CN111056551A - Method for preparing aquatic animal activated carbon by hydrothermal method - Google Patents
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- CN111056551A CN111056551A CN202010018561.XA CN202010018561A CN111056551A CN 111056551 A CN111056551 A CN 111056551A CN 202010018561 A CN202010018561 A CN 202010018561A CN 111056551 A CN111056551 A CN 111056551A
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- C01B32/342—Preparation characterised by non-gaseous activating agents
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention relates to the technical field of activated carbon, in particular to a method for preparing aquatic animal activated carbon by a hydrothermal method, which comprises the following steps: 1) pretreating aquatic animal waste and then crushing to obtain pasty biomass; 2) uniformly mixing the pasty biomass with a pore-forming activating agent, standing, carrying out hydrothermal carbonization treatment, taking out the obtained activated carbon after the reaction is finished, cleaning and drying to obtain the activated carbon. According to the invention, the activated carbon product is prepared by taking the aquatic animal waste as the raw material, so that the activated carbon with good performance is prepared, the resource utilization of the waste biomass is realized, and compared with plant biomass, the method utilizes the characteristic tissue composition characteristics of the aquatic animal waste, and selectively adds the pore-forming active agent, so that the reaction product can be optimized, and the generation of high-quality activated carbon with high porosity and good adsorption effect is facilitated; and the prepared activated carbon product has rich oxygen-containing and nitrogen-containing functional groups, such as carbonyl, carboxyl and the like, and is favorable for improving the pollutant adsorption effect.
Description
Technical Field
The invention relates to the technical field of activated carbon, in particular to a method for preparing aquatic animal activated carbon by a hydrothermal method.
Background
The information disclosed in this background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
The active carbon has the advantages of developed pores, good adsorption performance and the like, and is widely applied to the fields of sewage treatment, air purification and the like. At present, a pyrolysis carbonization method is mostly adopted for preparing the biomass activated carbon, and besides the pyrolysis carbonization method, a hydrothermal method can also be used for preparing the high-performance biomass activated carbon. The hydrothermal carbonization technology is a method for directly carbonizing biomass by reacting with an aqueous solution in a low-temperature closed environment, the method is simple in process, easy to operate and mild in condition, energy consumption in the carbon preparation process can be greatly reduced, formation of toxic and harmful byproducts is controlled, and the prepared active carbon contains rich oxygen-containing and nitrogen-containing functional groups on the surface and has an important influence on the adsorption performance of the active carbon, so that the active carbon prepared by the hydrothermal method has more advantages in the adsorption and further activation modification processes. Currently, the application of the activated carbon prepared by a hydrothermal method is mostly concentrated in the field of plant biomass, such as straw, shaddock peel (CN201610385938), hickory peel (CN201610013599) and the like are taken as raw materials. However, the yield of aquatic products in China is huge, but the processing and comprehensive utilization of the aquatic products are relatively lagged. A large amount of leftovers such as fish scales, fish bones and viscera, shrimp and crab shells and the like generated in the processes of processing aquatic products and the like can reach more than 200 million tons of fish wastes every year, which not only causes environmental pollution, but also is huge waste of biomass resources.
Disclosure of Invention
In order to solve the problems, the invention further researches and discovers that: the aquatic animal waste contains a large amount of protein, fat, calcium and the like, and has the foundation for preparing activated carbon; meanwhile, the fish scale contains a large amount of water, for example, the water content in the fish scales is 50-70%, and the water content in the fish bones is 39-55%. Therefore, the hydrothermal method for preparing the aquatic animal activated carbon has feasibility. Therefore, the invention provides a method for preparing aquatic animal activated carbon by a hydrothermal method, which not only can prepare activated carbon with good performance, but also can realize resource utilization of waste biomass.
In order to achieve the purpose, the invention adopts the following technical means:
firstly, the invention discloses a method for preparing aquatic animal activated carbon by a hydrothermal method, which comprises the following steps:
(1) pretreating aquatic animal waste and then crushing to obtain pasty biomass;
(2) uniformly mixing the pasty biomass with a pore-forming activating agent, standing, carrying out hydrothermal carbonization treatment, taking out the obtained activated carbon after the reaction is finished, cleaning and drying to obtain the activated carbon.
