CN114292361A - Preparation method of biomass charcoal hydrogel - Google Patents
Preparation method of biomass charcoal hydrogel Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 84
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- 238000002360 preparation method Methods 0.000 title claims abstract description 33
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 68
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 58
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
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- 239000011261 inert gas Substances 0.000 claims description 6
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Abstract
The invention discloses a preparation method of biomass charcoal hydrogel, which comprises the following steps: pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and drying to obtain dry pretreated sesame straws; preparing biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, carbonizing the powder sesame straws at high temperature, washing the powder sesame straws to be neutral by using hydrochloric acid and deionized water in sequence, and drying to obtain biomass pyrolytic activated carbon; preparing biomass charcoal hydrogel: adding acrylamide, ammonium persulfate and N, N-methylene-bisacrylamide into distilled water to prepare a solution; adding biomass pyrolytic activated carbon into the solution, and irradiating under an ultraviolet lamp to prepare the biomass charcoal hydrogel. According to the invention, sesame straws containing abundant lignin and cellulose are used as raw materials, so that the prepared hydrogel has better compressive strength and elasticity, and the specific surface area of the charcoal is larger due to the high lignin and cellulose.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a preparation method of biomass charcoal hydrogel.
Background
The rapid development of economic society of various countries cannot leave the utilization of energy, the demand of products such as petroleum and the like is rapidly increased, the pollution is caused by using a large amount of energy in coal and power industries, great threat is brought to the environment, renewable energy is vigorously developed, and the renewable energy and raw materials are used for replacing biochemical resources at all times.
The biomass is a renewable clean energy source, plays a significant role in developing society, economy and ecology and realizing carbon neutralization by development and utilization, and is one of important energy sources which human beings rely on to live in an energy form that the biomass can store solar energy in the biomass in a chemical energy form; the activated carbon has good thermal stability, rich pore channels and large specific surface area, and has a plurality of applications in the aspects of adsorption, capacitors and the like. Sesame straw is used as a main agricultural product processing residue in China, sesame straw is used as a biomass resource and is receiving more and more attention, the direct incineration of the sesame straw not only causes resource waste but also causes certain pollution to the atmospheric environment, and if the sesame straw is reasonably recycled, the sesame straw has good social and environmental benefits.
Hydrogel is a stretchable elastomer material, can realize tool portability by introducing substances with special functions into the hydrogel, and is widely applied to the fields of flexible conductive materials, supercapacitors, drug sustained release, sensors and the like at present.
Disclosure of Invention
The invention aims to provide a preparation method of biomass charcoal hydrogel, so as to overcome the technical problems.
A preparation method of biomass charcoal hydrogel comprises the following steps:
a) pretreatment of sesame straw:
cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into a drying oven at the temperature of 30-80 ℃ for drying to obtain dried pretreated sesame straws;
b) preparing biomass pyrolytic carbon:
crushing the pretreated sesame straws into powder and sieving;
carrying out high-temperature carbonization on powdery sesame straws under the protection of inert gas, sequentially washing the powdery sesame straws to be neutral by using hydrochloric acid and deionized water, and drying to obtain biomass pyrolytic carbon;
c) preparing biomass charcoal hydrogel:
adding acrylamide, Ammonium Persulfate (APS) and N, N-methylene Bisacrylamide (BIS) into distilled water according to a certain proportion to prepare a solution;
adding biomass pyrolytic activated carbon into the solution, injecting the solution into a mold, and placing under an ultraviolet lamp for irradiation to prepare the biomass charcoal hydrogel.
Further, in the step a), vacuum drying at 60 ℃ is adopted for drying, a 200-target standard sample sieve is adopted for sieving, and the inert gas is nitrogen or argon.
Further, in the step b), the specific process of high-temperature carbonization is as follows: the temperature is 450 ℃ and 850 ℃, the pyrolysis time is 2-4h, and the heating rate is 5-10 ℃/min.
Further, in the step b), the specific process of high-temperature carbonization is as follows: the temperature is 450 ℃ and 600 ℃, the pyrolysis time is 2-3h, and the heating rate is 5-10 ℃/min.
