CN111357868A - Method for simultaneously preparing modified biochar and liquid feed by using corn straws - Google Patents
Method for simultaneously preparing modified biochar and liquid feed by using corn straws Download PDFInfo
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- A—HUMAN NECESSITIES
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- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/10—Animal feeding-stuffs obtained by microbiological or biochemical processes
- A23K10/12—Animal feeding-stuffs obtained by microbiological or biochemical processes by fermentation of natural products, e.g. of vegetable material, animal waste material or biomass
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
- A23K10/37—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms from waste material
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
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Abstract
The invention provides a method for simultaneously preparing modified biochar and liquid feed by using corn straws. According to the invention, the corn straws are subjected to anaerobic digestion, so that nutrients such as protein, amino acid, saccharides and the like in the straws are fully utilized, and meanwhile, the biomass of the corn straws is greatly reduced, and the reduction is realized; the method utilizes in-vitro fermentation residues to prepare high-quality biochar with larger specific surface area and richer pores through one-step slow pyrolysis, and simultaneously greatly reduces the energy consumption for preparing the corn straw biochar; the liquid feed is prepared by using the in vitro fermentation filtrate, and the content of nutrient components in the liquid feed is measured, so that a new formula is provided for preparing the liquid feed with higher quality in the breeding industry.
Description
Technical Field
The invention relates to the field of agricultural waste recycling and aquaculture liquid feed preparation, in particular to a method for simultaneously preparing modified biochar and liquid feed by using corn straws.
Background
The biological modification of the biochar is to utilize a biological pretreated biomass raw material to prepare the biochar through digestion or bacterial conversion treatment. Previous studies found that anaerobic digestion processes can alter the redox potential and pH of the feedstock, thereby increasing the pH, specific surface area, Cation Exchange Capacity (CEC), hydrophobicity, and surface negative charge of the modified biochar. The research on beet shows that the anaerobic digestion obviously improves the adsorption capacity of the digestion residue biochar to nickel and cadmium. Yao et al found that the modified biochar obtained from the digestion residue can effectively remove silver ions from aqueous solutions. These results indicate that anaerobic digestion can be used as a new modification method to prepare high-efficiency carbon-based heavy metal adsorbents. In addition, this method has other advantages such as the production of renewable bio-energy and the reduction of waste management costs. However, less research is currently being conducted on the pyrolysis process of the digestion residues, and less research is being conducted on the benefits of coupling anaerobic digestion with the pyrolysis process.
The continuous growth of crop production worldwide also produces large quantities of crop stubbles that, if not properly disposed of, can be harmful to the environment. About 9 hundred million tons of crop straw are produced in China per year, wherein the corn straw accounts for 23.3 percent. At present, the resource utilization rate of the straws in China is less than 40 percent, and the utilization amount of the straw feed only accounts for 18.8 percent of the amount of the collectable resources. Recently, a new concept of improving energy recovery of crop straws by coupling anaerobic digestion and pyrolysis processes has been proposed, but the technology cannot fully utilize nutrients such as proteins, amino acids, sugars and mineral nutrients in the crop straws. On the other hand, the production of livestock feed by anaerobic degradation of straw is a popular technology, such as the preparation of fermented liquid feed by fermenting crop straw, etc., but the disposal of fermentation residues becomes a practical problem. Therefore, the method combines the utilization technology of the biochar resources, combines the anaerobic digestion-pyrolysis process, and prepares the modified biochar and the animal liquid feed raw material by utilizing the crop straws, so that the maximization of the economic benefit and the environmental benefit of the straw resource utilization is certainly realized, but a corresponding technical means is lacked at present.
In order to improve the resource utilization rate of the corn straws, the research tries to perform in-vitro fermentation on the corn straws through rumen fluid of cattle to obtain digestion residues and digestion liquid. Wherein the digestion residues are subjected to lower limit oxygen pyrolysis at 500 ℃ to prepare modified biochar, and the physicochemical properties of the biochar are evaluated. And the digestive juice is used for preparing animal liquid feed and measuring the content of nutrient components in the liquid feed.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a modified biochar and an animal liquid feed and a method for simultaneously preparing the modified biochar and the liquid feed. In order to achieve the purpose, corn silage is subjected to in-vitro fermentation by simulated rumen fluid of cattle to obtain digestion residues and digestion liquid, the biochar is prepared by a method of slowly pyrolyzing the digestion residues, and the digestion liquid is used for preparing liquid feed. The method not only realizes the multi-stage utilization of the corn straw resource, but also provides a new formula for preparing a liquid feed with higher quality in the breeding industry.