Further, in the step (1), the waste of aquatic animal material includes: one or more of fishbone, fish scale, fish viscera, shrimp shell, crab shell, waste after processing shrimp and crab in aquaculture, fish impurity discarded in aquaculture, etc.
Further, in the step (1), the pretreatment method comprises the following steps: washing with tap water and then with deionized water to remove impurities on the surfaces of the aquatic animal substances.
Further, in the step (1), the crushing method comprises the following steps: freezing at low temperature (-8-12 deg.C), cutting into blocks, and pulverizing; or directly adopting a meat grinder to carry out the mincing treatment; or putting into a grinder, adding a small amount of liquid nitrogen, grinding and crushing. Preferably, after the crushing treatment, the particle size of the obtained pasty biomass is controlled to be 0.1-0.3 mm.
Further, in the step (2), the pore-forming activating agent comprises any one of ammonium bicarbonate, urea, acetic acid, citric acid and the like; the space structure of the aquatic animal biomass charcoal is adjusted by adding the pore-forming activating agent, and the performance of the aquatic animal biomass charcoal is improved.
Preferably, the pore-forming activator is selected according to the type of the adopted aquatic animal, and the biomass materials with high calcium content, such as fishbone, shrimp shell, crab shell and the like, adopt acetic acid, citric acid and the like as the pore-forming activator, can react with calcium, improve the pore-forming efficiency and enhance the adsorption performance; for biomass materials with high protein content, such as fish scales, fish viscera and the like, ammonium bicarbonate, urea and the like are used as pore-forming activators, so that protein denaturation caused by hydrogen bonds in protein molecules can be destroyed, small molecules are further formed, the carbonization process is accelerated, and the pore-forming efficiency is improved.
Further, in the step (2), the mass ratio of the pore-forming activating agent to the biomass is 1: 1.5-1: 3.
Further, the ammonium bicarbonate, the urea, the acetic acid and the citric acid are added in the form of a solution (such as an aqueous solution), and optionally, the mass concentration of the solution is 2.5-7.5%.
Further, in the step (2), the standing time is 15-25 min, so that the pore-forming activating agent and the biomass can fully react, and the tissue structure of the biomass can be adjusted.
Further, in the step (2), the temperature of the hydrothermal carbonization treatment is 180-220 ℃, and the reaction time is 8-12 h.
Further, in the step (2), the cleaning method comprises the following steps: and taking out the obtained activated carbon, soaking the activated carbon in deionized water, and cleaning the activated carbon until the pH value is 6.5-7.5.
Further, in the step (2), the drying temperature is 100-115 ℃ and the time is 2-3 h.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) according to the invention, the activated carbon product is prepared by taking the aquatic animal waste as the raw material, so that the activated carbon with good performance is prepared, the resource utilization of the waste biomass is realized, and the industrial economic benefit is increased.
(2) Compared with plant biomass, the invention utilizes the characteristic tissue composition of the aquatic animal biomass and selectively adds the pore-forming active agent, thereby not only optimizing the reaction product, but also being beneficial to generating high-quality active carbon with high porosity and good adsorption effect; and the prepared activated carbon product has rich oxygen-containing and nitrogen-containing functional groups, such as carbonyl, carboxyl and the like, and is favorable for improving the pollutant adsorption effect.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a scanning electron micrograph of an activated carbon prepared according to a first embodiment of the present invention.
FIG. 2 is a scanning electron microscope photograph of the activated carbon prepared in the first experimental example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As mentioned above, the yield of aquatic products in China is huge, but the processing and comprehensive utilization of aquatic products are relatively lagged. Not only brings environmental pollution, but also is a huge waste of biomass resources. Therefore, the invention provides a method for preparing the aquatic animal activated carbon by a hydrothermal method; the invention will now be further described with reference to specific embodiments.
