CN110577221A - Preparation method of jatropha curcas-based biomass activated carbon - Google Patents
Preparation method of jatropha curcas-based biomass activated carbon Download PDFInfo
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- CN110577221A CN110577221A CN201911045448.4A CN201911045448A CN110577221A CN 110577221 A CN110577221 A CN 110577221A CN 201911045448 A CN201911045448 A CN 201911045448A CN 110577221 A CN110577221 A CN 110577221A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 241001048891 Jatropha curcas Species 0.000 title claims abstract description 71
- 239000002028 Biomass Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 34
- 239000002893 slag Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 26
- 230000004913 activation Effects 0.000 claims abstract description 24
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000007598 dipping method Methods 0.000 claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 230000003213 activating effect Effects 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 9
- 230000008859 change Effects 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000007873 sieving Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000005470 impregnation Methods 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 239000011148 porous material Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 229930013930 alkaloid Natural products 0.000 description 9
- 150000003797 alkaloid derivatives Chemical class 0.000 description 9
- 230000009471 action Effects 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000009264 composting Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000575 pesticide Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003225 biodiesel Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of jatropha curcas based biomass activated carbon, and belongs to the technical field of biomass activated carbon. The preparation process comprises the following steps: step 1: cleaning the Jatropha curcas base slag, and drying for later use; step 2: putting the jatropha curcas base slag into a phosphoric acid solution, uniformly mixing, dipping, introducing power ultrasonic waves for mixing and activating in the dipping process, and obtaining a sample a after dipping; and step 3: putting the sample a into an oven for drying until the weight of the sample a does not change any more, and obtaining a sample b; and 4, step 4: putting the sample b into a chemical activation furnace, and gradually heating to 500-850 ℃ for activation under the protection of nitrogen; and 5: and repeatedly washing the activated sample by using deionized water until the sample is neutral, drying the sample to constant weight, and grinding and sieving the sample to obtain an activated carbon product. Phosphoric acid is used as an activating agent, and a phosphoric acid solution and the Jatropha curcas slag are mixed according to a certain liquid-solid ratio, so that the Jatropha curcas-based biomass activated carbon material is successfully prepared, and the pore structure is rich and the adsorption capacity is strong.
Description
Technical Field
The invention belongs to the technical field of biomass activated carbon, and particularly relates to a preparation method of jatropha curcas based biomass activated carbon.
Background
The active carbon has a porous structure and a higher specific surface area, has large adsorption capacity, high speed and good physical and chemical stability, and is one of the most widely used adsorption materials at present. The jatropha curcas is an ideal biodiesel resource plant, belongs to renewable energy, and has wide comprehensive utilization prospect. The leaf, stem and shell of Jatropha curcas contain various biological medicinal sources, and can be extracted after being pulverized to prepare biological medicines and biological pesticides. Especially, the Jatropha curcas leaves produce 0.3 ton of leaves per mu per year, the extraction amount of crude alkaloid can reach five to ten thousandths, and the extracted crude alkaloid is used for biological pesticides and biological pharmacy and has extremely high additional value. However, the extracted slag is usually used for composting, so that visible profits cannot be generated, and closed-loop development of downstream products of jatropha curcas cannot be realized. The invention provides a method for preparing biomass activated carbon by taking the residue obtained after extraction of the leaves, branches or shells of jatropha curcas as a biomass carbon source and taking the jatropha curcas residue as a raw material, and the method has important scientific significance and application prospects in the fields of environmental protection, chemical engineering, medicines and the like.
Disclosure of Invention
In order to solve the problems that the slag after the alkaloid is extracted from the jatropha curcas leaves is used for composting, visible profit cannot be generated, and closed loop development of downstream products of the jatropha curcas cannot be realized, the invention provides the method for preparing the biomass activated carbon from the slag after the alkaloid is extracted from the jatropha curcas leaves. Phosphoric acid is used as an activating agent, a phosphoric acid solution and the jatropha curcas slag are mixed according to a certain liquid-solid ratio, the concentration of the phosphoric acid, the activation temperature, the dipping time and the ultrasonic wave applied power are adjusted, and the jatropha curcas based biomass activated carbon material is successfully prepared. The prepared active carbon has large specific surface area, rich pore structure and strong adsorption capacity, and can be used in the fields of environmental protection, chemical industry, medicine and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of jatropha curcas based biomass activated carbon comprises the following steps:
Step 1: cleaning the Jatropha curcas base slag, and drying for later use;
Step 2: putting the jatropha curcas base slag into a phosphoric acid solution, uniformly mixing, dipping, introducing power ultrasonic waves for mixing and activating in the dipping process, and obtaining a sample a after dipping;
And step 3: putting the sample a into an oven for drying until the weight of the sample a does not change any more, and obtaining a sample b;
And 4, step 4: putting the sample b into a chemical activation furnace, and gradually heating to 500-850 ℃ for activation under the protection of nitrogen;
And 5: and repeatedly washing the activated sample by using deionized water until the sample is neutral, drying the sample to constant weight, and grinding and sieving the sample to obtain an activated carbon product.