Further, in the step b), the specific process of high-temperature carbonization is as follows: the temperature is 450 ℃ and 500 ℃, the pyrolysis time is 2h, and the heating rate is 5-10 ℃/min.
Further, in the step b), the mass fraction of the hydrochloric acid is 10%, and the drying temperature is 105 ℃.
Further, in the step c), the mass ratio of the acrylamide to the Ammonium Persulfate (APS) to the N, N-methylene-Bisacrylamide (BIS) is 300-310:7-8: 1.
Further, in the step c), the mass ratio of the biomass pyrolytic carbon to the acrylamide is 1: 90-110.
Further, in the step c), the mass ratio of the biomass pyrolytic carbon to the acrylamide is 1: 100.
Further, in the step c), the wavelength of the ultraviolet lamp is 365nm, and the irradiation time is 20-60 min.
Has the advantages that:
according to the invention, sesame straws containing rich lignin and cellulose are used as raw materials, so that the waste of crops and environmental pollution are reduced, the prepared hydrogel has better compressive strength and elasticity due to the rich cellulose of the sesame straws, the specific surface area of carbon is larger due to the high lignin and cellulose, the application of the activated carbon is wider, and certain economic and social benefits are generated;
in the process of preparing the hydrogel, the method is simple and easy to operate, has low cost, does not pollute the environment and accords with the concept of green chemistry;
due to the high specific surface area and rich pore diameters of the activated carbon, the prepared hydrogel has the advantages of high resistance change rate, high crosslinking density, toughness and high sensitivity, can be used for manufacturing hydrogel sensors, and has certain practical value.
Drawings
FIG. 1 is a nitrogen adsorption and desorption curve and a pore size distribution diagram of biomass charcoal prepared in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph of the biomass char produced in example 1 of the present invention.
Fig. 3, 4, 5, 6, 7, 8, 9, and 10 are graphs showing the rate of change in electrical resistance of the biomass charcoal hydrogels obtained in examples 1, 2, 3, 4, 5, 6, and 7 of the present invention and comparative example 1, respectively.
FIG. 11 is a scanning electron microscope image of hydrogels prepared in example 1 of the present invention and comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the biomass charcoal hydrogel comprises the following steps:
a) pretreatment of sesame straw:
cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into a drying oven at 30-80 ℃ for drying to obtain dried pretreated sesame straws, wherein the drying adopts vacuum drying at 60 ℃;
b) preparing biomass pyrolytic carbon:
crushing the pretreated sesame straws into powder, and sieving by adopting a 200-target standard sample sieve;
carrying out high-temperature carbonization on powdery sesame straws under the protection of inert gas, wherein the inert gas is nitrogen or argon; washing the biomass pyrolysis carbon with hydrochloric acid and deionized water in sequence to be neutral, and drying to obtain biomass pyrolysis carbon, wherein the mass fraction of the hydrochloric acid is 10%, and the drying temperature is 105 ℃;
wherein, the specific process of high-temperature carbonization is as follows: the temperature is 450-; preferably, the temperature is 450-; more preferably, the temperature is 450-.
c) Preparing biomass charcoal hydrogel:
adding acrylamide, Ammonium Persulfate (APS) and N, N-methylene Bisacrylamide (BIS) into distilled water according to a certain proportion to prepare a solution, wherein the mass ratio of the acrylamide to the Ammonium Persulfate (APS) to the N, N-methylene Bisacrylamide (BIS) is 300-310:7-8: 1;
adding biomass pyrolytic activated carbon into the solution, wherein the mass ratio of the adopted biomass pyrolytic activated carbon to acrylamide is 1:90-110, and the preferred mass ratio of the biomass pyrolytic activated carbon to the acrylamide is 1: 100; and then injecting the solution into a mold, and putting the mold under an ultraviolet lamp for irradiation, wherein the wavelength of the ultraviolet lamp is 365nm, and the irradiation time is 20-60min, so as to prepare the biomass charcoal hydrogel.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw:
cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon:
(1) crushing the pretreated sesame straws into powder, and sieving the powder by a standard sample sieve of 200 meshes.
