CN115433742B - Method for co-producing biogas and organic fertilizer from agricultural and forestry residues through solid anaerobic fermentation - Google Patents

Method for co-producing biogas and organic fertilizer from agricultural and forestry residues through solid anaerobic fermentation Download PDF

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CN115433742B
CN115433742B CN202210965569.6A CN202210965569A CN115433742B CN 115433742 B CN115433742 B CN 115433742B CN 202210965569 A CN202210965569 A CN 202210965569A CN 115433742 B CN115433742 B CN 115433742B
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蒋剑春
解静聪
赵剑
徐浩
王奎
张宁
杨静
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Abstract

The invention belongs to the technical field of environmental protection in the field of solid waste recycling and energy conservation, and particularly relates to a method for co-producing biogas and organic fertilizer from agricultural and forestry residues through solid anaerobic fermentation. The invention provides a method for co-producing biogas and organic fertilizer by solid anaerobic fermentation of agriculture and forestry residues, which comprises the following steps: after the agriculture and forestry residues are treated by alkali liquor, solid products and alkali treatment waste liquor are obtained; and mixing the solid product, livestock manure and the inoculant, and performing solid anaerobic fermentation to obtain biogas and an organic fertilizer. And the alkali treatment waste liquid is mixed with ethanol to obtain hemicellulose. According to the technical scheme, biogas, organic fertilizer and hemicellulose can be obtained, the problems that a biomass anaerobic fermentation system is low in initial solid content and waste water is more and difficult to treat after fermentation is finished are solved, and high-value utilization of agriculture and forestry residues is realized.

Description

Method for co-producing biogas and organic fertilizer from agricultural and forestry residues through solid anaerobic fermentation
Technical Field
The invention belongs to the technical field of environmental protection in the field of solid waste recycling and energy conservation, and particularly relates to a method for co-producing biogas and organic fertilizer from agricultural and forestry residues through solid anaerobic fermentation.
Background
The method is characterized in that the method is a large country of energy consumption, conventional fossil energy is accelerated to be exhausted along with the increasing progress of human society, and a large amount of greenhouse gases are discharged after the fossil energy is combusted, so that the global climate warming problem is increased, and the global ecological environment safety is endangered. The resources of agricultural and forestry waste in China are huge, the annual average agricultural waste yield can reach 9.7 hundred million tons in 2015 to 2019, and the forestry remainder including urban garden branches and wood processing waste in China can reach 2.4 hundred million tons in 2019. Anaerobic fermentation is the main means of harmless recycling treatment of agricultural and forestry residues in China at present except for improper treatment methods such as landfill, returning to fields and incineration.
However, the initial solid content of the conventional wet anaerobic fermentation is mostly between 2% and 8%, the fermentation gas yield and the methane yield are more, the residual wastewater after the fermentation is over is large and is difficult to directly use, the local environment and the ecological system are destroyed by random discharge, and the production cost is increased by innocent treatment, so that the method becomes a bottleneck for restricting popularization and application of anaerobic fermentation treatment of agriculture and forestry residues. Therefore, the research of anaerobic fermentation of agriculture and forestry residues is enhanced, the problems that waste water is more and difficult to treat after the anaerobic fermentation of biomass is finished are solved, the fermentation gas yield and the methane yield are ensured, and the realization of high-value utilization of agriculture and forestry residues is particularly important.
Disclosure of Invention
In view of the above, the invention provides a method for co-producing biogas and organic fertilizer by solid anaerobic fermentation of agriculture and forestry residues, which realizes anaerobic fermentation of agriculture and forestry residues with high initial solid content, can obtain biogas, organic fertilizer and hemicellulose simultaneously, achieves similar gas yield and methane yield with conventional wet anaerobic fermentation (the initial solid content is mostly 2% -8%), but has no redundant waste water after fermentation, and solves the problems of low initial solid content of a biomass anaerobic fermentation system, and more and difficult treatment of waste water after fermentation.
In order to solve the problems, the invention provides the following technical scheme:
the invention provides a method for co-producing biogas and organic fertilizer by solid anaerobic fermentation of agriculture and forestry residues, which comprises the following steps: alkali liquor treatment is carried out on agriculture and forestry residues to obtain a solid product; carrying out solid anaerobic fermentation on the solid product and livestock manure to obtain biogas and organic fertilizer; the initial solid content of the solid anaerobic fermentation is 45% -55%;
the initial carbon-nitrogen ratio of the solid anaerobic fermentation is 20:1-45:1.
Preferably, the lye comprises NaOH solution; the mass fraction of NaOH is 1-4% when NaOH solution is alkali treated, the temperature is 60-100 ℃ and the time is 1-24 h;
the rotating speed of the alkali treatment of the NaOH solution is 100-180 rpm.
