CN113979423A - Straw-based biological composite material and preparation method thereof - Google Patents
Straw-based biological composite material and preparation method thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
The invention provides a straw-based biological composite material and a preparation method thereof. The preparation method provided by the invention comprises the steps of straw pretreatment, microbial treatment, chemical treatment and carbonization, the straws are treated into straws with proper size, the recovery of the composite material prepared in the later stage is facilitated, the proper carbon-nitrogen ratio is adjusted to be 16: 1-30: 1, and superior conditions can be provided for the propagation of microorganisms and the decomposition of the straws by controlling the water content. On the basis, aerobic fermentation is carried out by adopting microorganisms, the decomposed straw can be continuously degraded by different inorganic solution treatments, degraded substances formed in pores of the fermented straw can be well treated, the degradation rate of the straw can reach 5% -10% after the microbial fermentation and the inorganic solution treatment, and then impurities in raw materials and impurities generated in the processes of microbial treatment and chemical treatment are further cleaned by using ultrasonic waves, so that the prepared material has more pores and larger specific surface area.
Description
Technical Field
The invention belongs to the technical field of production of biological materials, and particularly relates to a straw-based biological composite material and a preparation method thereof.
Background
The straws are a general term of stems, leaves (ears) of mature crops, are main byproducts of agricultural production, account for about 50 percent of biological yield of the crops, and are a kind of renewable organic resources which are most directly utilized. With the development of intensive agricultural production, the yield of agricultural wastes represented by straws is increased sharply, and the yield is nearly 40 hundred million tons every year around the world. The quantity of crop straws in China is huge, the distribution range is large, and the annual yield of the straws can reach 9.8 hundred million tons.
The traditional straw utilization mainly comprises direct returning, burning or discarding, so that the utilization efficiency is low, and a great amount of social, economic and ecological problems such as air pollution, soil mineralization, fire accidents and the like can be caused. On the premise of not causing environmental pollution, the efficient utilization of straw resources becomes a research hotspot for realizing agricultural sustainable development.
At present, the water environment pollution of China has the characteristic of wide distribution range, rivers and lakes in all region ranges have water pollution phenomena to different degrees on the basis of the overall geographical layout, and heavy metal pollution is relatively serious in pollution. The water environment pollution can not only affect the balance of the water environment, but also threaten the life safety of human beings. In recent years, water environment pollution treatment has received more and more attention, and how to develop a material which can treat water environment pollution without causing secondary pollution has become a hotspot of research.
At present, the current situation of soil pollutionIt is very serious that toxic and harmful substances in the soil are transmitted through animals, plants, water and the atmosphere, thus harming the health of human beings and the stability of the ecological system. More than 80% of the polluted soil in China is caused by excessive heavy metals. About 1000 million hm in China2The heavy metal pollutes cultivated land, and the direct economic loss is hundreds of billions of yuan. The existing soil heavy metal pollution remediation technology mainly comprises a physical/chemical remediation technology, a biological remediation technology and an agricultural ecological remediation technology, and a great deal of research is conducted on the technologies by many scientific researchers, so that the purposes of finding substances for eliminating or reducing the heavy metal content in soil, generating no new pollutants, not destroying ecological balance and bringing better benefits are achieved.
The method for preparing the biological composite material by utilizing the agricultural wastes (straws) with rich resources can thoroughly change the traditional agriculture with resource waste, realize 'ordering grass to form gold, turning harm into benefit, changing waste into valuable, producing without waste and treating waste by waste', not only increase the value of the agricultural resources in multiple stages, but also treat water pollution and soil pollution, and open up a most effective and lasting shortcut for comprehensive development and utilization of the straw resources and pollution treatment.