(2) Adding powdered sesame straw into N2Under the protection of (1), high-temperature carbonization is carried out at 450 ℃, after pyrolysis is carried out for 2 hours, the biomass pyrolysis carbon is washed to be neutral by 10% hydrochloric acid and deionized water in sequence and dried in a drying oven at 105 ℃ to obtain biomass pyrolysis carbon;
step c) preparation of biomass charcoal hydrogel:
(1) 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS), and 13.86mg of N, N-methylene Bisacrylamide (BIS) were dissolved in 20ml of deionized water to prepare a solution.
(2) 0.0426g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 1 was tested.
FIG. 1 is a nitrogen adsorption and desorption curve and a pore size distribution diagram of the porous carbon material obtained in example 1, and according to IUPAC classification, N of these samples can be seen2The adsorption-desorption isotherm belongs to the type II curve, and the micropore filling effect occurs in a lower relative pressure range (P/P)0＝0-0.05)，N2The adsorption capacity is sharply increased along with the increase of the relative pressure, which shows that the material has a micropore structure, and the pore diameter of the activated carbon is mainly concentrated near 4nm as can be seen from the pore diameter distribution, which shows that the activated carbon contains more pores with the diameter of about 4nm, and a large number of micropores and mesopores exist.
FIG. 2 is an SEM image of the porous carbon material prepared in example 1 at different magnifications, and from the SEM image, the biomass carbon obtained by the method has a large number of pores, which is helpful for promoting ion migration to enable ions in acrylamide solution to be fully immersed in pores of activated carbon and provide more accessible active sites in a carbon matrix; by observing SEM images, the biomass charcoal has rough surface, smaller particles and smaller pore diameter, and the tiny pores can avoid stress concentration and absorb a large amount of free ions, so that the biomass charcoal hydrogel has higher crosslinking density, is more tenacious and stable.
FIG. 3 is a graph of the rate of change of resistance at 200% strain measured by a tensile machine for the biomass charcoal hydrogel prepared in example 1. Compared with the resistance change rate of other subsequent embodiments, the hydrogel with the same length is stretched, and the resistance change rate of the hydrogel added with the activated carbon is large, so that the hydrogel added with the activated carbon has better conductivity and high sensitivity, and the hydrogel can be applied to be manufactured into a sensor. The resistance change rate is stable all the time, which shows that the stability of the material is good.
Example 2
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, and screening the powder through a standard sample separation sieve of 200 meshes; adding powdered sesame straw into N2Under the protection of (1), high-temperature carbonization is carried out at 550 ℃, after pyrolysis is carried out for 2 hours, the biomass pyrolysis carbon is washed to be neutral by 10% hydrochloric acid and deionized water in sequence and dried in a drying oven at 105 ℃ to obtain biomass pyrolysis carbon;
step c) preparation of biomass charcoal hydrogel: dissolving 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) in 20ml of deionized water to prepare a solution; 0.0426g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 2 was tested.
Example 3
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, and screening the powder through a standard sample separation sieve of 200 meshes; adding powdered sesame straw into N2Under the protection of (1), performing high-temperature carbonization at 650 ℃, performing pyrolysis for 2 hours, sequentially washing the carbonized material to be neutral by using 10% hydrochloric acid and deionized water, and drying the washed material in a drying oven at 105 ℃ to obtain biomass pyrolytic carbon;
step c) preparation of biomass charcoal hydrogel: dissolving 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) in 20ml of deionized water to prepare a solution; 0.0426g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 3 was tested.
Example 4
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, and screening the powder through a standard sample separation sieve of 200 meshes; adding powdered sesame straw into N2Under the protection of (1), high-temperature carbonization is carried out at 750 ℃, after pyrolysis is carried out for 2 hours, the biomass pyrolysis carbon is washed to be neutral by 10% hydrochloric acid and deionized water in sequence and dried in a drying oven at 105 ℃ to obtain biomass pyrolysis carbon;
step c) preparation of biomass charcoal hydrogel: dissolving 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) in 20ml of deionized water to prepare a solution; 0.0426g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 4 was tested.
Example 5
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, and screening the powder through a standard sample separation sieve of 200 meshes; adding powdered sesame straw into N2Under the protection of (1), performing high-temperature carbonization at 850 ℃, performing pyrolysis for 2 hours, sequentially washing the materials to be neutral by using 10% hydrochloric acid and deionized water, and drying the materials in a drying oven at 105 ℃ to obtain biomass pyrolytic carbon;
step c) preparation of biomass charcoal hydrogel: dissolving 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) in 20ml of deionized water to prepare a solution; 0.0426g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 5 was tested.
