CN110002446A - A kind of method and product preparing active carbon using biomass castoff - Google Patents
A kind of method and product preparing active carbon using biomass castoff Download PDFInfo
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- CN110002446A CN110002446A CN201910068608.0A CN201910068608A CN110002446A CN 110002446 A CN110002446 A CN 110002446A CN 201910068608 A CN201910068608 A CN 201910068608A CN 110002446 A CN110002446 A CN 110002446A
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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
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Abstract
The invention belongs to biomass to recycle field, and disclose a kind of method and product that active carbon is prepared using biomass castoff.Biomass is crushed and obtains powdered biomass by this method, then the powdered biomass is placed in air atmosphere and pre-processes a period of time at 100 DEG C~130 DEG C, preprocessing biomass is made, preprocessing biomass and activator are sufficiently mixed again, it heats under an inert atmosphere and heat preservation for a period of time, obtains intermediate product after cooling at such a temperature;After the abundant pickling of intermediate product, it is washed with deionized water to neutrality, the active carbon is obtained after drying.The present invention by pre-processing biomass at low temperature, dry the inherent water in biomass completely, more activation sites are generated by the way that dehydroxylation and decarboxylized reaction occurs, it is then had into high-specific surface area and gap structure active carbon abundant with activator Hybrid Heating to generate again.
Description
Technical field
The invention belongs to biomass to recycle field, prepare activity using biomass castoff more particularly, to a kind of
The method and product of charcoal.
Background technique
Active carbon is a kind of with flourishing pore structure, biggish specific surface area and surface chemistry group abundant, and
And the general designation of the stronger Carbon Materials of adsorption capacity.Common active carbon is prepared by coal tar, biomass or other carbon materials.Mesh
Before, active carbon is essential in the market in the multiple fields extensive application such as petrochemical industry, medicine or even aerospace
Functional form material.In recent years, with the fast development of the industries such as environmental protection, new energy, the market demand of functional competence charcoal is increased sharply,
Still there is very huge demand in market to the active carbon with high-specific surface area or high absorption property.
Biomass is as a kind of the most abundant resource of reserves in renewable carbon resource, before being a kind of very ideal active carbon
Drive body.But the shortcomings that biomass and its waste are due to itself high-moisture high volatile, when leading to practical application there is
The practical problems such as yield is low, and carbon utilisation rate is low.Therefore, biomass is improved using usually requiring to be pre-processed to biomass
Quality.
Common biomass pretreatment mode has very much, such as hydro-thermal charing, bakes and is pyrolyzed, wherein baking and being pyrolyzed
Journey mainly promotes the carbon content and fixed carbon content of solid by effectively removing moisture and a part of volatile matter, to prepare
Coke best in quality out;And hydro-thermal charing then using the water in airtight chamber in critical state to the peptizaiton of biomass come
The decomposition and recombination for promoting biomass functional group, finally prepare moisture and are substantially reduced, the hydro-thermal charcoal that carbon content is obviously improved.But
It is that the temperature that these three modes need is relatively high, reaction temperature generally selects 300 DEG C~500 DEG C or so at least at 200 DEG C or more
Reaction condition, although obtain coke quality it is higher, need very high Energy input simultaneously, economy is slightly poor.
Summary of the invention
For the disadvantages mentioned above and/or Improvement requirement of the prior art, biomass castoff is utilized the present invention provides a kind of
The method and product of active carbon are prepared, wherein accordingly can be improved active carbon by the Cold pretreatment technique for increasing biomass
Specific surface area, be therefore particularly suitable for preparing the application of active carbon etc.
To achieve the above object, according to one aspect of the present invention, a kind of prepare using biomass castoff is proposed to live
The method of property charcoal, which is characterized in that the preparation method includes the following steps:
(a) by the broken acquisition powdered biomass of biomass, then the powdered biomass is placed in air atmosphere and 100
DEG C~130 DEG C at pre-process a period of time, be made preprocessing biomass;
(b) preprocessing biomass that step (a) obtains is sufficiently mixed with activator, is then heated under an inert atmosphere simultaneously
Heat preservation a period of time at such a temperature obtains intermediate product after cooling;
(c) it after the abundant pickling of intermediate product for obtaining step (b), is washed with deionized water to neutrality, institute is obtained after drying
State active carbon.
As it is further preferred that biomass is preferably peanut shell, rice straw or sawdust in the step (a).
As it is further preferred that the pretreated time is preferably 1h~for 24 hours in the step (a).