Further, in the step 1, the jatropha curcas base slag is slag obtained by crushing and extracting jatropha curcas leaves, jatropha curcas branches or jatropha curcas shells.
further, in the step 1, the drying temperature is 90-105 ℃.
further, in the step 2, in the dipping process, the ultrasonic frequency is 100Hz, the ultrasonic power is 0-100W, and the ultrasonic time is 0-24 hours.
further, in the step 2, mixing the jatropha curcas base slag charge and the phosphoric acid solution according to the mass ratio of 1: 3-3: 1.
Further, in the step 2, the mass fraction of the solute in the phosphoric acid solution is 40-60%, and the dipping time is 18-48 h.
Further, in step 3, the temperature of oven drying is 90-105 ℃.
Further, in step 4, the activation furnace is a muffle furnace or a program-controlled box-type electric furnace.
Further, in step 4, the temperature of the chemical activation furnace is increased at a temperature increase rate of 2-4 ℃/min.
Further, in the step 4, the activation time is 60-180 min.
Compared with the prior art, the invention has the beneficial effects that:
1. The invention provides a preparation method for preparing bio-based activated carbon by taking jatropha curcas-based slag charge as a raw material. In the dipping process, ultrasonic vibration is introduced, so that the reaction of slag and phosphoric acid is more sufficient, and the activation reaction is more thorough.
2. On the basis of phosphoric acid pretreatment, phosphoric acid is adopted as an activating agent, a phosphoric acid solution and jatropha curcas slag are mixed according to a certain liquid-solid ratio, the concentration of the phosphoric acid, the activation temperature, the dipping time and the ultrasonic wave applied power are adjusted, and the jatropha curcas based biomass activated carbon material is successfully prepared. Wherein, the dipping ratio of the phosphoric acid and the slag charge, the dipping time, the ultrasonic power and the application time, the high-temperature activation temperature, the activation time and the like influence the pore structure of the activated carbon. The ultrasonic vibration improves the contact area of the phosphoric acid and the slag charge, accelerates the activation time and improves the activation efficiency.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Example 1
The preparation method of the jatropha curcas based biomass activated carbon with high specific surface area comprises the following steps:
Step 1: crushing Jatropha curcas shells, extracting alkaloid, washing the Jatropha curcas base slag, and drying at 90 ℃;
Step 2: preparing a phosphoric acid solution with the phosphoric acid mass fraction of 50%, setting the mass ratio of the jatropha curcas base slag charge to the phosphoric acid solution to be 1:2, and soaking for 24 hours. In the dipping process, power ultrasonic wave is introduced for mixing and activation, the ultrasonic frequency is 100Hz, the ultrasonic power is 100W, the ultrasonic time is 12 hours, and the ultrasonic action mode is intermittent application. Obtaining a sample a after the impregnation is finished;
And step 3: putting the sample a into a 100 ℃ oven, and drying for 10 hours until the weight of the sample a does not change any more to obtain a sample b;
and 4, step 4: putting the sample b into a muffle furnace, heating to 500 ℃ at the heating rate of 2 ℃/min under the protection of nitrogen, and activating for 180 min;
And 5: and repeatedly washing the sample after cremation by using deionized water until the sample is neutral, drying the sample until the sample is constant in weight, and grinding and sieving the sample to obtain an activated carbon product.
The biomass activated carbon prepared by the method has the specific surface area of 1350 square meters per gram, the average pore diameter of 3.2nm and the total pore volume of 1.1m3the activated carbon has good adsorption effect and can be used as an environment-friendly low-cost adsorbent.
example 2
A preparation method of jatropha curcas based biomass activated carbon comprises the following steps:
step 1: the jatropha curcas base slag charge after the jatropha curcas shells are crushed and the alkaloid is extracted is cleaned and dried at the temperature of 100 ℃.
Step 2: preparing a phosphoric acid solution with 48% of phosphoric acid by mass, setting the mass ratio of the jatropha curcas base slag charge to the phosphoric acid solution to be 1:1, and soaking for 18 hours. In the dipping process, power ultrasonic wave is introduced for mixing and activation, the ultrasonic frequency is 100Hz, the ultrasonic power is 80W, the ultrasonic time is 10 hours, and the ultrasonic action mode is intermittent application. Sample a was obtained after completion of the impregnation.