Disclosure of Invention
The invention aims to provide a straw-based biological composite material and a preparation method thereof. The size, carbon-nitrogen ratio and water content of the straws are controlled by a pretreatment method, so that a more favorable fermentation environment is provided; after fermentation, chemical treatment is carried out to achieve the purpose of increasing the porosity of the material.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of a straw-based biological composite material, which comprises the following steps:
(1) straw pretreatment: cutting the dry straws into small sections of 1-3 cm, removing impurities, drying and sterilizing; spraying a nitrogen source solution on the straws to adjust the carbon-nitrogen ratio, wherein the water content of the straws is 40-70%;
(2) and (3) treating the microorganisms: spraying a microbial agent on the straws obtained in the step (1), uniformly mixing, and fermenting for 2-6 days at 28-37 ℃ to obtain decomposed straws;
(3) chemical treatment: immersing the decomposed straw in 0.5-2.0 mol/L inorganic solution, preserving heat for 1-5 h at 40-70 ℃, and then carrying out ultrasonic treatment for 15-60 min; drying after cleaning;
(4) carbonizing: and (4) keeping the temperature of the dried straws in the step (3) at 400-700 ℃ for carbonization for 30 min-12 h under the protection of micro oxygen or nitrogen, and cooling to obtain the straw-based biological composite material.
Further, the carbon-nitrogen ratio of the straw in the step (1) after adjustment is 16: 1-30: 1.
Further, the solute of the nitrogen source solution in the step (1) is at least one of urea, ammonium salt, nitrate and organic ammonia.
Further, the straw in the step (2) is yellow brown, has no odor, and is fermented at normal temperature to obtain decomposed straw.
Further, the microbial agent in the step (2) is a solid preparation with the effective viable count of more than or equal to 100 hundred million/g, and the dosage of the microbial agent is 0.5-2.0 g per kg of dry straw.
Further, the microbial agent comprises at least one of trichoderma viride, aspergillus niger, bacillus pumilus, trichoderma viride, aspergillus niger, bacillus subtilis, white rot fungi and aspergillus oryzae.
Further, the inorganic solution in the step (3) is an aqueous solution of one of hydrogen peroxide, potassium permanganate, sulfuric acid, phosphoric acid, citric acid, tartaric acid and potassium hydroxide.
Further, the drying temperature in the step (3) is 70-95 ℃.
Further, the degradation rate of the straws in the step (3) is 5-10%.
Further, the step (1) also comprises the step of drying for 1 hour at 90-110 ℃ after crushing to remove mixed bacteria.
The invention also provides the straw-based biological composite material prepared by the preparation method.
Compared with the prior art, the invention has the advantages and beneficial effects that:
in view of the urgency of agricultural waste straw treatment, water environment pollution and soil environment pollution treatment in China, how to reasonably treat waste with waste and protect the environment becomes the work key of agricultural workers. The prepared straw-based biological composite material can be applied to various environmental governments, combines agricultural waste utilization, sewage treatment and soil pollution remediation, and is low in use cost, environment-friendly, free of secondary pollution and stable in effect. The method is properly reformed according to the characteristics of sewage and polluted soil in various places, so that the method has quite wide applicability in the aspects of agricultural waste utilization, water pollution and soil pollution treatment.
(1) The invention mainly adopts the steps of biological treatment, inorganic solution treatment, ultrasonic treatment and the like which are continuous, aims to form more stable straw-based biological composite material and provide an adsorbable and more convenient-to-recycle material for water pollution treatment and soil pollution treatment.
(2) Compared with the biochar preparation treatment in the prior art, the method disclosed by the invention has the advantages that through a large number of experiments, the C/N ratio of the straws is adjusted by applying nitrogen sources such as urea and ammonium salt, and the appropriate C/N ratio after adjustment is as follows: 16: 1-30: 1, and creates more superior conditions for the propagation of microorganisms and the decomposition of straws. Particularly, inorganic materials including hydrogen peroxide, potassium permanganate, sulfuric acid, phosphoric acid, citric acid, tartaric acid, potassium hydroxide and the like are added to treat the straws, so that degradation substances formed in pores of the fermented straws can be well treated, and the prepared material has more pores and larger area.
(3) Compared with the biochar preparation treatment, the treatment process can reduce the preparation temperature through a large number of experiments, form a better pore structure, save more energy and enable the material to play a greater role in sewage treatment and polluted soil treatment.
(4) The invention focuses on realizing 'ordering grass to form gold, turning harm into benefit, changing waste into valuable, producing without waste, treating waste by waste', the whole process is green production, the degradation substance can be used as fertilizer, and the formed straw-based biological composite material can treat water pollution and heavy metal pollution.