As it is further preferred that activator is preferably sodium hydroxide in the step (b), potassium hydroxide, sodium bicarbonate,
Saleratus, iron chloride, zinc chloride, phosphoric acid or sulfuric acid.
As it is further preferred that preprocessing biomass and activator are preferably with the matter of 1:1~1:4 in the step (b)
Amount is than mixing.
As it is further preferred that the temperature program of heating process is with 3 DEG C/min~7 DEG C/min in the step (b)
Heating rate rise to 700 DEG C~900 DEG C from room temperature.
As it is further preferred that the time kept the temperature in the step (b) is preferably 1h~4h.
As it is further preferred that the reagent of pickling is preferably hydrochloric acid in the step (c), concentration is preferably
0.5mol/L~6mol/L.
It is another aspect of this invention to provide that providing a kind of active carbon prepared using the above method.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit:
1. the present invention is dried the inherent water in biomass completely, is led to by pre-processing biomass at low temperature
It crosses generation dehydroxylation and decarboxylized reaction generates more activation sites, then again generate it with activator Hybrid Heating
With high-specific surface area and gap structure active carbon abundant;
2. preprocessing process medium temperature is spent, low or pretreatment time is too short all can not to make inherent water dry completely, to reduce
Dehydroxylation and decarboxylized generation, cause the activation problem that site is less thus active carbon quality is lower, and preprocessing process
Medium temperature, which spends height, will cause biomass half cellulose decomposition, and yield reduces, increased costs, and drying time is too long also will increase
Manufacturing cost, therefore after biomass to be pre-processed to 1h~for 24 hours at 100 DEG C~130 DEG C, then with activator with the matter of 1:1~1:4
Amount keeps the temperature 1h~4h than mixing at 700 DEG C~900 DEG C, and available specific surface area reaches as high as 3317.7m2The activity of/g
Charcoal.
Detailed description of the invention
Fig. 1 is the process flow chart provided by the invention that active carbon is prepared using biomass castoff.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
As shown in Figure 1, the present invention provides a kind of method for preparing active carbon using biomass castoff, feature exists
In the preparation method includes the following steps:
(a) by biomass (such as peanut shell, rice straw or sawdust) broken acquisition powdered biomass, then by the powdered biomass
It is placed in air atmosphere, and pre-processes 1h~for 24 hours at 100 DEG C~130 DEG C, preprocessing biomass is made;
(b) preprocessing biomass and activator that step (a) obtains are sufficiently mixed with the mass ratio of 1:1~1:4, then
It heats under an inert atmosphere and keeps the temperature 1h~4h at such a temperature, it is finally cooling under an inert atmosphere to obtain intermediate product;
(c) it after the abundant pickling of intermediate product for obtaining step (c), is washed with deionized water to neutrality, institute is obtained after drying
State active carbon.
Further, activator is preferably sodium hydroxide in the step (b), potassium hydroxide, sodium bicarbonate, saleratus,
Iron chloride, zinc chloride, phosphoric acid or sulfuric acid, the temperature program of heating process are with 3 DEG C/min~7 DEG C/min heating rate from room
Temperature rise is to 700 DEG C~900 DEG C.
Further, the reagent of pickling is preferably hydrochloric acid in the step (c), and concentration is preferably 0.5mol/L~6mol/
L。
It is another aspect of this invention to provide that providing a kind of active carbon prepared using the above method.
Now for specifically preparation method and the product of active carbon using biomass castoff, the present invention is made further
Detailed description.
Embodiment 1
(a) by the broken acquisition peanut shell powder of peanut shell, then the peanut shell powder is placed under 100 DEG C of air atmosphere
1h is pre-processed, pretreatment peanut shell is made;
(b) pretreatment peanut shell and sodium hydroxide that step (a) obtains are sufficiently mixed with the mass ratio of 1:1, are then put
Enter in tube furnace, is heated to 700 DEG C from room temperature with the heating rate of 5 DEG C/min under an inert atmosphere, keeps the temperature 4h at such a temperature
After be cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 1mol/L the abundant pickling of hydrochloric acid after, be washed with deionized water
To neutrality, the active carbon is obtained after drying, is denoted as C-1.
BET characterization is carried out to the C-1, the specific surface area for obtaining the C-1 is 785.6m2/ g, total pore volume 0.3452cm3/
G, average pore size 1.8546nm.