The method for simultaneously preparing the modified biochar and the liquid feed by utilizing the corn straws comprises the following steps:
(1) preparing corn straw silage: washing fresh corn straws with distilled water for three times, cutting a corn straw sample into 2-3cm long after drying, mixing 0.5% of beer yeast, 0.2% of calcium carbonate and 0.1% of sodium chloride according to the mass percentage, keeping the water content at 65%, putting the mixture into a plastic bag, and ensiling at room temperature for 30 days to obtain corn silage.
(2) Collecting rumen fluid: the cow milk feed for collecting rumen fluid is quantitatively fed every day, and comprises the following components in percentage by mass: 30 percent of forage grass, 30 percent of corn silage, 30 percent of corn kernels and 10 percent of soybean meal, and is added with supplementary vitamins and minerals. Adopt traditional tumour stomach tube to collect rumen fluid, the rumen fluid of collecting washes with carbon dioxide, adopts four layers of gauze to filter after mixing, puts into anaerobic flask for subsequent use.
(3) Corn straw silage in vitro fermentation: 25 grams of prepared corn stover silage was weighed into 1L serum bottles, and 100mL of collected rumen fluid and 400mL of buffer solution (13.2mg L) were added to each bottle-1CaCl2.2H2O,10.0mg L- 1MnCl2.4H2O,1.0mg L-1CoCl2.6H2O,8.0mg L-1FeCl3.6H2O,0.83g L-1NH4HCO3,7.28g L- 1NaHCO3,1.97g L-1Na2HPO4.12H2O,1.29g L-1KH2PO4,0.12g L-1MgSO4,1mg L-1Resazurin, 390mgL-1Na2S), plugging the bottle mouth with a rubber plug, sealing with an aluminum bottle, and culturing in a constant-temperature shaking incubator at 39 ℃. After in vitro fermentation for 24h, corn straw silage residues and filtrate are obtained by vacuum filtration.
(4) Preparing modified biochar: washing the corn stalk silage residue with deionized water for 3 times, drying at 65 ℃ for 24h, and grinding the dried product through a 2mm sieve. The sieved powder was placed in a ceramic jar, covered with a lid and pyrolyzed in a muffle furnace (KBF11Q, shanghai, china). The pyrolysis condition is that the temperature is raised to 500 ℃ at the speed of 10 ℃/min in the nitrogen atmosphere, and the temperature is naturally reduced to the room temperature after 2 hours of pyrolysis. The fired charcoal was removed, ground and passed through a 0.5 mm sieve.
(5) Preparing liquid feed: mixing the filtrate with dry feed according to the mass ratio of 4:1, wherein the dry feed comprises 10% of barley, 75% of corn, 10% of soybean meal and 5% of fat by mass; fermented Liquid Feed (FLF) was prepared in a 1L fermentation flask. Stirring at 20 deg.C for 4 days, and stirring for 5 min per hour to allow the mixture to naturally ferment without adding leaven.
By means of the scheme, the invention has the following advantages: (1) according to the invention, the corn straws are subjected to anaerobic digestion, so that nutrients such as protein, amino acid, saccharides and the like in the straws are fully utilized, and meanwhile, the biomass of the corn straws is greatly reduced, and the reduction is realized; (2) the method utilizes the in vitro fermentation product (corn silage digestion residue) to prepare high-quality biochar with larger specific surface area and richer pores by one-step slow pyrolysis, and simultaneously greatly reduces the energy consumption for preparing the biochar from the corn straws; (3) the liquid feed is prepared by in vitro fermentation, and the content of the nutrient components in the liquid feed is measured, so that a new formula is provided for preparing the liquid feed with higher quality in the breeding industry.
Drawings
FIG. 1 is a scanning electron microscope image of biochar (CB) prepared by comparative example corn stalks at 500 ℃;
FIG. 2 is a scanning electron microscope image of biochar (BCB24) prepared from residue after anaerobic digestion of corn stover for 24h at 500 ℃ in example 1;
FIG. 3 is a schematic flow chart of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Comparative example
Meanwhile, taking fresh corn straws, cutting the fresh corn straws into small sections with the size of 2-3cm, air-drying for 1 week, drying for 24 hours at 65 ℃, then putting the corn straws into a muffle furnace, and preparing the biochar by adopting a one-step method for slow pyrolysis. The pyrolysis condition is that the temperature is raised to 500 ℃ at the speed of 10 ℃/min in the nitrogen atmosphere, and the temperature is naturally reduced to the room temperature after 2 hours of pyrolysis. The fired charcoal was removed, ground and passed through a 0.5 mm sieve.