Preferably, the alkali liquor treatment also obtains alkali treatment waste liquor, and the alkali treatment waste liquor is subjected to precipitation treatment to obtain the hemicellulose.
Preferably, ethanol is added during the precipitation treatment, and the mass fraction of ethanol in the solution after the alkali treatment waste liquid is mixed with the ethanol is 60% -95%.
Preferably, the solid state anaerobic fermentation further comprises adding an inoculum, the inoculum being activated sludge.
Preferably, the temperature of the solid anaerobic fermentation is 25-45 ℃, and the solid anaerobic fermentation is carried out until no gas is produced.
Preferably, the livestock manure comprises one or more of pig manure, sheep manure and cow manure.
The invention has the beneficial effects that: the invention provides a method for co-producing biogas and organic fertilizer by solid anaerobic fermentation of agriculture and forestry residues, which comprises the following steps: alkali liquor treatment is carried out on agriculture and forestry residues to obtain a solid product; carrying out solid anaerobic fermentation on the solid product and livestock manure to obtain biogas and organic fertilizer; the initial solid content of the solid anaerobic fermentation is 45% -55%; the initial carbon-nitrogen ratio of the solid anaerobic fermentation is 20:1-45:1. The initial solid content of the conventional wet anaerobic fermentation is mostly between 2% and 8%, the fermentation gas yield and methane yield are more, but the residual wastewater after the fermentation is finished is large, and after the solid content is improved, the fermentation gas yield and methane yield are reduced. The lignin in agriculture and forestry residues is effectively removed through alkali liquor treatment, and accessibility of microorganisms and biological enzymes secreted by the microorganisms to biomass is improved. Meanwhile, the initial solid content of the solid anaerobic fermentation is 45% -55%, the solid content is high, the solid anaerobic fermentation is guaranteed to have good stability and gas production efficiency through alkali liquor treatment and initial carbon nitrogen ratio adjustment, biogas can be obtained after the solid anaerobic fermentation, the water content in the initial stage of the solid anaerobic fermentation reaction is low, the product is agglomerated without dripping after the anaerobic fermentation is finished, redundant waste water is avoided after the fermentation, biogas residues can be comprehensively utilized as organic fertilizers, the problem that the waste water is more and difficult to treat after the conventional wet anaerobic fermentation is solved, and high-value biogas and organic fertilizers are obtained. Therefore, the technical scheme provided by the invention can solve the problems of low initial solid content of a biomass anaerobic fermentation system, more waste water and difficult treatment after fermentation is finished, and realize high-value utilization of agriculture and forestry residues.
Drawings
The drawings in the following description are only examples of embodiments of the present invention and other drawings may be made from these drawings by those of ordinary skill in the art without inventive faculty.
FIG. 1 is a schematic diagram of a real-time monitoring device for gas production and methane production used in the present invention; wherein 1 is a feed supplement port, 2 is a valve, 3 is a stirring motor, 4 is a sealed fermentation bottle, 5 is a water bath heat preservation device, 6 is a gas flow precision detector, and 7 is CO 2 Absorption device (containing 3M NaOH aqueous solution or CO) 2 Absorbent), 8 is a gas flow precision detector, 9 is a gas outlet/gas collecting port, and methane gas can be collected;
FIG. 2 is a graph showing the total biogas production and the total methane production of the solid anaerobic fermentation reaction system in each time point of examples 1 to 3 and comparative examples 1 to 2; wherein a is comparative example 1, b is example 2, c is example 1, d is example 3,e is comparative example 2;
FIG. 3 is a process flow chart of the technical scheme of the invention.
Detailed Description
The invention provides a method for co-producing biogas and organic fertilizer by solid anaerobic fermentation of agriculture and forestry residues, which comprises the following steps: alkali liquor treatment is carried out on agriculture and forestry residues to obtain a solid product; carrying out solid anaerobic fermentation on the solid product and livestock manure to obtain biogas and organic fertilizer; the initial solid content of the solid anaerobic fermentation is 45% -55%;
the initial carbon-nitrogen ratio of the solid anaerobic fermentation is 20:1-45:1.
The invention carries out alkali liquor treatment on agriculture and forestry residues to obtain a solid product. Before the alkali liquor treatment, the invention preferably carries out crushing treatment on the agriculture and forestry residues to obtain crushed agriculture and forestry residues, and the particle size of the crushed agriculture and forestry residues is preferably 22-80 meshes (0.81-0.17 mm). The pulverizing method is not particularly limited, and a conventional method may be adopted.