Embodiment 2
(a) by the broken acquisition peanut shell powder of peanut shell, then the peanut shell powder is placed under 100 DEG C of air atmosphere
For 24 hours, pretreatment peanut shell is made in pretreatment;
(b) pretreatment peanut shell and sodium hydroxide that step (a) obtains are sufficiently mixed with the mass ratio of 1:1, are then put
Enter in tube furnace, is heated to 700 DEG C from room temperature with the heating rate of 5 DEG C/min under an inert atmosphere, keeps the temperature 4h at such a temperature
After be cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 1mol/L the abundant pickling of hydrochloric acid after, be washed with deionized water
To neutrality, the active carbon is obtained after drying, is denoted as C-2.
BET characterization is carried out to the C-2, the specific surface area for obtaining the C-2 is 1423.5m2/ g, total pore volume are
0.6432cm3/ g, average pore size 2.1625nm.
By the way that the BET characterize data of C-1 and C-2 is compared discovery, the peanut shell powder pretreated time is longer, system
The active carbon specific surface area obtained is bigger, and gap structure is more flourishing, and average pore size is bigger.
Embodiment 3
(a) by the broken acquisition rice straw powder of rice straw, then the rice straw powder is placed under 105 DEG C of air atmosphere and is pre-processed
Pretreatment rice straw is made in 14h;
(b) pretreatment rice straw and potassium hydroxide that step (a) obtains are sufficiently mixed with the mass ratio of 1:3, are then placed in
In tube furnace, 800 DEG C are heated to from room temperature with the heating rate of 7 DEG C/min under an inert atmosphere, after keeping the temperature 1h at such a temperature
It is cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 0.5mol/L the abundant pickling of hydrochloric acid after, use deionized water
It is washed till neutrality, the active carbon is obtained after drying, is denoted as C-3.
BET characterization is carried out to the C-3, the specific surface area for obtaining the C-3 is 3028.9m2/ g, total pore volume are up to
1.7936cm3/ g, average pore size are up to 2.2225nm.
Embodiment 4
(a) by the broken acquisition rice straw powder of rice straw, then the rice straw powder is placed under 130 DEG C of air atmosphere and is pre-processed
Pretreatment rice straw is made in 14h;
(b) pretreatment rice straw and potassium hydroxide that step (a) obtains are sufficiently mixed with the mass ratio of 1:3, are then placed in
In tube furnace, 800 DEG C are heated to from room temperature with the heating rate of 7 DEG C/min under an inert atmosphere, after keeping the temperature 1h at such a temperature
It is cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 0.5mol/L the abundant pickling of hydrochloric acid after, use deionized water
It is washed till neutrality, the active carbon is obtained after drying, is denoted as C-4.
BET characterization is carried out to the C-4, the specific surface area for obtaining the C-4 is 3287.5m2/ g, total pore volume are up to
1.8526cm3/ g, average pore size are up to 2.2395nm.
Embodiment 5
(a) by the broken acquisition rice straw powder of rice straw, then the rice straw powder is placed under 130 DEG C of air atmosphere and is pre-processed
Pretreatment rice straw is made in 14h;
(b) pretreatment rice straw and potassium hydroxide that step (a) obtains are sufficiently mixed with the mass ratio of 1:3, are then placed in
In tube furnace, 900 DEG C are heated to from room temperature with the heating rate of 7 DEG C/min under an inert atmosphere, after keeping the temperature 1h at such a temperature
It is cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 0.5mol/L the abundant pickling of hydrochloric acid after, use deionized water
It is washed till neutrality, the active carbon is obtained after drying, is denoted as C-5.
BET characterization is carried out to the C-5, the specific surface area for obtaining the C-5 is 3317.7m2/ g, total pore volume are up to
1.9233cm3/ g, average pore size are up to 2.2612nm.
It is found by the way that the BET characterization result of C-3, C-4 and C-5 are compared analysis, the temperature in preprocessing process is got over
Temperature is higher in high or heating process, and the active carbon specific surface area of acquisition is bigger, and gap structure structure is more flourishing, average pore size
It is bigger.
Embodiment 6
(a) by the broken acquisition pine sawdust powder of pine sawdust, then which is placed in 110 DEG C of air
5h is pre-processed under atmosphere, pretreatment pine sawdust is made;
(b) pretreatment pine sawdust and iron chloride that step (a) obtains are sufficiently mixed with the mass ratio of 1:2, are then put
Enter in tube furnace, is heated to 800 DEG C from room temperature with the heating rate of 3 DEG C/min under an inert atmosphere, keeps the temperature 2h at such a temperature
After be cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 6mol/L the abundant pickling of hydrochloric acid after, be washed with deionized water
To neutrality, the active carbon is obtained after drying, is denoted as C-6.