Example 6
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, and screening the powder through a standard sample separation sieve of 200 meshes; adding powdered sesame straw into N2Under the protection of (1), performing high-temperature carbonization at 850 ℃, performing pyrolysis for 2 hours, sequentially washing the materials to be neutral by using 10% hydrochloric acid and deionized water, and drying the materials in a drying oven at 105 ℃ to obtain biomass pyrolytic carbon;
step c) preparation of biomass charcoal hydrogel: dissolving 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) in 20ml of deionized water to prepare a solution; 0.0473g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 6 was tested.
Example 7
A preparation method of biomass charcoal hydrogel and the hydrogel prepared by the method comprise the following steps:
step a) pretreatment of sesame straw: cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into an oven at 80 ℃ for drying for 24 hours to obtain dried sesame straws;
step b) preparation of biomass pyrolytic carbon: crushing the pretreated sesame straws into powder, and screening the powder through a standard sample separation sieve of 200 meshes; adding powdered sesame straw into N2Under the protection of (1), performing high-temperature carbonization at 850 ℃, performing pyrolysis for 2 hours, sequentially washing the materials to be neutral by using 10% hydrochloric acid and deionized water, and drying the materials in a drying oven at 105 ℃ to obtain biomass pyrolytic carbon;
step c) preparation of biomass charcoal hydrogel: dissolving 4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) in 20ml of deionized water to prepare a solution; 0.0387g of biomass pyrolytic activated carbon is added into the solution, then the solution is injected into a mould and placed under an ultraviolet lamp (365nm) to irradiate for half an hour, and the hydrogel with the thickness of 1mm is prepared.
The biomass charcoal hydrogel obtained in example 7 was tested.
Comparative example 1
A method of making a hydrogel comprising the steps of:
4.26g of acrylamide, 0.1g of Ammonium Persulfate (APS) and 13.86mg of N, N-methylene Bisacrylamide (BIS) are dissolved in 20ml of deionized water to prepare a solution, the solution is injected into a mold and irradiated under an ultraviolet lamp (365nm) for half an hour to prepare hydrogel with the thickness of 1 mm.
The hydrogel obtained in comparative example 1 was tested.
As can be seen from FIGS. 3 to 8, in examples 1 to 5, compared to comparative example 1, the hydrogel prepared under different conditions has a larger and more stable resistance change rate in real time response signal under the same tensile strain (200%), and the resistance change rate in FIG. 3 is larger and more stable than that in comparative example 1 shown in FIG. 8, so that the hydrogel has better sensitivity, good stability and durability.
As can be seen from the attached figure 9, compared with the comparative example 1, in the example 1, (a) is an SEM image of the hydrogel of the comparative example 1, and (b), (c) and (d) are structures of the biochar hydrogel prepared in the example 1, the raw gel is compact and smooth, the activated carbon hydrogel has a rough, loose and porous surface, the activated carbon can be well dispersed and embedded into an acrylamide solution matrix due to a large specific surface area and a reinforced interface effect, the activated carbon participates in a reaction to form a plurality of different aggregates, the pore wall is thick, the overall pore structure is stable, the characteristics of a through hole structure are provided, the framework structure is firm, the three-dimensional structure is provided with a large number of pore channels. The porous structure is rich, the pore diameter is smaller, the crosslinking density is higher, and the toughness is higher.
The product of the invention has high specific surface area, is porous, has high sensitivity and good biocompatibility, is very suitable for the application of hydrogel sensors, and has certain practical value.