First embodiment
The method for preparing the activated carbon by using the wastes after the processing treatment of the shrimp shells, the crab shells and the aquaculture shrimps and crabs as animal materials comprises the following steps:
1. after washing with tap water, further washing the wastes such as shrimp and crab shells with deionized water, after washing surface impurities, putting the wastes into a grinder, adding a small amount of liquid nitrogen, and grinding, wherein the crab shells with larger volume are firstly subjected to primary breaking treatment by using a hard tool to form small blocks, and then are subjected to crushing and grinding. The maximum particle size after treatment is not more than 0.3 mm.
2. Citric acid is used as a pore-forming activating agent, a citric acid aqueous solution with the mass concentration of 7.5% is prepared, the ground animal material and the pore-forming activating agent are mixed according to the proportion of 1:3, the mixture is stirred uniformly and then stands for 25min, and then the mixture is put into a closed high-pressure reaction kettle, the temperature is controlled at 180 ℃, the reaction time is 12h, and the hydrothermal carbonization treatment is carried out.
3. And after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the obtained product of the activated carbon, soaking the activated carbon in distilled water, washing the activated carbon to have the pH value of 6.5, filtering the activated carbon, and drying the filtered activated carbon in an oven for 3 hours at the temperature of 100 ℃ to obtain the activated carbon.
Second embodiment
The method for preparing the activated carbon by using the fishbone as the animal material comprises the following steps:
1. washing fishbone with tap water, further washing fishbone with deionized water, washing surface impurities, placing in a low-temperature freezer at-10 deg.C for 2 hr, taking out, cutting into pieces, and pulverizing with pulverizer to obtain pasty biomass with maximum particle size of 0.2mm or less.
2. And (2) taking acetic acid as a pore-forming activator, preparing an acetic acid water solution with the mass concentration of 5%, mixing the pasty biomass in the step (1) and the pore-forming activator according to the mass ratio of 1:1.5, uniformly stirring, standing for 20min, then placing into a closed high-pressure reaction kettle, controlling the temperature to be 200 ℃ and the reaction time to be 10h, and carrying out hydrothermal carbonization.
3. Naturally cooling the reaction kettle to room temperature after the reaction is finished, taking out the obtained product of the activated carbon, soaking and cleaning the activated carbon by using distilled water until the pH value is 7.5, filtering the product, and then putting the product into an oven to dry the product for 2.5 hours at the temperature of 105 ℃ to obtain the activated carbon.
Third embodiment
The method for preparing the activated carbon by using fish scales, fish viscera or fish impurities discarded in aquaculture as animal materials comprises the following steps:
1. washing with tap water, further washing fish scales, fish viscera and fish impurities with deionized water, cleaning surface impurities, and mincing in a meat mincer, wherein the maximum particle size after mincing is not more than 0.1 mm.
2. Taking ammonium bicarbonate as a pore-forming activating agent, preparing an ammonium bicarbonate aqueous solution with the mass concentration of 7.5%, mixing the ground animal material and the pore-forming activating solution according to the proportion of 1:2, uniformly stirring, standing for 20min, putting into a sealed high-pressure reaction kettle, controlling the temperature at 220 ℃ and the reaction time at 8h, and carrying out hydrothermal carbonization.
4. And after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the obtained product of the activated carbon, soaking the activated carbon in distilled water, cleaning the activated carbon to a pH value of 7.0, filtering the activated carbon, and drying the filtered activated carbon in an oven for 2 hours at a temperature of 115 ℃ to obtain the activated carbon.
First test example
The method for preparing the activated carbon by using the wastes after the processing treatment of the shrimp shells, the crab shells and the aquaculture shrimps and crabs as animal materials comprises the following steps:
1. after washing with tap water, further washing the wastes such as shrimp and crab shells with deionized water, after washing surface impurities, putting the wastes into a grinder, adding a small amount of liquid nitrogen, and grinding, wherein the crab shells with larger volume are firstly subjected to primary breaking treatment by using a hard tool to form small blocks, and then are subjected to crushing and grinding. The treated maximum particle size is not more than 0.3mm, and then the treated maximum particle size is put into a closed high-pressure reaction kettle, the temperature is controlled at 180 ℃, the reaction time is 12 hours, and hydrothermal carbonization treatment is carried out.
