental protection and equipment maintenance. At present, a method for producing biogas by high-valued conversion and anaerobic fermentation of corn straws, which gives consideration to economic benefits and environmental benefits, is lacked in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for producing biogas by fermenting mild moist heat pretreatment corn straws, which combines mild moist heat conditions with non-alkaline treatment agents and gives consideration to economic benefits and environmental benefits.
The specific technical scheme is as follows:
a method for producing biogas by fermenting mild moist heat pretreatment corn straws comprises the following steps:
(1) crushing straws: drying and crushing the straws to obtain crushed straws;
(2) pretreatment: mixing the crushed straws obtained in the step (1) with CaO2Mixing the solutions, treating at 75-85 ℃ for 12-24 h, and filtering to obtain straw paste;
(3) anaerobic fermentation: adjusting the pH value of the straw paste obtained in the step (2) to 6.8-7.3, mixing the straw paste with biogas slurry, fermenting in a closed manner for 10-30 days, and collecting biogas generated by fermentation.
Corn stover is mainly composed of highly lignified cell walls, where cellulose, hemicellulose and lignin are very tightly bound to form very difficult to destroy lignocellulose. In the process of anaerobic fermentation by taking corn straws as raw materials, because lignin and hemicellulose protect the winding of cellulose and the crystal structure of the cellulose, the contact of microorganisms and organic matters is hindered, and the efficiency of producing methane by anaerobic fermentation is reduced. In order to improve the conversion efficiency of the corn straws, proper pretreatment measures are necessary.
The basic non-alkaline solution includes all solutions having a pH >7 at normal temperature other than the alkaline solution, such as alkaline salt solutions, alkaline oxide solutions, organic solutions, and the like. The alkaline non-alkali solution is used, so that the damage of strong alkaline substances to the environment and equipment can be reduced, in addition, the alkaline non-alkali solution contains rich ions, if the biogas slurry is returned to the field, various elements necessary for plant growth can be provided, special effects such as fungus growth inhibition and the like can be achieved, the utilization efficiency of fermentation products can be greatly improved, and the efficient harmless treatment of the corn straws is realized.
CaO2Is a solid oxidant with low solubility, and can generate OH after slowly reacting with water-Ions, making the solution alkaline. With CaO2The solution has strong oxidability, and can destroy the crystal structure of crop straws to convert lignin into soluble aromatic compounds. Has no application in the field of the anaerobic fermentation production of methane by pretreating the corn straws.
Unexpectedly, the subject group discovered CaO2The solution is used as a mild heat treatment combined with a treating agent, and the efficiency of generating the biogas by fermenting the straws can be obviously improved. The principle may be that the alkaline non-alkali solution is in mild, humid and hot environmentThe degradation and dissolution of hemicellulose and lignin can be promoted, and more hemicellulose and lignin can be promoted to be converted into volatile fatty acid, so that the anaerobic fermentation of methane bacteria is facilitated.
The mild moist heat is different from the conventional moist heat pretreatment in that the temperature is low and the pretreatment is carried out under normal pressure. Conventional wet heat treatment is generally carried out under high pressure at 120 ℃ or higher.
Further, in the step (2), CaO2The concentration of the solution is 1.5-2.5 wt%. .
CaO2The definition of the solution concentration is necessary, too high a concentration having a negative effect on the efficiency of the biogas production.
Further, in the step (2), the straws and CaO are crushed2The mass ratio of the solution is 1: (8-15).
Further, in the step (3), before closed fermentation, adding water into the mixed liquid of the straw paste and the biogas slurry; dry matter in the straw paste: biogas slurry: the dosage ratio of water is 1 g: (10-16) mL: (2-5) mL.
Further, in the step (3), the pH adjustment is performed using an HCl solution. The HCL solution is preferably 0.3-0.5 mol/L dilute HCL solution "
Further, in the step (3), the fermentation temperature is 30-40 ℃.
Further, in the step (1), the straws are crushed into particles of 3-5 mm.