BET characterization is carried out to the C-6, the specific surface area for obtaining the C-6 is 769.2m2/ g, total pore volume are up to
0.4958cm3/ g, average pore size are up to 2.3512nm.
Embodiment 7
(a) by the broken acquisition pine sawdust powder of pine sawdust, then which is placed in 110 DEG C of air
5h is pre-processed under atmosphere, pretreatment pine sawdust is made;
(b) pretreatment pine sawdust and iron chloride that step (a) obtains are sufficiently mixed with the mass ratio of 1:4, are then put
Enter in tube furnace, is heated to 800 DEG C from room temperature with the heating rate of 3 DEG C/min under an inert atmosphere, keeps the temperature 2h at such a temperature
After be cooled to room temperature acquisition intermediate product;
(c) by step (c) obtain intermediate product with concentration be 6mol/L the abundant pickling of hydrochloric acid after, be washed with deionized water
To neutrality, the active carbon is obtained after drying, is denoted as C-7.
BET characterization is carried out to the C-7, the specific surface area for obtaining the C-7 is 835.2m2/ g, total pore volume are up to
0.5458cm3/ g, average pore size are up to 2.1512nm.
It is found by the way that the characterization result of C-6 and C-7 are carried out analysis, the adding proportion of activator is higher, activity obtained
Charcoal specific surface area is bigger, and gap structure structure is more flourishing, and average pore size is bigger.
Comparative example 1
(a) screening obtains peanut shell powder after being crushed peanut shell, then by the peanut shell powder and sodium hydroxide with 1:1
Mass ratio be fully ground mixing, be then placed in tube furnace, added under an inert atmosphere with the heating rate of 5 DEG C/min from room temperature
Heat is cooled to room temperature acquisition intermediate product after keeping the temperature 4h at such a temperature to 700 DEG C;
(b) by step (a) obtain intermediate product with concentration be 1mol/L the abundant pickling of hydrochloric acid after, be washed with deionized water
To neutrality, the active carbon is obtained after drying, is denoted as C-8.
BET characterization is carried out to the C-8, the specific surface area for obtaining the C-8 is 610.5m2/ g, total pore volume 0.2739cm3/
G, average pore size 1.7946nm.
Comparative example 2
(a) screening obtains rice straw powder after being crushed rice straw, then by the rice straw powder and potassium hydroxide with the quality of 1:3
Than being fully ground mixing, it is then placed in tube furnace, 900 DEG C is heated to from room temperature with the heating rate of 7 DEG C/min, in the temperature
Acquisition intermediate product is cooled to room temperature after lower heat preservation 1h;
(b) by step (a) obtain intermediate product with concentration be 0.5mol/L the abundant pickling of hydrochloric acid after, use deionized water
It is washed till neutrality, the active carbon is obtained after drying, is denoted as C-9.
BET characterization is carried out to the C-9, the specific surface area for obtaining the C-9 is 2965.6m2/ g, total pore volume are
1.3309cm3/ g, average pore size 1.7948nm.
Comparative example 3
(a) screening obtains pine sawdust powder after being crushed pine sawdust, then by the sawdust powder and iron chloride with 1:4
Mass ratio be fully ground mixing, be then placed in tube furnace, be heated to 800 DEG C from room temperature with the heating rate of 3 DEG C/min,
Acquisition intermediate product is cooled to room temperature after keeping the temperature 2h at this temperature;
(b) by step (a) obtain intermediate product with concentration be 6mol/L the abundant pickling of hydrochloric acid after, be washed with deionized water
To neutrality, the active carbon is obtained after drying, is denoted as C-10.
BET characterization is carried out to the C-10, the specific surface area for obtaining the C-10 is 722m2/ g, total pore volume 0.4671cm3/
G, average pore size 2.5877nm.
The BET characterization result of C-1 and C-8, C-5 and C-9, C-7 and C-10 are compared discovery respectively, biomass is passed through
The active carbon prepared after pretreatment specific surface area compared with the active carbon prepared after without pretreatment is bigger, and pore structure is more sent out
It reaches and average pore size is also bigger, this explanation is more advantageous to preparation with activator Hybrid Heating again after being pre-processed biomass
Active carbon with high-specific surface area.
