CN103350994B - Specific surface area and the controlled micro-meso-porous carbon material preparation method of pore volume and micro-meso-porous carbon material - Google Patents
Specific surface area and the controlled micro-meso-porous carbon material preparation method of pore volume and micro-meso-porous carbon material Download PDFInfo
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Abstract
The invention discloses a kind of specific surface area and the controlled micro-meso-porous carbon material preparation method of pore volume and micro-meso-porous carbon material obtained by this method, the method makes it that crosslinking reaction occur after first polysiloxane precursor being heated, and obtains carbon matrix precursor after then carrying out fragmentation, Pintsch process, ball milling; Recycling carbide-derived carbon method carries out chlorination etching, obtains containing the micro-meso-porous carbon material of Cl; Finally adopt ammonia or hydrogen to carry out aftertreatment, obtain not containing micro-meso-porous carbon material of Cl.The specific surface area of micro-meso-porous carbon material of the present invention is 1016 ~ 2950m
2/ g, mean pore size is 1.8 ~ 9.4nm, and pore capacities is 0.521 ~ 2.567cc/g, and micropore hole content is 0.160 ~ 1.125cc/g, and mesoporous hole content is 0.035 ~ 2.110cc/g.The present invention has the advantages such as cost is low, processing step is easy, preparation temperature is low, good moldability, product performance are controlled.
Description
Technical field
The present invention relates to a kind of preparation of carbon material, particularly relate to a kind of micro-meso-porous carbon material product and preparation method thereof.
Background technology
Nanoporous carbon materials (Nanoporous Carbon is called for short " NPC ") refers to a class carbon material with nano pore structure, and aperture is generally less than 100nm.Porous carbon can be divided into microporous carbon (Micropore according to pore size, ≤ 2nm), mesoporous carbon (Mesopore, 2nm ~ 50nm) and grand hole carbon material (Macropore, >=50nm), wherein microporous carbon can be divided into again one-level microporous carbon (<0.8nm) and secondary microporous carbon (0.8nm ~ 2nm).Porous carbon materials is primarily of C atom composition, but the impurity atoms also usually containing some trace, comprise O, H, N, S etc.Nanoporous carbon materials had both had carbonaceous material low density, high strength, the feature that good biocompatibility, chemical stability (non-oxygenated environment), excellent conductivity and workability are strong, also there is the porosity characteristics such as specific surface area is high, pore volume is large, pore passage structure is abundant, thus in fields such as electrode materials, sorbent material, lagging material, support of the catalyst, there is wide application background.
In order to cater to the growing application demand of different field, develop the not high and preparation technology that can either the microtextures such as porous carbon specific surface area, pore volume, aperture be regulated, can be finely controlled again of a kind of cost on a large scale, become an important development trend.
The method being usually used in preparing nanoporous carbon at present mainly contains carbide-derived carbon method (Carbide derived carbon is called for short CDC method), activation method (comprising Physical and chemical activation method), template (comprising hard template method and soft template method), catalytic activation method, mixed with polymers carborization and organic gel carbonization method.Wherein, CDC ratio juris etches next by etching agents such as chlorine (Cl2) by the non-carbon in carbide thus obtains porous carbon (Carbide derived carbons, represent with " CDCs "), because of it, to have carbon matrix precursor wide material sources, pore size distribution narrower and keep the advantages such as the original form of carbon matrix precursor, causes the extensive concern of this area researchist nearly ten years gradually and develop rapidly.
But existing preparation technology, comprise CDC method, all be difficult to regulate on a large scale the microtexture such as specific surface area, pore volume, aperture of carbon material, this is main because the carbon matrix precursor of current most of CDC technical study personnel is the good binary of crystallinity or double carbide, it is obtained by modes such as sintering, and mainly exist, as SiC, TiC and Ti3SiC2 etc. with the form of powder particle.And these carbide structures are more single, be difficult to regulate on a large scale CDCs.In addition, these ceramic operability are poor, are unfavorable for shaping or prepare complex component.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, there is provided that a kind of cost is low, processing step is easy, preparation temperature is low, micro-meso-porous carbon material preparation method that good moldability, the specific surface area that lower to processing unit requirement, product performance are controlled and pore volume are controlled, and micro-meso-porous carbon material that the performance providing this preparation method to obtain is better, microtexture is controllable.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is the controlled micro-meso-porous carbon material preparation method of a kind of specific surface area and pore volume, comprises the following steps:
(1) preparation of carbon matrix precursor (Si (O) C): make it that crosslinking reaction occur after polysiloxane precursor being heated, cross-linking products is carried out fragmentation, then the cross-linking products particle after fragmentation is placed in Pintsch process under inert atmosphere or vacuum atmosphere, product cool to room temperature after cracking, obtains the carbon matrix precursor that particle size range is 0.1 μm ~ 50 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method (CDC method) to carry out chlorination etching to the carbon matrix precursor that above-mentioned steps (1) obtains, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt NH
3or H
2what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl (reaction principle is: 4NH
3+ 6Cl
surf→ 2NH
4cl+N
2+ 4HCl or
, until Cl element is removed, obtain not containing micro-meso-porous carbon material of Cl.