Further, in the step (1), the water content of the dried straw is below 0.5 wt%. The drying method is preferably hot air drying.
The invention has the following beneficial effects:
the invention adopts CaO2As a pretreatment agent, the corn straw is treated under the mild damp and hot conditions, and an ideal methane generating effect is obtained. Compared with the conventional method, the method can obtain ideal treatment effect, increase treatment speed, reduce chemical use and generation of inhibitors, and has high utilization rate of the substrate. In addition, CaO2The solution contains Ca2+If the biogas slurry is returned to the field, the ions can provide elements required by plant growth and can play a special role in inhibiting the growth of bacteria and the like, which will bring great importance to the fieldGreatly improves the utilization efficiency of fermentation products and realizes the high-efficiency harmless treatment of the straws. The COD value (chemical oxygen demand) and TVFA (total volatile fatty acid) content of the biogas residues obtained by the method are obviously lower than those of the conventional method, and ideal environmental benefits are obtained. The invention is economic, efficient and environment-friendly, and is suitable for large-scale fermentation production of biogas by using the corn straws.
Drawings
FIG. 1 is a schematic view showing the structure of a laboratory-made fermentation apparatus used in the present invention;
in the figure: 1. a sampling port; 2. a sealing cover; 3. a stirring motor; 4. a stirring paddle; 5. an air outlet; 6. an air collecting bag.
Detailed Description
The principles and features of this invention are described below in conjunction with examples, which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The corn straws used in the specific embodiment are taken from the experiment base of the tobacco stand research institute of Chinese agriculture university, and the straws are naturally air-dried and are dark yellow as a whole;
the inoculation biogas slurry used in the specific embodiment is black brown and sticky, and is taken from a biomass engineering laboratory of the tobacco institute of China university;
the main physicochemical properties of the above materials are shown in table 1.
TABLE 1 Main physicochemical Properties of the materials tested
In the specific implementation mode:
drying the TS content to constant weight at 110 ℃, and measuring by a differential weight method;
the pH value is measured by a thunder magnet PHSJ-6L type pH meter;
the cellulose and lignin adopt K2Cr2O7-H2SO4Measuring by an oxidation method;
measuring hemicellulose by adopting a copper iodine method;
c content is defined as K2Cr2O7-H2SO4Measuring by an oxidation method;
the content of N is measured by adopting a Kjeldahl method;
anaerobic fermentation gas production is collected by a gas collection bag, measured by a scale injector and then stored in the gas collection bag;
the methane content is measured by a Gasboard-3200plus methane analyzer;
the COD value is determined according to GB/T11914-89;
the TVFA measurement is calculated by a distillation titration method based on the acetic acid content.
Example 1
A method for producing biogas by fermenting mild, moist and hot pretreated straws comprises the following steps:
(1) crushing straws: carrying out hot air drying on the corn straws until the moisture content is below 0.5 wt%; crushing the dried corn straws into particles of 3-5 mm to obtain crushed straws;
(2) pretreatment: mixing the crushed straws obtained in the step (1) with CaO with the concentration of 2 wt%2Mixing the solutions, and filling into a conical flask; crushing straw and CaO2The mass ratio of the solution is 1: 12.5; placing the conical flask in a water bath kettle at 80 deg.C for 12 hr, filtering, and discarding filtrate to obtain straw paste;
determining the contents of lignin, cellulose and hemicellulose in the straw paste;
diluting the straw paste to 10 times of the original mass by using distilled water, uniformly stirring, filtering by using qualitative filter paper to obtain a straw paste leaching liquor, and determining the COD value and the TVFA content of the straw paste leaching liquor;
(3) anaerobic fermentation: carrying out anaerobic fermentation on the straw paste obtained in the step (2) by using an anaerobic fermentation device shown in figure 1, wherein the device comprises a fermentation bottle with a sealing cover 2, a sampling port 1 and an air outlet 5 are arranged on the fermentation bottle, and the air outlet 5 is connected with an air collecting bag 6; the sealing cover 2 is connected with a stirring paddle 4, and the stirring paddle 4 is driven to rotate by being connected with a stirring motor arranged outside the sealing cover 2; continuously stirring in the fermentation process;
adjusting the pH value of the corn straw paste obtained in the step (2) to 7 by using a dilute HCl solution, putting the straw paste (the total weight is 165g) with the dry matter mass of 16g into a fermentation bottle, adding 200mL of fresh biogas slurry, and adding 40mL of distilled water; hermetically fermenting for 14 days at 37 +/-1 ℃, and collecting biogas generated by fermentation in a gas collection bag;
measuring indexes such as methane quantity, methane content in methane, pH value of fermentation liquor and the like every day in the fermentation process; and (3) after the anaerobic fermentation is finished, discharging and standing for 24h, after solid-liquid separation, measuring the pH value, the COD value and the TVFA content in the biogas slurry, and measuring the weight of dry substances in the biogas residues.
