CN111196932A - Method for preparing nano biochar - Google Patents
Method for preparing nano biochar Download PDFInfo
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- CN111196932A CN111196932A CN202010055395.0A CN202010055395A CN111196932A CN 111196932 A CN111196932 A CN 111196932A CN 202010055395 A CN202010055395 A CN 202010055395A CN 111196932 A CN111196932 A CN 111196932A
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- biochar
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- suspension
- reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a method for rapidly preparing a large amount of nano-scale biochar, which reduces the loss of biochar nano-particles, increases the yield of nano-scale biochar, and utilizes reverse osmosis to purify a biochar suspension to further obtain high-purity nano-scale biochar particles for rapidly preparing a large amount of biochar nano-particles.
Description
Technical Field
The invention relates to the field of biomass energy, in particular to a method for producing nano biochar.
Background
Biochar (Biochar) is a substance formed by pyrolysis of biomass under anoxic conditions, according to the definition of International Biochar Initiative (IBI), which is applied to the soil and yields agricultural and environmental benefits. A great deal of research in recent years shows that the application of the biochar in the soil can effectively seal CO2 in the atmosphere, improve the soil quality from multiple aspects (pH, CEC, nutrient utilization rate, water utilization rate, bioavailability of heavy metals and organic pollutants and the like) and improve the crop yield. It is estimated that the storage amount of the global agricultural soil to the biochar can be up to 4280 hundred million tons. Therefore, there is a great market demand for biochar for agriculture globally in the future.
Although various small-sized pyrolysis systems for manufacturing biochar have been developed in various laboratories around the world, industrial technologies for rapidly manufacturing nano-sized biochar on a large scale are not yet mature, and technologies and equipment systems for rapidly manufacturing nano-sized biochar on a large scale are still lacking. The nanometer biochar can be obtained by a traditional biomass combustion method and dry ball milling, but the nanometer biochar has high loss rate and low yield, generates a large amount of smoke and seriously pollutes the atmospheric environment.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for rapidly preparing a large amount of nano biochar, which comprises the following steps:
s1, drying the biomass, crushing, putting into a muffle furnace, calcining at the temperature of more than 500 ℃, grinding and sieving after calcining, and drying to obtain charcoal powder; the biomass can be various plant straws, excrement and the like, including rice straws and sugarcane straws;
s2, putting the charcoal powder into a ball mill, adding ultrapure water to wet a sample, carrying out wet grinding by the ball mill, and carrying out freeze drying after grinding to obtain a charcoal sample;
s3, adding the biochar sample into ultrapure water, and performing ultrasonic dispersion treatment on the biochar sample to obtain a biochar suspension;
s4, centrifugal extraction: centrifuging the biochar suspension, and extracting supernatant to obtain nano biochar particle solution;
s5, removing impurities in the biochar suspension by using a reverse osmosis membrane; the reverse osmosis purification method comprises the following steps: the control system opens the sample injection valve and the sample outlet valve to carry out reverse osmosis for the first time, the biochar suspension enters from the sample injection valve, and the impurity solution enters the central liquid collecting pipe under the action of the filter element reverse osmosis membrane, so that impurities such as dissolved salts, colloids and microorganisms flow out through an outlet of the central liquid collecting pipe. The biochar suspension liquid with impurities removed is gathered near the pressure balloon, and flows out through the sample outlet valve after the pressure balloon is compressed. When the pressure sensor detects that the pressure of the biochar suspension liquid for removing impurities rises to a given pressure, the control system controls to close the sample injection valve and the sample outlet valve to perform reverse osmosis purification for the second time, the pressure balloon is reacted by the pressure generated by compressing the biochar suspension liquid to the biochar suspension liquid, the biochar suspension liquid is reversely recycled through the filter element, so that the generated impurity solution enters the central liquid collecting pipe and flows out along the outlet of the central liquid collecting pipe, the pressure generated by the pressure balloon is reduced along with the output of the impurity solution, the pressure sensor detects that the pressure of the biochar suspension liquid is reduced to the given pressure, the control system controls to open the sample injection valve and the sample outlet valve, and then reverse osmosis purification is performed repeatedly. The reverse osmosis membrane may be any one of a flat membrane (flat membrane), a tubular membrane (tubular membrane), a spiral membrane (spiral membrane), a hollow fiber membrane (hollow fiber membrane), and the like.
And S6, performing low-temperature freezing preservation on the nano biochar particle solution, freezing and then performing freeze drying treatment to obtain the nano biochar particles.
The invention reduces the loss of the biological carbon nano particles, increases the yield of the nano-scale biological carbon, and utilizes reverse osmosis to purify the biological carbon suspension to further obtain the high-purity nano-scale biological carbon particles for rapidly preparing a large amount of biological carbon nano particles.