2. And after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the obtained product of the activated carbon, soaking the activated carbon in distilled water, washing the activated carbon to have the pH value of 6.5, filtering the activated carbon, and drying the filtered activated carbon in an oven for 3 hours at the temperature of 100 ℃ to obtain the activated carbon.
Second test example
The method for preparing the activated carbon by using the fishbone as the animal material comprises the following steps:
1. washing fishbone with tap water, further washing fishbone with deionized water, washing surface impurities, placing in a low-temperature freezer at-10 ℃ for 2 hours, taking out, cutting into pieces, placing in a grinder for grinding, and placing in a closed high-pressure reaction kettle at 200 ℃ for 10 hours to obtain pasty biomass with maximum particles of not more than 0.2mm, and performing hydrothermal carbonization.
2. Naturally cooling the reaction kettle to room temperature after the reaction is finished, taking out the obtained product of the activated carbon, soaking and cleaning the activated carbon by using distilled water until the pH value is 7.5, filtering the product, and then putting the product into an oven to dry the product for 2.5 hours at the temperature of 105 ℃ to obtain the activated carbon.
Third test example
The method for preparing the activated carbon by using fish scales, fish viscera or fish impurities discarded in aquaculture as animal materials comprises the following steps:
1. washing with tap water, further washing fish scales, fish viscera and fish impurities with deionized water, washing to remove surface impurities, mincing in a meat mincer, controlling the maximum particle size to be not more than 0.1mm, placing in a sealed high-pressure reaction kettle, controlling the temperature to be 220 ℃, and reacting for 8 hours to carry out hydrothermal carbonization.
2. And after the reaction is finished, naturally cooling the reaction kettle to room temperature, taking out the obtained product of the activated carbon, soaking the activated carbon in distilled water, cleaning the activated carbon to a pH value of 7.0, filtering the activated carbon, and drying the filtered activated carbon in an oven for 2 hours at a temperature of 115 ℃ to obtain the activated carbon.
And (3) performance testing:
taking the first example and the first test example as examples, the specific surface area and the total pore volume of the activated carbon prepared by the method were measured, and the results are shown in table 1.
TABLE 1
| First embodiment | First test example | |
| Specific surface area SBET (m)2/g) | 1205.23 | 1083.03 |
| Total pore volume Vtot (cm)3/g) | 1.309 | 1.081 |
As can be seen from the detection data in table 1, the specific surface area and the total pore volume of the prepared activated carbon are significantly improved by selectively adding the pore-forming active agent according to the characteristic of tissue components specific to aquatic animal biomass, so that the activated carbon prepared by the method of the present invention has excellent activated carbon with high porosity and good adsorption effect, which can be seen from the SEM images of the activated carbon in fig. 1 and 2. In addition, the activated carbon prepared by the aquatic animal substances also has rich oxygen-containing and nitrogen-containing functional groups, such as carbonyl, carboxyl and the like, and is favorable for improving the pollutant adsorption effect.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing aquatic animal activated carbon by a hydrothermal method is characterized by comprising the following steps:
(1) pretreating aquatic animal waste and then crushing to obtain pasty biomass;
(2) uniformly mixing the pasty biomass with a pore-forming activating agent, standing, carrying out hydrothermal carbonization treatment, taking out the obtained activated carbon after the reaction is finished, cleaning and drying to obtain the activated carbon.
2. The hydrothermal process for producing activated carbon derived from aquatic animals as claimed in claim 1, wherein in step (1), the waste aquatic animals comprises: one or more of fishbone, fish scale, fish viscera, shrimp shell, crab shell, waste after processing shrimp and crab in aquaculture, fish impurity discarded in aquaculture, etc.