The technical flow adopted in the following embodiment is shown in fig. 3.
Example 1
(1) Preparing corn straw silage: washing fresh corn stalks with distilled water for three times, drying, cutting corn stalk samples into 2-3cm long, mixing 0.5% of beer yeast, 0.2% of calcium carbonate, 0.1% of sodium chloride and keeping the water content at 65%, putting the mixture into a plastic bag, and ensiling at room temperature for 30 days to obtain corn silage.
(2) Collecting rumen fluid: daily ration feeding of cows for collection of rumen fluid: 30 percent of forage grass, 30 percent of corn stalk silage, 30 percent of corn kernels and 10 percent of soybean meal, and is added with supplementary vitamins and minerals. Adopt traditional tumour stomach tube to collect rumen fluid, the rumen fluid of collecting washes with carbon dioxide, adopts four layers of gauze to filter after mixing, puts into anaerobic flask for subsequent use.
(3) Corn straw silage in vitro fermentation: 25 grams of prepared corn stover silage was weighed into 1L serum bottles, and 100mL of collected rumen fluid and 400mL of buffer solution (13.2mg L) were added to each bottle-1CaCl2.2H2O,10.0mg L- 1MnCl2.4H2O,1.0mg L-1CoCl2.6H2O,8.0mg L-1FeCl3.6H2O,0.83g L-1NH4HCO3,7.28g L- 1NaHCO3,1.97g L-1Na2HPO4.12H2O,1.29g L-1KH2PO4,0.12g L-1MgSO4,1mg L-1Resazurin, 390mgL-1Na2S), plugging the bottle mouth with a rubber plug, sealing with an aluminum bottle, and culturing in a constant-temperature shaking incubator at 39 DEG C. After in vitro fermentation for 24h, corn straw silage residues and filtrate are obtained by vacuum filtration.
(4) Preparing modified biochar: washing corn silage residue with deionized water for 3 times, drying at 65 deg.C for 24 hr, drying, and grinding with 2mm sieve. The sieved powder was placed in a ceramic jar, covered with a lid and pyrolyzed in a muffle furnace (KBF11Q, shanghai, china). The pyrolysis condition is that the temperature is raised to 500 ℃ at the speed of 10 ℃/min in the nitrogen atmosphere, and the temperature is naturally reduced to the room temperature after 2 hours of pyrolysis. The fired charcoal was removed, ground and passed through a 0.5 mm sieve.
(5) Basic physicochemical properties of the biochar: the pH, ash content, elemental composition and BET specific surface area of the biochar product were determined and the data are shown in Table 1. Meanwhile, the morphology characteristics of the biochar are analyzed by adopting a scanning electron microscope, and the result is shown in figures 1 and 2.
As can be seen from Table 1, under the condition of 500 ℃, the ash content and the specific surface area of the biochar after the anaerobic digestion of the corn straws are obviously increased, wherein the ash content is increased by 62.9 percent, and the specific surface area is improved by 3.0 times. Meanwhile, as can be seen from fig. 1 and 2, the corn stalk biochar has smooth surface and less porous structures in comparison example, and the surface porous structures of the corn stalk biochar after anaerobic digestion are obviously increased and arranged in order, so that the specific surface area is obviously increased.
TABLE 1 comparative examples the basic physicochemical properties of corn stover biochar and anaerobically digested corn stover biochar
Example 2
(1) Preparing corn straw silage: washing fresh corn stalks with distilled water for three times, drying, cutting corn stalk samples into 2-3cm long, mixing 1.5% of beer yeast, 0.1% of calcium carbonate, 0.2% of sodium chloride and keeping the water content at 65%, putting the mixture into a plastic bag, and ensiling at room temperature for 30 days to obtain corn silage.
(2) Collecting rumen fluid: daily ration feeding of cows for collection of rumen fluid: 30 percent of forage grass, 30 percent of corn stalk silage, 30 percent of corn kernels and 10 percent of soybean meal, and is added with supplementary vitamins and minerals. Adopt traditional tumour stomach tube to collect rumen fluid, the rumen fluid of collecting washes with carbon dioxide, adopts four layers of gauze to filter after mixing, puts into anaerobic flask for subsequent use.
(3) Corn straw silage in vitro fermentation: 25g of prepared corn silage are weighed into 1L serum bottles, and 100mL of the collected rumen fluid and 400mL of buffer solution (13.2mg L) are added to each bottle-1CaCl2.2H2O,10.0mg L- 1MnCl2.4H2O,1.0mg L-1CoCl2.6H2O,8.0mg L-1FeCl3.6H2O,0.83g L-1NH4HCO3,7.28g L- 1NaHCO3,1.97g L-1Na2HPO4.12H2O,1.29g L-1KH2PO4,0.12g L-1MgSO4,1mg L-1Resazurin, 390mgL-1Na2S), plugging the bottle mouth with a rubber plug, sealing with an aluminum bottle, and culturing in a constant-temperature shaking incubator at 39 ℃. After in vitro fermentation for 24h, corn straw silage residues and filtrate are obtained by vacuum filtration.