Drawings
FIG. 1 shows the state of the straw after the pretreatment;
FIG. 2 is a state of the straw being decomposed;
FIG. 3 shows the state of the treated straw with inorganic solution;
fig. 4 is a straw-based biocomposite.
FIG. 5 is an electron microscope scanning image of the straw-based biocomposite.
Detailed Description
The following embodiments better illustrate the present invention. However, the present invention is not limited to the following examples.
Example 1
The straw adopted in the invention is gramineous crop straw, and comprises rice straw, wheat straw, corn straw and the like.
The specific preparation method of the straw-based biological composite material in the embodiment comprises the following steps:
(1) straw pretreatment: cutting 10kg dry straw into 1-3 cm small sections with a hay cutter, removing impurities, pulverizing for 1min with a pulverizer, and drying at 105 deg.C for 1 hr to remove mixed bacteria; uniformly spraying a nitrogen source solution on the straws to adjust the carbon-nitrogen ratio, wherein the water content of the straws is 50-60%; the state of the pretreated straws is shown in figure 1;
nitrogen source solution: dissolving 239g of urea in 12.2kg of water to obtain a urea solution, wherein the urea solution is suitable for adjusting the carbon-nitrogen ratio of which the ratio is more than 25; the dissolving process is a heat absorption process, and the temperature can be controlled by using methods such as dissolving with hot water or drying water after dissolving urea. But the urea can be promoted to be converted into ammonia at a too high temperature, and the bacteria are not favorable for degrading the straws; therefore, the temperature of the urea solution is less than or equal to 30 ℃.
(2) And (3) treating the microorganisms: spraying 10g of microbial inoculum on the straws, uniformly mixing, putting into a beaker, covering a preservative film, leaving small holes on the film, maintaining the degradation temperature and humidity of the straws and an aerobic environment, carrying out aerobic fermentation for 3-4 days at 32 ℃, stopping fermentation until the straws are yellow brown in color, loose and fragile, odorless and moderate in temperature, cleaning, and drying at 70-95 ℃ to obtain thoroughly decomposed straws (figure 2).
The microbial agent is aspergillus oryzae and trichoderma viride with the weight ratio of 1: 1; the effective viable count of the microbial agent is more than or equal to 100 hundred million/g.
(3) Chemical treatment: immersing the decomposed straw obtained in the step (2) in 1.0mol/L sulfuric acid solution, preserving heat for 3h at 60 ℃, putting the treated straw into an ultrasonic groove, and performing ultrasonic treatment for 30min, wherein the treated straw is in a state shown in figure 3; drying after cleaning; the measured straw degradation rate is 8.3%.
(4) Carbonizing: and (4) carbonizing the straws dried in the step (3) for 10min at 600 ℃ under the protection of nitrogen, and cooling to obtain the straw-based biological composite material (figure 4).
The nitrogen source solution can also be a nitrate solution, and any carbon-nitrogen ratio is suitable, but the nitrate nitrogen is easy to be leached by over-wetting so that the nitrogen is unevenly distributed; therefore, when nitrate solution is used as nitrogen source solution, the humidity of the straw is not more than 55%.
Example 2
The preparation method of the straw-based biological composite material in the embodiment comprises the following steps:
(1) straw pretreatment: cutting 10kg of dry straws into small sections of 1-3 cm by using a hay cutter, and removing impurities; crushing for 2min by using a crusher, uniformly spraying a nitrogen source solution on the straws to adjust the carbon-nitrogen ratio, and controlling the water content of the straws to be 50-60%;
nitrogen source solution of amino acid: 616g of amino acid powder was dissolved in 12.2kg of water to obtain an amino acid solution suitable for any carbon to nitrogen ratio.
(2) And (3) treating the microorganisms: spraying 15g of microbial inoculum on the straws, uniformly mixing, putting into a beaker, covering a preservative film, and leaving small holes on the film, so that the degradation temperature and humidity of the straws can be kept, an aerobic environment can be kept, aerobic fermentation is carried out for 3-4 days at 32 ℃, the fermentation is stopped until the straws are yellow brown in color, loose and fragile, odorless and moderate in temperature, and the straws are dried to obtain thoroughly decomposed straws;
the microbial agent is bacillus pumilus and white rot fungus with the ratio of 1: 1; the effective viable count of the microbial agent is more than or equal to 100 hundred million/g.