Example 2
A method for producing biogas by fermenting mild, moist and hot pretreated straws comprises the following steps:
(1) crushing straws: carrying out hot air drying on the corn straws until the moisture content is below 0.5 wt%; crushing the dried corn straws into particles of 3-5 mm to obtain crushed straws;
(2) pretreatment: mixing the crushed straws obtained in the step (1) with CaO with the concentration of 1.5 wt%2Mixing the solutions, and filling into a conical flask; crushing straw and CaO2The mass ratio of the solution is 1: 15; placing the conical flask in a water bath kettle at 85 ℃ for treatment for 20h, filtering, and discarding filtrate to obtain straw paste;
determining the contents of lignin, cellulose and hemicellulose in the straw paste;
diluting the straw paste to 10 times of the original mass by using distilled water, uniformly stirring, filtering by using qualitative filter paper to obtain a straw paste leaching liquor, and determining the COD value and the TVFA content of the straw paste leaching liquor;
(3) anaerobic fermentation: anaerobic fermentation is carried out on the straw paste obtained in the step (2) by using an anaerobic fermentation device as shown in figure 1; the apparatus is described as in example 1; continuously stirring in the fermentation process;
adjusting the pH value of the corn straw paste obtained in the step (2) to 6.8 by using a dilute HCL solution, putting the straw paste (the total weight is 162g) with the dry matter mass of 16g into a fermentation bottle, adding 240mL of fresh biogas slurry, and adding 80mL of distilled water; fermenting at 32 + -1 deg.C for 12 days in a sealed condition, and collecting the biogas generated by fermentation in a gas collecting bag;
measuring indexes such as methane quantity, methane content in methane, pH value of fermentation liquor and the like every day in the fermentation process; and (3) after the anaerobic fermentation is finished, discharging and standing for 24h, after solid-liquid separation, measuring the pH value, the COD value and the TVFA content in the biogas slurry, and measuring the weight of dry substances in the biogas residues.
Example 3
A method for producing biogas by fermenting mild, moist and hot pretreated straws comprises the following steps:
(1) crushing straws: carrying out hot air drying on the corn straws until the moisture content is below 0.5 wt%; crushing the dried corn straws into particles of 3-5 mm to obtain crushed straws;
(2) pretreatment: mixing the crushed straws obtained in the step (1) with CaO with the concentration of 2.5 wt%2Mixing the solutions, and filling into a conical flask; crushing straw and CaO2The mass ratio of the solution is 1: 10; placing the conical flask in a 75 ℃ water bath pot for treatment for 16h, filtering, and discarding filtrate to obtain straw paste;
determining the contents of lignin, cellulose and hemicellulose in the straw paste;
diluting the straw paste to 10 times of the original mass by using distilled water, uniformly stirring, filtering by using qualitative filter paper to obtain a straw paste leaching liquor, and determining the COD value and the TVFA content of the straw paste leaching liquor;
(3) anaerobic fermentation: anaerobic fermentation is carried out on the straw paste obtained in the step (2) by using an anaerobic fermentation device as shown in figure 1; the apparatus is described as in example 1; continuously stirring in the fermentation process;
adjusting the pH value of the corn straw paste obtained in the step (2) to 7 by using a dilute HCl solution, putting the straw paste (the total weight of 178g) with the dry matter mass of 16g into a fermentation bottle, adding 180mL of fresh biogas slurry, and adding 60mL of distilled water; fermenting at 37 + -1 deg.C for 20 days in a sealed condition, and collecting the biogas generated by fermentation in a gas collecting bag;
measuring indexes such as methane quantity, methane content in methane, pH value of fermentation liquor and the like every day in the fermentation process; and (3) after the anaerobic fermentation is finished, discharging and standing for 24h, after solid-liquid separation, measuring the pH value, the COD value and the TVFA content in the biogas slurry, and measuring the weight of dry substances in the biogas residues.