(4) Corn straw, corn straw silage, and the determination of the nutrient content of corn straw silage residues: and (2) determining the dry matter (DW) content of corn straws, corn straw silage (obtained in the step (1)), and corn straw silage residues (obtained in the step (3)) by heating for 48 hours at 65 ℃ through microwaves, and respectively determining the content of Organic Matters (OM), Crude Proteins (CP), Neutral Detergent Fibers (NDF), Acid Detergent Fibers (ADF) and Acid Detergent Lignin (ADL) after a heated sample passes through a 1.0mm sieve, wherein the specific results are shown in a table 2.
As can be seen from Table 2, after 30d of ensiling, compared with corn stalks, the CP content in the corn stalk ensiling is obviously increased (p <0.05), and the OM, NDF and ADF content are obviously reduced (p < 0.05). Researches show that the fiber can lock dietary nutrients and prevent the dietary nutrients from being digested and utilized, and table 2 shows that the silage can improve the nutrient content of the corn straws, improve the protein content and reduce the fiber content. The change of the chemical components has the function of promoting the in vitro fermentation of the feed. Generally, high fiber content resulted in decreased feed degradability, and in this study, corn stover silage was fermented in vitro for 24 hours with significant decreases in OM, CP, NDF, ADF, and ADL content, and the degradability of these nutrients, except ADL, was no less than 50%.
TABLE 2 nutrient content of corn stover, corn stover silage residue
Data were calculated using corn silage dry matter.
Example 3
(1) Preparing corn straw silage: washing fresh corn stalks with distilled water for three times, drying, cutting corn stalk samples into 2-3cm long, mixing 1.0% of beer yeast, 0.3% of calcium carbonate, 0.1% of sodium chloride and keeping the water content at 65%, putting the mixture into a plastic bag, and ensiling at room temperature for 30 days to obtain corn silage.
(2) Collecting rumen fluid: daily ration feeding of cows for collection of rumen fluid: 30 percent of forage grass, 30 percent of corn stalk silage, 30 percent of corn kernels and 10 percent of soybean meal, and is added with supplementary vitamins and minerals. Adopt traditional tumour stomach tube to collect rumen fluid, the rumen fluid of collecting washes with carbon dioxide, adopts four layers of gauze to filter after mixing, puts into anaerobic flask for subsequent use.
(3) Corn straw silage in vitro fermentation: 25g of prepared corn silage are weighed into 1L serum bottles, and 100mL of the collected rumen fluid and 400mL of buffer solution (13.2mg L) are added to each bottle-1CaCl2.2H2O,10.0mg L- 1MnCl2.4H2O,1.0mg L-1CoCl2.6H2O,8.0mg L-1FeCl3.6H2O,0.83g L-1NH4HCO3,7.28g L- 1NaHCO3,1.97g L-1Na2HPO4.12H2O,1.29g L-1KH2PO4,0.12g L-1MgSO4,1mg L-1Resazurin, 390mgL-1Na2S), plugging the bottle mouth with a rubber plug, sealing with an aluminum bottle, and culturing in a constant-temperature shaking incubator at 39 ℃. After in vitro fermentation is carried out for 24h, filtrate and corn straw silage residues are obtained by vacuum filtration.
(4) Preparation of Fermented Liquid Feed (FLF): the filtrate was mixed with dry feed (10% barley, 75% corn, 10% soybean meal, 5% fat) at a ratio of 4:1 to prepare FLF in a 1L fermentation flask. The mixture was allowed to ferment spontaneously (without addition of starter) with stirring at 20 ℃ for 4 days (5 minutes per hour).
(5) Characteristics and nutritional ingredients of the filtrate and FLF: the dry matter content, pH, lactic acid bacteria count, lactic acid content, acetic acid content, ethanol content and crude protein content of the filtrate (obtained from step (3)) and FLF (obtained from step (4)) were determined and the specific results are shown in table 3.
TABLE 3 nutrient composition of the filtrate after in vitro fermentation and of the liquid feed (FLF) obtained
aFLF standards refer to Beal et al 2002, Canibe et al 2012, and van Winsen et al 2012.