(3) Chemical treatment: immersing the decomposed straw obtained in the step (2) into a hydrogen peroxide solution with the mass fraction of 1% at 40 ℃ for 5h, placing the solution into an ultrasonic groove, and performing ultrasonic treatment for 45 min; after cleaning, drying, the degradation rate of the straws is determined to be 7.8%.
(4) Carbonizing: and (4) carbonizing the straws dried in the step (3) for 30min at 500 ℃ under the protection of nitrogen, and cooling to obtain the straw-based biological composite material.
Example 3
The preparation method of the straw-based biological composite material comprises the following steps:
(1) straw pretreatment: cutting 10kg of dry straws into small sections of 1-3 cm by using a hay cutter, and removing impurities; crushing for 1min by using a crusher, and uniformly spraying a nitrogen source solution on the straws to adjust the carbon-nitrogen ratio, wherein the water content of the straws is 50-60%.
Nitrogen source solution: 861g of diammonium phosphate is dissolved in 12.2kg of water to obtain a diammonium phosphate solution which is suitable for adjusting the carbon-nitrogen ratio of which the ratio is more than 20; the added phosphorus is beneficial to the degradation of the straw by the strain; the temperature of the ammonium salt solution is less than or equal to 35 ℃.
(2) And (3) treating the microorganisms: spraying 20g of microbial inoculum on the straws, uniformly mixing, putting into a beaker, covering a preservative film, and leaving small holes on the film, so that the degradation temperature and humidity of the straws can be kept, an aerobic environment can be kept, aerobic fermentation is carried out for 3-4 days at 32 ℃, the fermentation is stopped until the straws are yellow brown in color, loose and fragile, odorless and moderate in temperature, and the straws are dried to obtain thoroughly decomposed straws;
the microbial agent is bacillus pumilus, bacillus subtilis and aspergillus oryzae in a ratio of 3:3: 4; the effective viable count of the microbial agent is more than or equal to 100 hundred million/g.
(3) Chemical treatment: immersing the decomposed straw obtained in the step (2) in 2.0mol/L citric acid solution, preserving heat for 3 hours at 60 ℃, putting the straw into an ultrasonic groove, and carrying out ultrasonic treatment for 1 hour; after cleaning, drying, the degradation rate of the straws is determined to be 8.6%.
(4) Carbonizing: and (4) carbonizing the straws dried in the step (3) for 1h at the temperature of 400 ℃ under the micro-oxygen condition, and cooling to obtain the straw-based biological composite material.
The invention provides a chemical treatment method, which comprises the steps of carrying out oxidation treatment by using a hydrogen peroxide solution, carrying out acidification treatment on a sulfuric acid solution, and carrying out organic acidification treatment on a citric acid solution; the corresponding treatment can also be carried out by adopting aqueous solutions of potassium permanganate, phosphoric acid, tartaric acid and the like, and the alkalization treatment can also be carried out by adopting a potassium hydroxide solution. Different adsorption materials can be formed by different treatments to treat different pollutants, and the composite material formed by alkalization treatment and oxidation treatment can better treat heavy metal pollution.
According to the preparation method of the straw-based biological composite material, the size of the raw material is controlled through straw pretreatment, the raw material is too large and difficult to be pretreated in batch, the proper crushing degree is more favorable for fermentation, and the composite material prepared in the later period is easy to recover. The carbon-nitrogen ratio is adjusted to be 16: 1-30: 1, the water content is controlled, and superior conditions can be provided for the propagation of microorganisms and the decomposition of straws. On the basis, aerobic fermentation is carried out by adopting microorganisms, decomposed straws are treated by different inorganic solutions (solutions of hydrogen peroxide, potassium permanganate, sulfuric acid, phosphoric acid, citric acid, tartaric acid, potassium hydroxide and the like) to well treat degradation substances formed in pores of the fermented straws, and after double degradation of microbial fermentation and organic solution treatment, the straw degradation and decomposition can reach 5-10%. Then, the impurities in the raw materials and the impurities in the processes of microbial treatment and chemical treatment are further cleaned by using ultrasonic waves, so that the prepared material has more pores and larger specific surface area.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (10)
1. A preparation method of straw-based biological composite material is characterized by comprising the following steps: the preparation method comprises the following steps:
(1) straw pretreatment: cutting the dry straws into small sections of 1-3 cm, removing impurities, drying and sterilizing; spraying a nitrogen source solution on the straws to adjust the carbon-nitrogen ratio, wherein the water content of the straws is 40-70%;
(2) and (3) treating the microorganisms: spraying a microbial agent on the straws obtained in the step (1), uniformly mixing, and fermenting for 2-6 days at 28-37 ℃ to obtain decomposed straws;
(3) chemical treatment: immersing the decomposed straw in 0.5-2.0 mol/L inorganic solution, preserving heat for 1-5 h at 40-70 ℃, and then carrying out ultrasonic treatment for 15-60 min; drying after cleaning;
(4) carbonizing: and (4) keeping the temperature of the dried straws in the step (3) at 400-700 ℃ for carbonization for 30 min-12 h under the protection of micro oxygen or nitrogen, and cooling to obtain the straw-based biological composite material.