The agricultural residues according to the present invention may be, but are not limited to, lignocellulosic materials such as agricultural waste, forestry processing residues, and municipal garden waste, and the agricultural residues preferably include, but are not limited to, straw, rice hulls, edible fungus substrates, vinegar residues, fruit shells, and the like. In the embodiment of the invention, the agriculture and forestry residues are preferably corn stalks.
In the present invention, the alkali liquid treatment preferably includes an alkali treatment with a NaOH solution. In the present invention, the NaOH solution is used in the alkali treatment of 1 to 4% by mass, preferably 1.5 to 3% by mass, more preferably 2% by mass. The temperature of the NaOH solution in the alkali treatment of the present invention is preferably 50 to 100 ℃, more preferably 52 to 80 ℃, and even more preferably 55 ℃. The alkali treatment time of the NaOH solution of the present invention is preferably 1 to 24 hours, more preferably 1.5 to 10 hours, and still more preferably 2 to 5 hours.
In the present invention, the rotational speed of the alkali treatment of the NaOH solution is preferably 100 to 180rpm, more preferably 110 to 160rpm, and still more preferably 120rpm. In the embodiment of the invention, the alkali treatment of the NaOH solution is preferably carried out on a shaking table, and the rotating speed of the shaking table is preferably 100rpm.
In the invention, the solid-to-liquid ratio of agriculture and forestry residues to the NaOH solution is preferably 1:10 (g/mL) when the NaOH solution is subjected to alkali treatment.
The alkali liquor treatment effect is realized under the specific temperature, time and rotating speed settings. The NaOH alkali treatment is an efficient biomass pretreatment mode which is easy and convenient to operate, reduces the lignin content, effectively damages the original compact structure of the biomass of the agriculture and forestry residues, enables the wood fiber structure to be loose and porous, improves the specific surface area of the wood fiber structure, thereby improving accessibility of anaerobic microorganisms and biological enzymes secreted by the anaerobic microorganisms to materials, improving degradability of the agriculture and forestry residues, promoting gas production of subsequent solid anaerobic fermentation reactions, and improving gas production efficiency of the subsequent solid anaerobic fermentation reactions.
The concentration range of the conventional alkali in the prior art can be 2-20%, the temperature is more than 100 ℃, and the extraction time is 20 min-2 h. In order to improve the yield and reduce the extraction time, high alkali concentration is generally selected, as in the prior art (see 'Li Yahui. Alkali pre-extracted bagasse hemicellulose and the research on the influence of alkali pre-extraction on the subsequent pulping performance [ D ]. University of North China and the university of North China, 2019'), the alkali concentration of alkali pre-extraction is 40-200 g/L, and the alkali concentration is high. In the prior art (see 'Cheng Geli, zhan Huaiyu; the influence of the alkaline process on subsequent pulping [ J ]. Chinese paper-making journal, 2010 (1): 4'), the alkali concentration of the alkaline process pre-extracted cornstalk hemicellulose is 10%, and the alkali concentration is high. In addition, there are reports of additional microwave treatment during alkali treatment ("An, shen Chunyin, zhao Ling, etc.) for improving extraction efficiency of hemicellulose in lignocellulose, a microwave-alkali pre-extraction process of hemicellulose in corn straw [ J ]. University of eastern chemical university: nature science edition, 2010,36 (4): 6"). Compared with the conventional alkali treatment method, the alkali concentration of the NaOH alkali treatment method is low, the mass fraction of NaOH in the alkali treatment is 1-4%, the condition is mild, and the method has a promoting effect on the gas production performance of solid anaerobic fermentation.
After the alkali liquor treatment, the invention preferably obtains an alkali treatment solid product and an alkali treatment waste liquor through solid-liquid separation. The solid-liquid separation mode is not particularly limited and can be a conventional mode, and comprises standing layering, plate-frame filter pressing, centrifugal separation, negative pressure suction filtration, gauze filtration and the like.
In the invention, when a small amount of alkali treated corn straw products are subjected to solid-liquid separation, a gauze filtering mode can be adopted, and the mode is time-saving; when a large amount of alkali treated corn straw products are subjected to solid-liquid separation, the solid-liquid separation can also be directly performed by adopting a negative pressure suction filtration mode. The obtained alkali treatment waste liquid can be used for further removing solid particles by a negative pressure suction filtration mode before hemicellulose is recovered.
In the embodiment of the invention, the separation is preferably performed by adopting a gauze filtering mode, medical gauze with proper size is selected, 3-5 layers of medical gauze are stacked for filtering to obtain a solid product, more preferably, medical gauze with proper size is selected, and 4 layers of medical gauze are stacked for filtering to obtain a solid product.