And step 3: putting the sample a into a 100 ℃ oven, and drying for 10 hours until the weight of the sample a does not change any more to obtain a sample b;
And 4, step 4: and (3) putting the sample b into a muffle furnace, heating to 600 ℃ at the heating rate of 4 ℃/min under the protection of nitrogen, and activating for 100 min.
and 5: and repeatedly washing the sample after cremation by using deionized water until the sample is neutral, drying the sample until the sample is constant in weight, and grinding and sieving the sample to obtain an activated carbon product.
The biomass activated carbon prepared by the method has the specific surface area of 1000 square meters per gram, can effectively absorb heavy metal ions, and is a good resource recycling of jatropha curcas leaves.
example 3
a preparation method of jatropha curcas based biomass activated carbon comprises the following steps:
Step 1: the jatropha curcas base slag charge after the jatropha curcas shells are crushed and the alkaloid is extracted is cleaned and dried at 105 ℃.
step 2: preparing a phosphoric acid solution with the phosphoric acid mass fraction of 50%, setting the mass ratio of the jatropha curcas base slag charge to the phosphoric acid solution to be 1:2, and soaking for 48 hours. In the dipping process, power ultrasonic wave is introduced for mixing and activation, the ultrasonic frequency is 100Hz, the ultrasonic power is 100W, the ultrasonic time is 24 hours, and the ultrasonic action mode is intermittent application. Sample a was obtained after completion of the impregnation.
and step 3: putting the sample a into a 90 ℃ oven, and drying for 10 hours until the weight of the sample a does not change any more to obtain a sample b;
and 4, step 4: and (3) putting the sample b into a program-controlled box type electric furnace, heating to 600 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen, and activating for 100 min.
And 5: and repeatedly washing the sample after cremation by using deionized water until the sample is neutral, drying the sample until the sample is constant in weight, and grinding and sieving the sample to obtain an activated carbon product.
The biomass activated carbon prepared by the method has the specific surface area of 900 square meters per gram, has a good formaldehyde adsorption effect, and provides some reference basis for resource utilization of jatropha curcas branches.
example 4
a preparation method of jatropha curcas based biomass activated carbon comprises the following steps:
Step 1: the jatropha curcas base slag charge after the jatropha curcas shells are crushed and the alkaloid is extracted is cleaned and dried at the temperature of 95 ℃.
step 2: preparing a phosphoric acid solution with the phosphoric acid mass fraction of 60%, setting the mass ratio of the jatropha curcas base slag charge to the phosphoric acid solution to be 1:3, and soaking for 18 hours. In the dipping process, power ultrasonic wave is introduced for mixing and activation, the ultrasonic frequency is 100Hz, the ultrasonic power is 80W, the ultrasonic time is 10 hours, and the ultrasonic action mode is intermittent application. Sample a was obtained after completion of the impregnation.
And step 3: putting the sample a into a 100 ℃ oven, and drying for 10 hours until the weight of the sample a does not change any more to obtain a sample b;
and 4, step 4: and (3) putting the sample b into a muffle furnace, heating to 600 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen, and activating for 100 min.
And 5: and repeatedly washing the sample after cremation by using deionized water until the sample is neutral, drying the sample until the sample is constant in weight, and grinding and sieving the sample to obtain an activated carbon product.
the biomass activated carbon prepared by the method has the specific surface area of 1100 square meters per gram, can effectively absorb heavy metal ions, and is a good resource recycle of jatropha curcas leaves.
Example 5
a preparation method of jatropha curcas based biomass activated carbon comprises the following steps:
Step 1: the jatropha curcas base slag charge after the jatropha curcas shells are crushed and the alkaloid is extracted is cleaned and dried at the temperature of 95 ℃.
Step 2: preparing a phosphoric acid solution with the phosphoric acid mass fraction of 40%, setting the mass ratio of the jatropha curcas base slag charge to the phosphoric acid solution to be 3:1, and soaking for 18 hours. In the dipping process, power ultrasonic wave is introduced for mixing and activation, the ultrasonic frequency is 100Hz, the ultrasonic power is 1W, the ultrasonic time is 1 hour, and the ultrasonic action mode is intermittent application. Sample a was obtained after completion of the impregnation.
And step 3: putting the sample a into a 105 ℃ oven, and drying for 10 hours until the weight of the sample a does not change any more to obtain a sample b;
and 4, step 4: and (3) putting the sample b into a muffle furnace, heating to 850 ℃ at the heating rate of 3 ℃/min under the protection of nitrogen, and activating for 60 min.
And 5: and repeatedly washing the sample after cremation by using deionized water until the sample is neutral, drying the sample until the sample is constant in weight, and grinding and sieving the sample to obtain an activated carbon product.
The biomass activated carbon prepared by the method has the specific surface area of 800 square meters per gram, can effectively absorb heavy metal ions, and is a good resource recycle of jatropha curcas leaves.