2. The preparation method according to claim 1, wherein the carbon-nitrogen ratio of the straw in the step (1) after adjustment is 16: 1-30: 1.
3. The method according to claim 1, wherein the solute of the nitrogen source solution in step (1) is at least one of urea, ammonium salt, nitrate, and organic ammonia.
4. The preparation method according to claim 1, wherein the straw in step (2) is yellow brown in color and odorless, and fermentation is terminated when the temperature is changed to normal temperature to obtain decomposed straw.
5. The preparation method according to claim 1, wherein the microbial agent in the step (2) is a solid preparation with an effective viable count of more than or equal to 100 hundred million/g, and the dosage of the microbial agent is 0.5-2.0 g per kg of dry straw.
6. The method according to claim 1, wherein the microbial agent comprises at least one of Trichoderma viride, Aspergillus niger, Bacillus pumilus, Trichoderma viride, Aspergillus niger, Bacillus subtilis, white rot fungi, and Aspergillus oryzae.
7. The preparation method according to claim 1, wherein the inorganic solution in the step (3) is an aqueous solution of one of hydrogen peroxide, potassium permanganate, sulfuric acid, phosphoric acid, citric acid, tartaric acid and potassium hydroxide.
8. The method according to claim 1, wherein the drying temperature in the step (3) is 70 to 95 ℃.
9. The preparation method according to claim 1, wherein the step (1) further comprises drying for 1 hour at 90-110 ℃ after crushing to remove mixed bacteria.
10. Straw-based biocomposites produced by the process of any one of claims 1-9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471463A (en) * | 2022-02-21 | 2022-05-13 | 湖南农业大学 | Biochar for adsorbing heavy metal cadmium and preparation method and application thereof |
| CN116986581A (en) * | 2023-09-27 | 2023-11-03 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Biomass hard carbon and preparation method and application thereof |
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| CN107721640A (en) * | 2017-11-20 | 2018-02-23 | 芜湖继伟农业有限公司 | A kind of preparation method of the charcoal base microbe slow release fertilizer of EM bacterium fermented stalk |
| CN108383119A (en) * | 2018-04-16 | 2018-08-10 | 吉林农业大学 | A kind of method that microorganism prepares maize straw multi-stage porous absorbent charcoal material |
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2021
- 2021-11-25 CN CN202111409215.5A patent/CN113979423A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107721640A (en) * | 2017-11-20 | 2018-02-23 | 芜湖继伟农业有限公司 | A kind of preparation method of the charcoal base microbe slow release fertilizer of EM bacterium fermented stalk |
| CN108383119A (en) * | 2018-04-16 | 2018-08-10 | 吉林农业大学 | A kind of method that microorganism prepares maize straw multi-stage porous absorbent charcoal material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114471463A (en) * | 2022-02-21 | 2022-05-13 | 湖南农业大学 | Biochar for adsorbing heavy metal cadmium and preparation method and application thereof |
| CN116986581A (en) * | 2023-09-27 | 2023-11-03 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Biomass hard carbon and preparation method and application thereof |
| CN116986581B (en) * | 2023-09-27 | 2024-01-09 | 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) | Biomass hard carbon and preparation method and application thereof |
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