In the embodiment of the invention, in order to remove solid particles remained in the alkali treatment waste liquid, before the hemicellulose is recovered, the alkali treatment liquid is subjected to solid-liquid separation, the separation preferably adopts a negative pressure suction filtration mode, the vacuum degree of the negative pressure suction filtration is-0.09 MPa, and common qualitative filter paper is selected.
After the solid product is obtained, the solid product and the livestock manure are subjected to solid anaerobic fermentation to obtain the biogas and the organic fertilizer. In the present invention, the livestock manure preferably includes one or more of pig manure, sheep manure and cow manure. The livestock manure according to the invention is preferably dry livestock manure. The source of the livestock manure is not particularly limited, and the livestock manure is prepared from conventional products.
The invention preferably mixes the solid product with the livestock manure and then inoculates the inoculant for solid anaerobic fermentation. The inoculant of the present invention is preferably activated sludge. The source of the activated sludge is not particularly limited, and the activated sludge can be obtained by adopting a conventional commercial product.
Microorganisms in the activated sludge according to the present invention include, but are not limited to, one or more of clostridium ruminalis (ruminicola), ruminococcus (ruminococcus) and linear bacillus ruminolyticus (ruminobacter), campylobacter (Syntrophobacter), campylomonas (Syntrophomonas), methanobacterium (methanobacterium) and methanothrix (methanothrix). In an embodiment of the invention, the activated sludge is taken from Shandong Libo source environmental materials company.
In the present invention, the mass ratio of the solid product, the livestock manure and the inoculum is preferably determined by the initial carbon to nitrogen ratio of the solid product, the livestock manure and the inoculum. The initial solid content of the solid anaerobic fermentation is 45% -55%, and the solid content refers to the solid content of an initial mixture obtained by mixing a solid product, livestock manure and an inoculum.
The mass ratio of the solid product, the livestock manure and the inoculant is determined according to the carbon-nitrogen ratio of the solid product, the livestock manure and the inoculant and by adjusting the initial carbon-nitrogen ratio of the solid anaerobic fermentation to be 20:1-45:1.
In the present invention, the initial carbon to nitrogen ratio of the solid anaerobic fermentation is 20:1 to 45:1, preferably 20:1 to 35:1, more preferably 20:1, 21:1, 22:1, 23:1, 24:1, 25:1, 26:1 and 27:1. The initial carbon-nitrogen ratio of the solid anaerobic fermentation is kept in the interval of 20:1-45:1. The carbon-nitrogen ratio can adjust and improve the nutrition structure of an anaerobic fermentation system of agriculture and forestry residues, so that the anaerobic fermentation system, especially a solid anaerobic fermentation system with low water content, is optimized, and biogas and organic fertilizer are obtained.
In the present invention, the temperature of the solid anaerobic fermentation is preferably 25℃to 45℃and more preferably 30℃to 40℃and still more preferably 37 ℃. In the invention, the solid anaerobic fermentation is preferably carried out until no gas is produced, and the solid anaerobic fermentation is carried out until no gas is produced. In the embodiment of the invention, the time of the solid anaerobic fermentation is preferably 14d.
The solid anaerobic fermentation device is not particularly limited, and a conventional device is adopted. The solid anaerobic fermentation device is preferably a fermentation bottle with a volume of 1L and a stirring function, and is used for detecting the gas yield and the methane yield in real time, and is not a necessary device in the scheme.
After the agriculture and forestry residues are subjected to alkali treatment, alkali treatment waste liquid is preferably obtained. The invention preferably carries out precipitation treatment on the alkali treatment waste liquid to obtain hemicellulose, thereby realizing the co-production of methane, organic fertilizer and hemicellulose. In the invention, the alkali treatment waste liquid and the ethanol are preferably mixed for precipitation treatment; the mass fraction of ethanol in the mixed solution of the alkali treatment waste liquid and ethanol is preferably 60% -95%, more preferably 70% -90%, and even more preferably 85%. The invention can improve the yield of hemicellulose by adjusting the mass fraction of ethanol in the precipitation treatment.
In the present invention, the alkali-treated waste liquid is preferably subjected to a impurity removal treatment before being subjected to a precipitation treatment. The impurity removal treatment mode is not particularly limited, and a conventional mode is adopted. In the embodiment of the invention, the impurity removal treatment is preferably carried out by adopting a buchner funnel to carry out suction filtration to remove large-particle impurities such as straw scraps, soil particles and the like.
The invention establishes a stable solid anaerobic fermentation system of agriculture and forestry residues through the adjustment of the initial carbon nitrogen ratio of the agriculture and forestry residues and anaerobic fermentation raw materials in alkaline pretreatment, and provides a clean and efficient method for co-producing methane, bio-organic fertilizer and hemicellulose by the solid anaerobic fermentation of agriculture and forestry residues.