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of jatropha curcas based biomass activated carbon is characterized by comprising the following steps:
Step 1: cleaning the Jatropha curcas base slag, and drying for later use;
Step 2: putting the jatropha curcas base slag into a phosphoric acid solution, uniformly mixing, dipping, introducing power ultrasonic waves for mixing and activating in the dipping process, and obtaining a sample a after dipping;
and step 3: putting the sample a into an oven for drying until the weight of the sample a does not change any more, and obtaining a sample b;
and 4, step 4: putting the sample b into a chemical activation furnace, and gradually heating to 500-850 ℃ for activation under the protection of nitrogen;
And 5: and repeatedly washing the activated sample by using deionized water until the sample is neutral, drying the sample to constant weight, and grinding and sieving the sample to obtain an activated carbon product.
2. The method for preparing a jatropha curcas based biomass activated carbon as claimed in claim 1, wherein in step 1, the jatropha curcas based slag is extracted from crushed jatropha curcas leaves, jatropha curcas branches or jatropha curcas shells.
3. The method for preparing jatropha curcas based biomass activated carbon as claimed in claim 1, wherein in step 1, the drying temperature is 90-105 ℃.
4. The method for preparing jatropha curcas based biomass activated carbon as claimed in claim 1, wherein in the step 2, in the impregnation process, the ultrasonic frequency is 100Hz, the ultrasonic power is 0-100W, and the ultrasonic time is 0-24 hours.
5. The preparation method of the jatropha curcas based biomass activated carbon according to claim 1, wherein in the step 2, the jatropha curcas based slag and the phosphoric acid solution are mixed according to the mass ratio of 1: 3-3: 1.
6. The preparation method of jatropha curcas based biomass activated carbon as claimed in claim 1, wherein in step 2, the mass fraction of the solute in the phosphoric acid solution is 40% -60%, and the impregnation time is 18-48 h.
7. The method for preparing jatropha curcas based biomass activated carbon as claimed in claim 1, wherein the temperature of oven drying in step 3 is 90-105 ℃.
8. The method for preparing jatropha curcas based biomass activated carbon according to claim 1, wherein in step 4, the activation furnace is a muffle furnace or a programmed box type electric furnace.
9. the method for preparing jatropha curcas based biomass activated carbon as claimed in claim 1, wherein in step 4, the temperature of the chemical activation furnace is raised at a rate of 2-4 ℃/min.
10. The method for preparing jatropha curcas based biomass activated carbon as claimed in claim 1, wherein in step 4, the activation time is 60-180 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116812909A (en) * | 2023-06-30 | 2023-09-29 | 河海大学 | Preparation method of phosphorus-doped porous biochar and application of phosphorus-doped porous biochar in electrocatalytic production of hydrogen peroxide |
| CN118696839A (en) * | 2024-07-31 | 2024-09-27 | 广西大学 | A kind of deodorizing and antibacterial cat litter and preparation method thereof |
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| CN102583369A (en) * | 2012-01-12 | 2012-07-18 | 江西师范大学 | Method for preparing powdered activated carbon from longan seeds |
| CN102659101A (en) * | 2012-01-12 | 2012-09-12 | 江西师范大学 | Method for preparing activated carbon from longan shells |
| CN108059159A (en) * | 2018-01-18 | 2018-05-22 | 中国石油大学(华东) | A kind of method for preparing high-performance biomass activated carbon |
-
2019
- 2019-10-30 CN CN201911045448.4A patent/CN110577221A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717084A (en) * | 2009-12-09 | 2010-06-02 | 昆明理工大学 | Method for preparing mesoporous activated carbon by using jatropha curcas shells |
| CN102583369A (en) * | 2012-01-12 | 2012-07-18 | 江西师范大学 | Method for preparing powdered activated carbon from longan seeds |
| CN102659101A (en) * | 2012-01-12 | 2012-09-12 | 江西师范大学 | Method for preparing activated carbon from longan shells |
| CN108059159A (en) * | 2018-01-18 | 2018-05-22 | 中国石油大学(华东) | A kind of method for preparing high-performance biomass activated carbon |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116812909A (en) * | 2023-06-30 | 2023-09-29 | 河海大学 | Preparation method of phosphorus-doped porous biochar and application of phosphorus-doped porous biochar in electrocatalytic production of hydrogen peroxide |
| CN118696839A (en) * | 2024-07-31 | 2024-09-27 | 广西大学 | A kind of deodorizing and antibacterial cat litter and preparation method thereof |
| CN118696839B (en) * | 2024-07-31 | 2025-12-19 | 广西大学 | Deodorization and bacteriostasis cat litter and preparation method thereof |
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Application publication date: 20191217 |