The above-mentioned embodiments are only for describing the preferred mode of the present invention, and do not limit the scope of the present invention, and those skilled in the art should make various changes and modifications to the technical solution of the present invention without departing from the spirit of the present invention, and all such changes and modifications should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. The preparation method of the biomass charcoal hydrogel is characterized by comprising the following steps:
a) pretreatment of sesame straw:
cleaning sesame straws by using ethanol and deionized water, and then putting the cleaned sesame straws into a drying oven at the temperature of 30-80 ℃ for drying to obtain dried pretreated sesame straws;
b) preparing biomass pyrolytic carbon:
crushing the pretreated sesame straws into powder and sieving;
carrying out high-temperature carbonization on powdery sesame straws under the protection of inert gas, sequentially washing the powdery sesame straws to be neutral by using hydrochloric acid and deionized water, and drying to obtain biomass pyrolytic activated carbon;
c) preparing biomass charcoal hydrogel:
adding acrylamide, Ammonium Persulfate (APS) and N, N-methylene Bisacrylamide (BIS) into distilled water according to a certain proportion to prepare a solution;
adding biomass pyrolytic activated carbon into the solution, injecting the solution into a mold, and placing under an ultraviolet lamp for irradiation to prepare the biomass charcoal hydrogel.
2. The method for preparing biomass charcoal hydrogel according to claim 1, wherein in step a), vacuum drying at 60 ℃ is adopted for drying; in the step b), a 200-target standard sample sieve is adopted for sieving, and the inert gas is nitrogen or argon.
3. The preparation method of biomass charcoal hydrogel according to claim 1, wherein in step b), the specific process of high temperature carbonization is as follows: the temperature is 450 ℃ and 850 ℃, the pyrolysis time is 2-4h, and the heating rate is 5-10 ℃/min.
4. The preparation method of biomass charcoal hydrogel according to claim 4, wherein in the step b), the specific process of high temperature carbonization is as follows: the temperature is 450 ℃ and 600 ℃, the pyrolysis time is 2-3h, and the heating rate is 5-10 ℃/min.
5. The preparation method of biomass charcoal hydrogel according to claim 5, wherein in step b), the specific process of high temperature carbonization is as follows: the temperature is 450 ℃ and 500 ℃, the pyrolysis time is 2h, and the heating rate is 5-10 ℃/min.
6. The method for preparing biomass charcoal hydrogel according to claim 1, wherein in step b), the mass fraction of the hydrochloric acid is 10%, and the drying temperature is 105 ℃.
7. The method for preparing biomass charcoal hydrogel according to claim 1, wherein in step c), the mass ratio of acrylamide, Ammonium Persulfate (APS) and N, N-methylene Bisacrylamide (BIS) is 300-310:7-8: 1.
8. The method for preparing biomass charcoal hydrogel according to claim 1, wherein in step c), the mass ratio of biomass pyrolysis activated carbon to acrylamide is 1: 90-110.
9. The method for preparing biomass charcoal hydrogel according to claim 1, wherein in step c), the mass ratio of biomass pyrolysis activated carbon to acrylamide is 1: 100.
10. The method for preparing biomass charcoal hydrogel according to claim 1, wherein in step c), the wavelength of the ultraviolet lamp is 365nm, and the irradiation time is 20-60 min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111871385A (en) * | 2020-06-03 | 2020-11-03 | 江苏大学 | Preparation method and application of coconut shell biomass charcoal composite carboxymethyl cellulose adsorbent |
| CN112058035A (en) * | 2020-09-18 | 2020-12-11 | 苏州花仙子环保科技有限公司 | Dehumidifying agent and preparation method thereof |
-
2021
- 2021-12-22 CN CN202111582813.2A patent/CN114292361A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111871385A (en) * | 2020-06-03 | 2020-11-03 | 江苏大学 | Preparation method and application of coconut shell biomass charcoal composite carboxymethyl cellulose adsorbent |
| CN112058035A (en) * | 2020-09-18 | 2020-12-11 | 苏州花仙子环保科技有限公司 | Dehumidifying agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| N H MERI等: "Effect of Chemical Washing Pre-treatment of Empty Fruit Bunch (EFB) biochar on Characterization of Hydrogel Biochar composite as Bioadsorbent", 《IOP CONF. SERIES: MATERIALS SCIENCE AND ENGINEERING》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282338A (en) * | 2023-04-27 | 2023-06-23 | 东华工程科技股份有限公司 | Chemical wastewater treatment agent and preparation method thereof |
| CN116282338B (en) * | 2023-04-27 | 2023-08-22 | 东华工程科技股份有限公司 | Chemical wastewater treatment agent and preparation method thereof |
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