Aiming at the problems that the existing biomass anaerobic fermentation system is low in initial solid content and more in waste water is difficult to treat after fermentation, a clean high-efficiency solid anaerobic fermentation method for agriculture and forestry residues is established by combining a mild alkali pretreatment mode and a raw material initial carbon nitrogen ratio regulation mode, the agriculture and forestry residues are treated by the method, the obtained waste liquid after pretreatment is recycled to obtain hemicellulose, solid residues are subjected to solid anaerobic fermentation to obtain biogas, no redundant waste water exists after fermentation, and biogas residues can be used as organic fertilizer comprehensively. The invention solves the problem of wastewater treatment after conventional wet anaerobic fermentation from the source and ensures the operation of a solid anaerobic fermentation system. And meanwhile, the alkali pretreatment waste liquid is subjected to precipitation treatment to obtain a hemicellulose crude product, so that the high-value utilization of agriculture and forestry residues is realized.
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
The following examples and applications were performed according to the process flow diagram shown in fig. 3.
Example 1
The grain diameter of the crushed corn straw is 20-80 meshes (0.180-0.710 mm); 100g (dry matter) of crushed corn straw is taken and placed in a 2000mL Erlenmeyer flask, and the solid-liquid ratio is 1g:10mL of NaOH solution is added and mixed, and the mass concentration of the NaOH solution is 2%. And (3) placing the triangular flask filled with the mixture of the corn straw and the NaOH solution on a shaking table, treating for 2 hours at the temperature of 50 ℃ and the rotating speed of 100 revolutions per minute, filtering out filtrate to obtain a solid product (corn straw alkali treatment residues), cleaning the solid product to be neutral, and measuring the chemical composition of the corn straw alkali treatment solid product.
Example 2
The crushed corn stalks are subjected to alkali treatment by NaOH solution, the mass concentration of the NaOH solution is 1%, and the rest conditions are the same as in example 1.
Example 3
The crushed corn stalks are subjected to alkali treatment by NaOH solution, the mass concentration of the NaOH solution is 4%, and the rest conditions are the same as in example 1.
Comparative example 1
The crushed corn stalks are not subjected to alkali treatment by NaOH solution, and the rest conditions are the same as in example 1.
Comparative example 2
The crushed corn stalks are subjected to alkali treatment by NaOH solution, the mass concentration of the NaOH solution is 10%, and the rest conditions are the same as in example 1.
Application example 1
The corn stover alkali-treated solid products obtained in examples 1 to 3 and comparative examples 1 to 2 were measured for water content, carbon-nitrogen ratio, cellulose, hemicellulose, and lignin components, and the results are shown in table 1. The cellulose, hemicellulose, lignin determination method uses the U.S. department of energy NREL to determine the standard NREL/TP-510-42618 for three-element in lignocellulosic feedstock.
TABLE 1 physicochemical index of alkali treated corn straw
Water content Carbon to nitrogen ratio Cellulose/% Hemicellulose/% Lignin/%
Comparative example 1 8.12 43:1 32.07 21.51 12.74
Example 2 5.88 46:1 35.7 17.39 13.26
Example 1 6.74 48:1 39.24 15.02 13.48
Example 3 6.56 49:1 42.21 12.04 15.19
Comparative example 2 7.12 52:1 43.03 8.89 16.85
As can be seen from Table 1, after the treatment of NaOH solution, the hemicellulose content of the corn straw is reduced, and meanwhile, the originally compact structure of the corn straw biomass is effectively destroyed, so that the wood fiber structure is loose and porous, and the specific surface area of the wood fiber structure is improved. The compact structure of the wood treated by the NaOH solution is destroyed and becomes loose, which indicates that the wood is roughened and porous, and the specific surface area is obviously increased. The contact area of the microorganism and the lignocellulose degrading enzyme secreted by the microorganism with lignocellulose is also increased, namely the accessibility of the anaerobic microorganism and the biological enzyme secreted by the anaerobic microorganism is improved, so that the degradation of corn straw is accelerated. The corn straw lignin removal rate is low under the treatment of low alkali concentration, only hemicellulose in the corn straw is largely removed, and lignin is reduced, so that the lignin proportion in the solid product is improved instead.
Application example 2
Examples 1 to 3 and comparative examples 1 to 2 were treated with NaOH solution, and then solid-liquid separation was performed by using a gauze filtration method for solid products and an alkali-treated waste liquid, and 4 pieces of ordinary medical gauze were stacked and separated.