In a preferred embodiment, the weight ratio of the charcoal powder to the ultrapure water used in step S2 is 1: 1-1: 500.
in a preferred embodiment, the ultrasonic dispersion treatment method in step S3 is to use an ultrasonic cell disruptor.
In a preferred embodiment, in step S5, the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, a reverse osmosis purification step is added between the step S3 and the step S4: and removing impurities in the obtained nano biochar particle solution by using a reverse osmosis membrane.
In a preferred embodiment, in step S4, the centrifugation rate and the sedimentation time for the nano biochar particles with the particle size of less than 100nm to settle to a specific position are calculated according to the temperature of the biochar suspension and the Stokes equation.
Drawings
The invention and its advantages will be better understood by studying the following detailed description of specific embodiments, given by way of non-limiting example, and illustrated in the accompanying drawings, in which:
FIG. 1 is a Scanning Electron Microscope (SEM) picture for observing the original surface appearance and particle size of the rice straw biochar.
FIG. 2 is a Scanning Electron Microscope (SEM) picture for observing the surface morphology and particle size of the prepared nano-scale rice straw biochar.
Detailed Description
The word "embodiment" is used herein to mean serving as an example, instance, or illustration. In addition, the articles "a" and "an" as used in this specification and the appended claims may generally be construed to mean "one or more" unless specified otherwise or clear from context to be directed to a singular form.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
Examples
First, referring to fig. 1-2, a method for producing nano biochar by using straw according to an embodiment of the present invention is described:
s1) drying rice straws at 60 ℃ for 48h, crushing, putting into a muffle furnace, burning for 2h at 550 ℃, grinding and sieving (100 meshes) after calcination, and drying to obtain charcoal powder;
s2) putting the sieved charcoal powder into a ball mill, adding ultrapure water until the charcoal powder is just wet, wet-grinding for 72 hours by using the ball mill, freezing by using a refrigerator at minus 80 ℃ after grinding, and freezing and air-drying by using a freeze dryer to obtain a charcoal sample;
s3) taking 7.5g of the frozen and air-dried biochar sample, adding the 7.5g of the biochar sample into a beaker filled with 500ml of ultrapure water, and after gentle stirring, carrying out ultrasonic treatment on the biochar sample for 30min by using an ultrasonic cell disruption instrument (660W, model JY98-IIIDN) so as to stably disperse the biochar suspension;
s4) taking 40ml of each of the biochar suspensions in centrifuge tubes 1, 2, 3, setting a centrifuge (model Allegra X-15R, rotor F0650, based on stokes law equation): 10100rpm, time: 40min, RCF: 9579.96 separating, and taking out the centrifuged supernatant to obtain charcoal suspension; calculating the centrifugal rate and the sedimentation time of the nano biochar particles with the particle size of less than 100nm sedimenting to a certain specific position according to the temperature of the biochar suspension and a Stokes equation;
s5) purifying the suspension of biochar with a reverse osmosis membrane to remove impurities therein, wherein the reverse osmosis membrane uses polyvinyl alcohol (PVA) with negatively charged surface in order to inhibit the contaminants from being adsorbed on the membrane by charge repulsion since the contaminants (fouling substances) in the treated soil are generally negatively charged. The reverse osmosis purification method comprises the following steps: the control system opens the sample injection valve and the sample outlet valve to carry out reverse osmosis for the first time, the biochar suspension enters from the sample injection valve, and the impurity solution enters the central liquid collecting pipe under the action of the filter element reverse osmosis membrane, so that impurities such as dissolved salts, colloids and microorganisms flow out through an outlet of the central liquid collecting pipe. The biochar suspension liquid with impurities removed is gathered near the pressure balloon, and flows out through the sample outlet valve after the pressure balloon is compressed. When the pressure sensor detects that the pressure of the biochar suspension liquid for removing impurities rises to a given pressure, the control system controls to close the sample injection valve and the sample outlet valve to perform reverse osmosis purification for the second time, the pressure balloon is reacted by the pressure generated by compressing the biochar suspension liquid to the biochar suspension liquid, the biochar suspension liquid is reversely recycled through the filter element, so that the generated impurity solution enters the central liquid collecting pipe and flows out along the outlet of the central liquid collecting pipe, the pressure generated by the pressure balloon is reduced along with the output of the impurity solution, the pressure sensor detects that the pressure of the biochar suspension liquid is reduced to the given pressure, the control system controls to open the sample injection valve and the sample outlet valve, and reverse osmosis purification is performed for the second time.
S6) sealing the bottle mouth with tinfoil, pricking several small holes on the tinfoil, and refrigerating in a refrigerator at-80 deg.C; and after the sample is completely frozen, freezing and air-drying the sample by using a freeze dryer to obtain the biochar nano-particles of the rice straw.