The especially inherent water of moisture in biomass mainly exists in the form of hydroxyl and carboxyl, passes through in preprocessing process
Low-temperature heat is carried out to biomass, the generation of dehydroxylation and decarboxylation reaction is promoted, to provide more work for biomass
Change site, the generation of the increase of specific surface area and pore structure when being conducive to prepare active carbon, therefore temperature in preprocessing process
Higher, pretreatment time is longer, and the active carbon quality of generation is higher;It is undried because biomass moisture content itself is lower
Biomass is directly contacted with activator, and impregnation occurs for a part that will lead in biomass, instead results in activation unevenly,
And pretreated powdered biomass is substantially free of moisture, reduces the maceration of activator, is conducive to keep reaction more equal
It is even;In addition, small amounts effect and devolatilization also has occurred in powdered biomass in preprocessing process, be conducive to subsequent anti-
The expansion and intensification for answering middle hole, are conducive to mesoporous generation.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (9)
1. a kind of method for preparing active carbon using biomass castoff, which is characterized in that the preparation method includes the following steps:
(a) obtain powdered biomass for biomass is broken, then by the powdered biomass be placed in air atmosphere and 100 DEG C~
A period of time is pre-processed at 130 DEG C, and preprocessing biomass is made;
(b) preprocessing biomass that step (a) obtains is sufficiently mixed with activator, is then heated under an inert atmosphere and at this
At a temperature of keep the temperature a period of time, obtain intermediate product after cooling;
(c) it after the abundant pickling of intermediate product for obtaining step (b), is washed with deionized water to neutrality, the work is obtained after drying
Property charcoal.
2. the method for preparing active carbon using biomass castoff as described in claim 1, which is characterized in that the step
(a) biomass is preferably peanut shell, rice straw or sawdust in.
3. the method for preparing active carbon using biomass castoff as claimed in claim 1 or 2, which is characterized in that the step
Suddenly the pretreated time is preferably 1h~for 24 hours in (a).
4. the method as claimed in any one of claims 1 to 3 for preparing active carbon using biomass castoff, which is characterized in that
Activator is preferably sodium hydroxide, potassium hydroxide, sodium bicarbonate, saleratus, iron chloride, zinc chloride, phosphorus in the step (b)
Acid or sulfuric acid.
5. such as the described in any item methods for preparing active carbon using biomass castoff of Claims 1 to 4, which is characterized in that
Preprocessing biomass is preferably mixed with activator with the mass ratio of 1:1~1:4 in the step (b).
6. the method as claimed in any one of claims 1 to 5 for preparing active carbon using biomass castoff, which is characterized in that
The temperature program of heating process is to rise to 700 DEG C from room temperature with 3 DEG C/min~7 DEG C/min heating rate in the step (b)
~900 DEG C.
7. the method as described in any one of claims 1 to 6 for preparing active carbon using biomass castoff, which is characterized in that
The time kept the temperature in the step (b) is preferably 1h~4h.
8. the method as described in any one of claims 1 to 7 for preparing active carbon using biomass castoff, which is characterized in that
The reagent of pickling is preferably hydrochloric acid in the step (c), and concentration is preferably 0.5mol/L~6mol/L.
9. a kind of active carbon using such as the method preparation of any one of claim 1~8.
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CN110615435A (en) * | 2019-10-29 | 2019-12-27 | 西南大学 | Preparation method and application of biomass activated carbon material |
CN110918061A (en) * | 2019-12-17 | 2020-03-27 | 甘肃农业大学 | Biomass waste activated carbon, preparation method thereof and application of biomass waste activated carbon in treatment of nitrophenol compounds in wastewater |
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CN110615435A (en) * | 2019-10-29 | 2019-12-27 | 西南大学 | Preparation method and application of biomass activated carbon material |
CN110918061A (en) * | 2019-12-17 | 2020-03-27 | 甘肃农业大学 | Biomass waste activated carbon, preparation method thereof and application of biomass waste activated carbon in treatment of nitrophenol compounds in wastewater |
CN114162818A (en) * | 2020-09-10 | 2022-03-11 | 宝武炭材料科技有限公司 | Preparation method, material and application of porous carbon electrode material |
CN112374497A (en) * | 2020-11-30 | 2021-02-19 | 中国矿业大学 | Preparation method of porous carbonized wood chip packed bed material based on alkali activation and application of porous carbonized wood chip packed bed material in aspect of solar seawater desalination |
CN113000041A (en) * | 2021-02-26 | 2021-06-22 | 上海大学材料基因组工程(萍乡)研究院 | Regeneration method of waste activated carbon by using biomass |
CN113694885A (en) * | 2021-07-20 | 2021-11-26 | 红河学院 | Biological activated carbon-loaded hydroxyapatite composite material and application method thereof |
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