Solid products (corn stalk alkali treated products) treated with NaOH solutions obtained in examples 1 to 3 and comparative examples 1 to 2 were subjected to solid anaerobic fermentation, and 2 parallel experiments were set. The specific experimental process is as follows:
putting solid products obtained by different treatments and dry cow dung into a fermentation bottle of a solid anaerobic reactor with the volume of 1L, mixing, adding an inoculum, and mixing the solid products obtained by alkali treatment, the dry cow dung and the activated sludge, wherein the initial carbon-nitrogen ratio is 25:1; the inoculum was activated sludge (purchased from Shandong Libo source environmental materials Co., ltd., hereinafter). Wherein the water content of the dry cow dung is 8.16%, the carbon-nitrogen ratio is 15:1, the cellulose content is 22.14%, the hemicellulose content is 27.83% and the lignin content is 10.95%. The water content of the activated sludge is 95.27%, and the carbon-nitrogen ratio is 5:1. the proportions of the components of the solid anaerobic fermentation system in the preparation of the fermentation by different treatments are shown in Table 2.
The schematic diagram of the device for monitoring the gas yield and the methane yield in real time is shown in figure 1. The fermentation bottles were placed in a thermostat water bath and subjected to solid anaerobic fermentation at 37℃for a fermentation period of 14 days with a gas flow monitoring device for real-time monitoring of total gas yield and methane yield, and the maximum value was reached after fermentation for 14 days in examples 1 to 3 and comparative examples 1 to 2, and no gas production was detected. Biogas production and methane production results after the end of the solid state anaerobic fermentation of examples 1 to 3 and comparative examples 1 to 2 are shown in Table 3 and FIG. 2. FIG. 2 is the total biogas production and total methane production of the solid anaerobic fermentation reaction system at each time point of examples 1 to 3 and comparative examples 1 to 2; where a is comparative example 1, b is example 2, c is example 1, d is example 3,e is comparative example 2.
TABLE 2 composition ratios of solid anaerobic fermentation systems
Comparative example 1 Example 1 Example 2 Example 3 Comparative example 2
Alkali-treated solid product/g 6.85 6.45 6.37 6.30 6.21
Dry cow dung/g 3.93 4.18 4.31 4.37 4.57
Activated sludge/g 2.00 2.00 2.00 2.00 2.00
Water/g 9.44 9.60 9.54 9.55 9.58
TABLE 3 Total biogas yield and Total methane yield after the end of solid anaerobic fermentation of examples 1 to 3 and comparative examples 1 to 2
Comparative example 1 Example 1 Example 2 Example 3 Comparative example 2
Biogas yield (mL) 1094.5 2451.9 1888.9 2314.8 2231.5
Methane production (mL) 628.17 1538.9 1154.0 1445.6 1371.9
Methane yield (%) 57.39 62.76 61.09 62.45 61.48
Experimental results show that the solid products obtained in the examples 1-3 and the comparative examples 1-2 can release biogas in an anaerobic fermentation system with high initial solid content, but the gas yield of the solid products obtained in the examples 1-3 and the comparative example 2 by treating the corn straw alkali with NaOH solution is obviously higher than that of the solid products obtained in the comparative example 1. From this, it can be seen that the 2% naoh pretreatment of corn stalks in example 1 achieves higher gas yield under solid anaerobic fermentation conditions.
Example 4
The solid product obtained in example 1 was taken. 4.04g of the solid product of example 1, 6.68g of dry cow dung, 2g of activated sludge and 9.50g of water are mixed for solid anaerobic fermentation. Putting the solid product and the dry cow dung into a fermentation bottle of a solid anaerobic reactor with the volume of 1L, adding an inoculum after mixing, and mixing the solid product, the dry cow dung and the activated sludge with an initial carbon-nitrogen ratio of 20:1; the inoculum is activated sludge. Wherein the water content of the dry cow dung is 8.16%, the carbon-nitrogen ratio is 15:1, the cellulose content is 22.14%, the hemicellulose content is 27.83% and the lignin content is 10.95%. The water content of the activated sludge is 95.27%, and the carbon-nitrogen ratio is 5:1.
the initial solid content of the solid anaerobic fermentation system is 45%, the fermentation bottle is placed in a constant-temperature water bath kettle, solid anaerobic fermentation is carried out at 37 ℃, the fermentation period is about 14 days, and the fermentation products biogas residues and biogas are obtained. The total methane yield and the methane yield of the biogas are monitored in real time by the device shown in fig. 1.
Example 5
The corn stalk alkali treated solid product obtained in example 1 after 2% NaOH treatment is used as a raw material, 6.37g of corn stalk alkali treated matter, 4.31g of dry cow dung, 2g of activated sludge and 9.53g of water are added, the initial carbon nitrogen ratio of the corn stalk alkali treated matter, the dry cow dung and the activated sludge after being mixed is 25:1, and the initial solid content of a fermentation system is 45%. The other conditions were the same as in example 4.