3. The hydrothermal process for producing activated carbon derived from aquatic animals as claimed in claim 1, wherein in step (1), the crushing is performed by: freezing at low temperature, cutting into pieces, and pulverizing with a pulverizer; the temperature of the low-temperature freezing is preferably-8 to-12 ℃;
or directly adopting a meat grinder to carry out the mincing treatment;
or, putting the mixture into a grinder, adding a small amount of liquid nitrogen, grinding and crushing;
preferably, after the crushing treatment, the particle size of the obtained pasty biomass is controlled to be 0.1-0.3 mm.
4. The hydrothermal process for preparing activated carbon for aquatic animals according to claim 1, wherein in the step (2), the pore-forming activator comprises any one of ammonium bicarbonate, urea, acetic acid and citric acid;
preferably, for biomass materials with high calcium content, such as fishbone, shrimp shell and crab shell, acetic acid, citric acid and the like are adopted as pore-forming activators;
preferably, for biomass materials with high protein content, such as fish scales and fish viscera, ammonium bicarbonate, urea and the like are used as pore-forming activators.
5. A hydrothermal process for the preparation of an aquatic activated carbon according to claim 4, wherein the ammonium bicarbonate, urea, acetic acid, citric acid are added as a solution, preferably as an aqueous solution;
preferably, the mass concentration of the solution is 2.5-7.5%.
6. The hydrothermal method for preparing activated carbon for aquatic animals according to claim 4, wherein in the step (2), the mass ratio of the pore-forming activator to the biomass is 1: 1.5-1: 3.
7. A hydrothermal process for preparing activated carbon derived from aquatic animals as claimed in any of claims 1 to 6, wherein in step (2), the standing time is 15 to 25 min.
8. A hydrothermal method for preparing activated carbon derived from aquatic animals as defined in any of claims 1-6, wherein in step (2), the temperature of the hydrothermal carbonization treatment is 180-220 ℃ and the reaction time is 8-12 h.
9. A hydrothermal process for the production of activated carbon derived from aquatic animals as claimed in any of claims 1 to 6, wherein in step (2), the washing is carried out by: taking out the obtained activated carbon, soaking the activated carbon in deionized water, and cleaning the activated carbon until the pH value is 6.5-7.5; preferably, in the step (2), the drying temperature is 100-115 ℃ and the time is 2-3 h.
10. A hydrothermal process for the production of activated carbon derived from aquatic animals as claimed in any of claims 1 to 6 wherein in step (1) the pretreatment is by: the water is firstly washed by tap water and then by deionized water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113546664A (en) * | 2021-07-25 | 2021-10-26 | 湘潭大学 | Cobalt-nitrogen co-doped fish scale biochar catalyst and preparation method and application thereof |
| CN114853125A (en) * | 2022-04-28 | 2022-08-05 | 东北农业大学 | Preparation method of carbon-based adsorption electrode and three-electrode electric flocculation system |
| CN115259151A (en) * | 2022-06-20 | 2022-11-01 | 中国建筑第八工程局有限公司 | High-alkalinity biochar and preparation method and application thereof |
| CN115501857A (en) * | 2022-09-29 | 2022-12-23 | 中建八局发展建设有限公司 | Biochar capable of removing high-nitrogen functional groups and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113546664A (en) * | 2021-07-25 | 2021-10-26 | 湘潭大学 | Cobalt-nitrogen co-doped fish scale biochar catalyst and preparation method and application thereof |
| CN114853125A (en) * | 2022-04-28 | 2022-08-05 | 东北农业大学 | Preparation method of carbon-based adsorption electrode and three-electrode electric flocculation system |
| CN115259151A (en) * | 2022-06-20 | 2022-11-01 | 中国建筑第八工程局有限公司 | High-alkalinity biochar and preparation method and application thereof |
| CN115501857A (en) * | 2022-09-29 | 2022-12-23 | 中建八局发展建设有限公司 | Biochar capable of removing high-nitrogen functional groups and preparation method thereof |
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Application publication date: 20200424 |