Comparative example 1
The difference from example 1 is that CaO is added2Replacement by Na in equal mass2CO3；
The remaining technical features are the same as those of example 1.
Comparative example 2
The difference from example 1 is that CaO is added2Replacement by Na in equal mass2SO3；
The remaining technical features are the same as those of example 1.
Comparative example 3
The difference from example 1 is that CaO is added2Replacement by K2HPO4；
The remaining technical features are the same as those of example 1.
Comparative example 4
The difference from example 1 is that in step (2), the heat treatment temperature is 120 ℃ and the heat treatment is carried out at a corresponding high pressure (0.2 MPa);
the remaining technical features are the same as those of example 1.
Comparative example 5
The difference from example 1 is that CaO2The concentration of the solution was 6 wt%;
the remaining technical features are the same as those of example 1.
Comparative example 6
The difference from the example 1 is that the biogas fermentation is directly carried out without the pretreatment of the step (2);
the remaining technical features are the same as those of example 1.
Experiment 1
And (3) detecting the content of wood fiber in the straw paste after pretreatment in the step (2) of the examples 1-3 and the comparative examples 1-5 and the chemical characteristics of the straw paste leaching liquor. The results are shown in Table 2.
The COD and TVFA content of the leaching solution after the treatment of the example 1 are obviously increased, and are respectively increased by 172.65% and 201.39% compared with the comparative example 6. The results show that the pretreated cellulose and hemicellulose components are not only converted into soluble organic matters such as monosaccharide and the like, but also further converted into TVFA, so that the conversion of monosaccharide to fermentation inhibitors such as furfural and the like is reduced.
TABLE 2 lignocellulosic content of pretreated stalks and chemical Properties of the leach solution (A)
Experiment 2
The amount of biogas produced per TS of the anaerobic fermentations of examples 1-3 and comparative examples 1-6 was measured.
As can be seen from Table 3, Na2CO3、Na2SO3、K2HPO4The biogas yield can be improved to a certain extent, but the effect is not ideal; example 1 uses CaO under otherwise identical reaction conditions2As a treating agent, the effect is obviously superior to that of Na2CO3、Na2SO3、K2HPO4. The mechanism of the method is that the obstruction of fermentation is reduced, the contact area of fermentation substrates and the concentration of the available substrates in fermentation liquor are increased, so that the methane yield per TS of anaerobic fermentation after pretreatment is improved.
In addition, the invention adopts mild damp-heat treatment, and the yield of the obtained biogas is obviously superior to that of high-pressure high-heat treatment; and, high concentration of CaO2But also has obvious blocking effect on the production of the methane.
In example 1, the methane yield per unit TS is the most, which is 133.07% higher than that in comparative example 6.
TABLE 3 biogas production by anaerobic fermentation unit TS of different pretreated corn stalks
Experiment 3
The methane content in the anaerobic fermentation biogas of examples 1-3 and comparative examples 1-6 was measured.
As can be seen from Table 4, the methane content in the biogas produced after the treatment of example 1 is the largest, which is 39.02% higher than that of comparative example 6, and is significantly higher than that of comparative examples 1-5. This is probably due to CaO2Ca (OH) produced upon dissolution in water2To CO2The in-situ fixation can increase the concentration of methane in the biogas.