Example 6
The corn stalk alkali treated solid product obtained in example 1 after 2% NaOH treatment is used as a raw material, 7.96g of corn stalk alkali treated matter, 2.71g of dry cow dung, 2g of activated sludge and 9.57g of water are added, the initial carbon nitrogen ratio of the corn stalk alkali treated matter, the dry cow dung and the activated sludge after mixing is 30:1, and the initial solid content of a fermentation system is 45%. The other conditions were the same as in example 4.
Example 7
The corn stalk alkali treated solid product obtained in example 1 after 2% NaOH treatment is used as a raw material, 9.10g of corn stalk alkali treated matter, 1.55g of dry cow dung, 2g of activated sludge and 9.58g of water are added, the initial carbon nitrogen ratio of the corn stalk alkali treated matter, the dry cow dung and the activated sludge after being mixed is 35:1, and the initial solid content of a fermentation system is 45%. The other conditions were the same as in example 4.
Example 8
The corn stalk alkali treated solid product obtained in example 1 after 2% NaOH treatment is used as a raw material, 9.96g of corn stalk alkali treated matter, 0.67g of dry cow dung, 2g of activated sludge and 9.59g of water are added, the initial carbon nitrogen ratio of the corn stalk alkali treated matter, the dry cow dung and the activated sludge after being mixed is 40:1, and the initial solid content of a fermentation system is 45%. The other conditions were the same as in example 4.
Example 9
10.07g of corn stalk alkali treatment solid product, 0g of dry cow dung, 2g of activated sludge and 9.69g of water are added, the initial carbon-nitrogen ratio of the corn stalk alkali treatment product, the dry cow dung and the activated sludge after being mixed is 45:1, and the rest conditions are the same as in example 4.
The results of monitoring the biogas yield and methane yield of the solid anaerobic fermentations of examples 4-9 in the manner of application example 2 are shown in Table 4. As can be seen from Table 4, the biogas yield in the solid anaerobic fermentation systems of examples 4 to 9 showed a decreasing trend of fluctuation with increasing initial carbon nitrogen ratio, but the methane yield was stabilized between 59.14% and 62.78%. When the initial carbon nitrogen ratio of the solid anaerobic fermentation system is 25:1, the methane yield is slightly better than other conditions. From the results, the corn straw treated by 2% NaOH is subjected to solid anaerobic fermentation under the condition of the initial carbon nitrogen ratio of 25:1, so that higher biogas yield and methane yield can be obtained.
Table 4 examples 4 to 9 initial carbon to nitrogen ratios for comparison of biogas yield from solid anaerobic fermentation and methane yield
Example 10
And (3) carrying out suction filtration on the NaOH treatment waste liquid obtained in the embodiment 1 by using a Buchner funnel paved with qualitative filter paper under the pressure of-0.09 MPa, and removing large particle impurities such as straw scraps, soil particles and the like after suction filtration to obtain the removed NaOH treatment waste liquid.
And adding absolute ethanol into 200mL of the decontaminated NaOH treatment waste liquid until the mass fraction of the ethanol is 60%, so that hemicellulose is separated out from the solution. The precipitate was obtained after centrifugation at 5000 Xg for 10min at 4℃with a low-temperature centrifuge. The precipitate was washed with 95% aqueous ethanol to neutral pH. And (5) drying the precipitate in an oven at 65 ℃ for 2 hours to obtain a hemicellulose crude product. In addition, ethanol in the supernatant obtained after low-temperature centrifugation may be recovered by rotary evaporation.
Example 11
And adding absolute ethanol into 200mL of the decontaminated NaOH treatment waste liquid until the mass fraction of the ethanol is 65%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
Example 12
And adding absolute ethanol into 200mL of the decontaminated NaOH treatment waste liquid until the mass fraction of the ethanol is 70%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
Example 13
And adding absolute ethyl alcohol into 200mL of the impurity-removed NaOH treatment waste liquid until the mass fraction of the absolute ethyl alcohol is 75%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
Example 14
And adding absolute ethyl alcohol into 200mL of the impurity-removed NaOH treatment waste liquid until the mass fraction of the absolute ethyl alcohol is 80%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
Example 15
And adding absolute ethyl alcohol into 200mL of the impurity-removed NaOH treatment waste liquid until the mass fraction of the absolute ethyl alcohol is 85%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
Example 16
And adding absolute ethyl alcohol into 200mL of the decontaminated NaOH treatment waste liquid until the mass fraction of the absolute ethyl alcohol is 90%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
Example 17
And adding absolute ethanol into 200mL of the decontaminated NaOH treatment waste liquid until the mass fraction of the ethanol is 95%, so that hemicellulose is separated out from the solution. The other conditions were the same as in example 10.