Table 3 shows the dry matter content of FLF (240.5g kg)-1) Compared with the filtrate, the amount of the filtrate is obviously increased. FLF (4.3) had a significantly lower pH than the filtrate (6.2) because the filtrate after fermentation promoted lactic acid bacteria (9.1log cfu mL)-1) The growth of (2) produces more lactic acid, acetic acid and ethanol, lowering the pH of the mixture. After the dry feed is added, the content of the middle crude protein in the FLF is obviously increased (P)<0.05). And the indexes of all nutrient components of the prepared FLF all meet the standard of animal liquid feed.
Claims (9)
1. A method for simultaneously preparing modified biochar and liquid feed by using corn straws is characterized in that fresh corn straws are subjected to ensiling and bovine rumen liquid external fermentation to obtain digestion residues and digestion liquid, the biochar is prepared by a slow pyrolysis digestion residue method, and the digestion liquid is used for preparing animal liquid feed.
2. The method for preparing modified biochar and liquid feed simultaneously by using corn stalks as claimed in claim 1, wherein the method comprises the following steps:
(1) preparing corn straw silage: drying fresh corn straws, cutting into small sections with uniform size, adding silage ingredients, keeping the water content at 65%, putting the small sections into a plastic bag, and performing silage for 30 days at room temperature to obtain corn silage;
(2) collecting rumen fluid: washing the collected cow rumen fluid with carbon dioxide, mixing, filtering with four layers of gauze, and placing into an oxygen-free flask for later use;
(3) corn straw silage in vitro fermentation: adding rumen fluid and buffer solution into corn straw silage, sealing, and performing constant-temperature shake culture; after in vitro fermentation for a certain time, vacuum filtration is utilized to obtain corn straw silage residues and filtrate;
(4) preparing modified biochar: washing the corn straw silage residues with deionized water, drying, grinding and sieving; placing the sieved powder into a muffle furnace, preparing biochar by slow pyrolysis under the anoxic condition by adopting a one-step method, and grinding and sieving the biochar prepared by pyrolysis;
(5) preparing liquid feed: mixing the filtrate with dry feed in a certain proportion, and preparing fermented liquid feed in a fermentation container.
3. The method for simultaneously preparing the modified biochar and the liquid feed by utilizing the corn stalks according to the claim 2, wherein the silage ingredients in the step (1) comprise the following components in percentage by mass: 0.5-1.5% of beer yeast, 0.1-0.3% of calcium carbonate and 0.1-0.2% of sodium chloride.
4. The method for simultaneously preparing modified biochar and liquid feed by using corn stalks as claimed in claim 2, wherein the dairy cows for collecting rumen fluid in the step (2) are fed quantitatively every day, and the feed components are configured according to the following percentages: 30% forage grass, 30% corn silage, 30% corn kernels and 10% soybean meal; and adding supplementary vitamins and minerals.
5. The method for simultaneously preparing the modified biochar and the liquid feed by utilizing the corn stalks as claimed in claim 2, is characterized in that: in the step (3), 25g of prepared corn straw silage is weighed and poured into 1L of serum bottles, and then 100mL of collected rumen fluid and 400mL of buffer solution are added into each bottle, wherein the buffer solution comprises the following components: 13.2mg L-1CaCl2.2H2O,10.0mg L-1MnCl2.4H2O,1.0mg L-1CoCl2.6H2O,8.0mg L-1FeCl3.6H2O,0.83g L-1NH4HCO3,7.28g L-1NaHCO3,1.97g L-1Na2HPO4.12H2O,1.29g L-1KH2PO4,0.12g L-1MgSO4,1mg L-1Resazurin, 390mg L-1Na2S。
6. The method for simultaneously preparing modified biochar and liquid feed by using corn stalks according to claim 2, wherein the deionized water in the step (4) is washed 3 times, dried for 24 hours at 65 ℃, and ground through a 2mm sieve after drying; the one-step pyrolysis condition is that the temperature is raised to 500 ℃ at the speed of 10 ℃/min in the nitrogen atmosphere, and the temperature is naturally reduced to the room temperature after 2 hours of pyrolysis.
7. The method for simultaneously preparing modified biochar and liquid feed by using corn stalks as claimed in claim 2, wherein the dry feed in the step (5) comprises 10% of barley, 75% of corn, 10% of soybean meal and 5% of fat by mass, and the fermented liquid feed is prepared by stirring for 4 days at a temperature of 20 ℃ and for 5 minutes per hour to allow the mixture to naturally ferment.
8. A modified biochar characterized by being prepared by the preparation method of any one of claims 1 to 6.
9. A liquid feed produced by the production method according to any one of claims 1 to 7.
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