TABLE 4 methane content in biogas from anaerobic fermentation of different pretreated corn stalks
Experiment 4
And detecting the components of the biogas residues and the biogas slurry after anaerobic fermentation in examples 1-3 and comparative examples 1-6.
The dry basis weight loss rate of the biogas residue reflects the utilization degree of the substrate by anaerobic fermentation, and as can be seen from table 5, the dry basis weight loss rate of the biogas residue in example 1 is the highest, and is improved by 2.36 times compared with the comparative example 6. Na (Na)2CO3、Na2SO3、K2HPO4The dry basis weight loss ratio of the treated biogas residue is improved compared with the proportion 6, but the treatment effect is not as good as that of CaO2And (6) processing. The pretreatment of the mixture under mild and damp-heat conditions with alkaline non-alkali solution increases the utilization degree of the anaerobic fermentation to the substrate, improves the conversion rate of the product, and accords with the result of experiment 2.
COD and TVFA in the biogas slurry can evaluate the environmental benefit of fermentation, and the COD and TVFA content in the discharged biogas slurry after fermentation in example 1 are the lowest and are respectively reduced by 56.3% and 62.5% compared with the comparative example 6. The pretreatment promotes the utilization of the fermentation microorganisms to the soluble organic matters, and reduces the pollution treatment difficulty of the discharged biogas slurry.
TABLE 5 biogas residue and biogas slurry composition after anaerobic fermentation of different pretreated corn stalks
| Group of | Dry basis weight loss/%) | COD/mg·L-1 | TVFA/mg·L-1 |
| Example 1 | 45.16 | 3447.33 | 62.20 |
| Example 2 | 44.12 | 3398.45 | 61.89 |
| Example 3 | 45.68 | 3578.21 | 67.54 |
| Comparative example 1 | 30.71 | 6902.33 | 134.71 |
| Comparative example 2 | 34.37 | 4701.33 | 90.21 |
| Comparative example 3 | 32.82 | 4801.33 | 92.98 |
| Comparative example 4 | 43.12 | 3654.14 | 78.24 |
| Comparative example 5 | 18.11 | 8102.67 | 160.80 |
| Comparative example 6 | 19.11 | 7880.00 | 161.34 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A method for producing biogas by fermenting mild moist heat pretreatment corn straws is characterized by comprising the following steps:
(1) crushing straws: drying and crushing the straws to obtain crushed straws;
(2) pretreatment: mixing the crushed straws obtained in the step (1) with CaO2Mixing the solutions, treating at 75-85 ℃ for 12-24 h, and filtering to obtain straw paste;
(3) anaerobic fermentation: adjusting the pH value of the straw paste obtained in the step (2) to 6.8-7.3, mixing the straw paste with biogas slurry, fermenting in a closed manner for 10-30 days, and collecting biogas generated by fermentation.
2. The method according to claim 1, wherein in step (2), CaO is added2The concentration of the solution is 1.5-2.5 wt%.
3. The method according to claim 1 or 2, wherein in step (2), the straw and CaO are crushed2The mass ratio of the solution is 1: (8-15).
4. The method according to claim 1 or 2, wherein in the step (3), before the closed fermentation, water is added into the mixed liquid of the straw paste and the biogas slurry; dry matter in the straw paste: biogas slurry: the dosage ratio of water is 1 g: (10-16) mL: (2-5) mL.
5. The method according to claim 1 or 2, wherein the temperature of the fermentation in the step (3) is 30 to 40 ℃.
6. The method according to claim 1 or 2, wherein in step (3), the pH adjustment is performed using a HCL solution.
7. The method according to claim 1 or 2, wherein in the step (1), the straws are crushed into 3-5 mm particles.
8. The method according to claim 1 or 2, wherein in step (1), the moisture content of the dried straw is below 0.5 wt%.
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