The recovery rate of hemicellulose after ethanol treatment of the NaOH-treated waste liquid of examples 10 to 17 is shown in Table 5. As is clear from Table 5, hemicellulose having a high degree of polymerization and a small amount of lignin gradually precipitated after the increase in the ethanol concentration, and the hemicellulose recovery rate was 64.8% and the hemicellulose content in the precipitate was 56.3% in example 15 when the ethanol mass fraction was 85%.
Hemicellulose recovery (%) = (mass of hemicellulose in precipitate/mass of hemicellulose lost in alkali treated feedstock) ×100%
TABLE 5 recovery rate of hemicellulose after ethanol treatment of alkali-treated waste liquid of examples 10 to 17
Example 18
The biogas residue obtained in the example 5 is exposed to the sun for 2 to 3 hours to obtain the powdery biogas residue organic fertilizer raw material with no malodor and uniform morphology. And (3) determining indexes such as the mass fraction of total organic matters, the mass fraction of total nutrients, the heavy metal content, the pH value, the colibacillus group number, the roundworm egg mortality and the like of the dried biogas residues by referring to an organic fertilizer industry standard < NY/T525-2021 >. The results are shown in Table 6. According to Table 6, after the corn stalks are treated by the method provided by the invention, the performance index of the obtained biogas residue product reaches or is superior to the industrial standard of organic fertilizers, and the biogas residue product can be used as an organic fertilizer raw material or can be compounded with other fertilizers.
Table 6 biogas residue organic fertilizer index Performance detection
Project Index (I) Biogas residue measurement value
Mass fraction (%) ≥30 47
Total nutrient (nitrogen + phosphorus pentoxide + potassium oxide) mass fraction (%) ≥4 5.9
Heavy metal arsenic (As) content (mg/kg) ≤15 0.7
Heavy metal mercury (Hg) content (mg/kg) ≤2 ＜0.5
Heavy metal lead (Pb) content (mg/kg) ≤50 1.6
Heavy metal cadmium (Cd) content (mg/kg) ≤3 0.2
Heavy metal chromium (Cr) content (mg/kg) ≤150 2.3
pH value of 5.5-8.5 8.1
Coliform count (number/g) ≤100 Not detected
Ascariasis egg mortality (%) ≥95 100％
According to the method for preparing the solid anaerobic fermentation agriculture and forestry residues, biogas can be obtained through solid anaerobic fermentation, the initial water content of the solid anaerobic fermentation is low, the initial solid content is high by 45% -55%, filtering and dewatering are not needed for materials after fermentation is completed, the biogas residues can be used as organic fertilizers comprehensively, hemicellulose can be obtained by precipitating alkali treatment waste liquid, and the problem that the waste water is more and difficult to treat after the conventional wet anaerobic fermentation is finished is solved. The initial solid content of wet solid state fermentation is usually 2-8%, and the biogas residue in 1000g fermentation product is only 20-80 g, but the wastewater is more than 900 mL.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.

Claims (6)

1. The method for co-producing biogas and organic fertilizer by solid anaerobic fermentation of agriculture and forestry residues is characterized by comprising the following steps:
alkali liquor treatment is carried out on agriculture and forestry residues to obtain a solid product; the alkali liquor is NaOH solution; the mass fraction of NaOH is 2% when NaOH solution is subjected to alkali treatment, the temperature is 50 ℃ and the time is 2 hours; the rotating speed of the alkali treatment of the NaOH solution is 100-180 rpm;
carrying out solid anaerobic fermentation on the solid product and livestock manure to obtain biogas and organic fertilizer; the initial solid content of the solid anaerobic fermentation is 45%; the solid anaerobic fermentation further comprises adding an inoculum, wherein the inoculum is activated sludge; the livestock manure comprises one or more of pig manure, sheep manure and cow manure;
the initial carbon-nitrogen ratio of the solid anaerobic fermentation is 25:1.
2. The method according to claim 1, wherein the alkali liquor treatment further comprises an alkali treatment waste liquor, and wherein the alkali treatment waste liquor is subjected to precipitation treatment to obtain hemicellulose.
3. The method according to claim 2, wherein ethanol is added during the precipitation treatment, and the mass fraction of ethanol in the mixed solution of the alkali treatment waste liquid and the ethanol is 60% -95%.
4. The process according to claim 1, wherein the solid state anaerobic fermentation is carried out at a temperature of 37 ℃.
5. A method according to claim 3, wherein ethanol is added during the precipitation treatment, and the mass fraction of ethanol in the mixed solution of the alkali treatment waste liquid and ethanol is 75% or 80% or 85% or 90%.
6. The method of claim 1, wherein the livestock manure is dry cow manure.
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