The embodiment reduces the loss of the biological carbon nano particles, increases the yield of the nano-scale biological carbon, and utilizes reverse osmosis to purify the biological carbon suspension, thereby obtaining the high-purity nano-scale biological carbon particles for rapidly preparing a large amount of biological carbon nano particles.
FIG. 1 is a Scanning Electron Microscope (SEM) picture for observing the original surface appearance and particle size of the rice straw biochar.
FIG. 2 is a Scanning Electron Microscope (SEM) picture for observing the surface morphology and particle size of the prepared nano-scale rice straw biochar.
Claims (6)
1. A method for preparing nano biochar is characterized by comprising the following steps:
s1, drying the biomass, crushing, putting into a muffle furnace, calcining at the temperature of more than 500 ℃, grinding and sieving after calcining, and drying to obtain charcoal powder;
s2, putting the charcoal powder into a ball mill, adding ultrapure water to wet a sample, carrying out wet grinding by the ball mill, and carrying out freeze drying after grinding to obtain a charcoal sample;
s3, adding the biochar sample into ultrapure water, and performing ultrasonic dispersion treatment on the biochar sample to obtain a biochar suspension;
s4, centrifugal extraction: centrifuging the biochar suspension, and extracting supernatant to obtain nano biochar particle solution;
s5, removing impurities in the biochar suspension by using a reverse osmosis membrane;
and S6, performing low-temperature freezing preservation on the nano biochar particle solution, freezing and then performing freeze drying treatment to obtain the nano biochar particles.
2. The method for preparing nano biochar according to claim 1, wherein: the weight ratio of the charcoal powder to the used ultrapure water in the step S2 is 1: 1-1: 500.
3. the method for preparing nano biochar according to claim 1, wherein: the ultrasonic dispersion treatment method in step S3 is to use an ultrasonic cell disruptor.
4. The method for preparing nano biochar according to claim 1, wherein: in step S5, the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
5. The method for preparing nano biochar according to claim 1, wherein: a reverse osmosis purification step is added between the step S3 and the step S4: and removing impurities in the obtained nano biochar particle solution by using a reverse osmosis membrane.
6. The method for preparing nano biochar according to claim 1, wherein: in step S4, the centrifugal rate and the settling time of the nano biochar particles with the particle size of less than 100nm settling to a certain position are calculated according to the temperature of the biochar suspension and the Stokes equation.
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| CN202010055395.0A CN111196932A (en) | 2020-01-17 | 2020-01-17 | Method for preparing nano biochar |
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| CN202010055395.0A CN111196932A (en) | 2020-01-17 | 2020-01-17 | Method for preparing nano biochar |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661893A (en) * | 2020-06-08 | 2020-09-15 | 江南大学 | Method for eliminating antibiotic resistance genes in water by using nano biochar |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4873213B2 (en) * | 2004-05-18 | 2012-02-08 | 株式会社還元溶融技術研究所 | Method and apparatus for producing carbon fine particles |
| CN105236386A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing carbon nanoparticles through corncob |
| CN106268632A (en) * | 2016-07-19 | 2017-01-04 | 浙江绿冠环保科技有限公司 | A kind of charcoal photocatalyst formaldehyde purifying agent and preparation method thereof |
| CN108611096A (en) * | 2018-06-02 | 2018-10-02 | 韩芳 | A kind of efficient renovation agent of soil and preparation method thereof |
| CN109847697A (en) * | 2019-01-30 | 2019-06-07 | 中山大学 | A kind of charcoal base zero-valent iron material and preparation method thereof |
-
2020
- 2020-01-17 CN CN202010055395.0A patent/CN111196932A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4873213B2 (en) * | 2004-05-18 | 2012-02-08 | 株式会社還元溶融技術研究所 | Method and apparatus for producing carbon fine particles |
| CN105236386A (en) * | 2015-11-10 | 2016-01-13 | 东华大学 | Method for preparing carbon nanoparticles through corncob |
| CN106268632A (en) * | 2016-07-19 | 2017-01-04 | 浙江绿冠环保科技有限公司 | A kind of charcoal photocatalyst formaldehyde purifying agent and preparation method thereof |
| CN108611096A (en) * | 2018-06-02 | 2018-10-02 | 韩芳 | A kind of efficient renovation agent of soil and preparation method thereof |
| CN109847697A (en) * | 2019-01-30 | 2019-06-07 | 中山大学 | A kind of charcoal base zero-valent iron material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661893A (en) * | 2020-06-08 | 2020-09-15 | 江南大学 | Method for eliminating antibiotic resistance genes in water by using nano biochar |
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