The technical scheme of the invention described above provides a kind of novel micro-meso-porous carbon material that can obtain superhigh specific surface area, large pore volume, and by adopting above-mentioned technique of the present invention, can regulate on a large scale the specific surface area, pore volume etc. of micro-meso-porous carbon material product, the Precise control to micro-meso-porous carbon material product aperture and degree of crystallinity can also be realized.Controllability specifically realizes by following three aspects: 1) by controlling the kind, cracking temperature, cracking atmosphere, temperature rise rate, particle diameter etc. of step (1) Raw; 2) by controlling the etching temperature, time etc. in step (2); 3) by controlling the atmosphere kind, time, temperature etc. of aftertreatment in step (3).By adjusting the processing parameter of these three aspects, just can realize the control of aperture to final CDCs and carbon degree of crystallinity, specific surface area and pore volume, and regulating on a large scale.Such as will obtain the product of small-bore, atmosphere can be adopted vacuum, Pintsch process controls more than 1500 DEG C, and etching temperature need control more than 800 DEG C; Such as will obtain the product of extra specific surface area, then adopt atmosphere protection during cracking, cracking temperature controls at 1000 DEG C ~ 1300 DEG C, and etching temperature need control more than 900 DEG C.
Above-mentioned micro-meso-porous carbon material preparation method, in described step (1), described polysiloxane precursor is preferably the silicone resin containing Si-OH group.Polysiloxane in the present invention mainly with-Si-O-Si-be main chain, with R for the superpolymer that side chain is formed; Its molecular formula can be expressed as:
Wherein, R group can be saturated group (as: CH
3, C
2h
5, C
3h
7deng); Also can be unsaturated group (as: C
2h
3, C
6h
5deng); Also can be OH group etc.In the preparation process of precursor, can by controlling the chain length of R group, the character of group and the quantity of group regulate carbon content wherein.
Above-mentioned micro-meso-porous carbon material preparation method, in described step (1), the temperature of described crosslinking reaction is preferably 150 DEG C ~ 300 DEG C, and the time of crosslinking reaction is preferably 2h ~ 6h.
Above-mentioned micro-meso-porous carbon material preparation method, in described step (1), the particle size distribution range of the cross-linking products particle after fragmentation preferably controls at 150 μm ~ 250 μm.
Above-mentioned micro-meso-porous carbon material preparation method, in described step (1), inert atmosphere is preferably N
2or Ar atmosphere, under described inert atmosphere, the cracking temperature of Pintsch process preferably controls at 1000 DEG C ~ 1700 DEG C; Under described vacuum atmosphere, the cracking temperature of Pintsch process preferably controls at 1400 DEG C ~ 2000 DEG C; Heat-up rate during Pintsch process is preferably 5 DEG C/min ~ 20 DEG C/min.
Above-mentioned micro-meso-porous carbon material preparation method, the time of described Pintsch process preferably controls as 1h ~ 6h, and the time of described ball milling preferably controls as 5h ~ 40h.
Above-mentioned micro-meso-porous carbon material preparation method, in described step (2), the etching temperature of chlorination etching is preferably 750 DEG C ~ 1200 DEG C, and heat-up rate is 5 DEG C/min ~ 20 DEG C/min, reaction atmosphere is Cl2, logical N in whole chlorination etching process
2or Ar is as carrier gas.
Above-mentioned micro-meso-porous carbon material preparation method, the time of described chlorination etching is preferably 1h ~ 5h.
Above-mentioned micro-meso-porous carbon material preparation method, the treatment temp of described aftertreatment is preferably 400 DEG C ~ 800 DEG C.
Above-mentioned micro-meso-porous carbon material preparation method, the treatment time of described aftertreatment is preferably 0.5h ~ 4h.
As a total technical conceive, the present invention also provides a kind of micro-meso-porous carbon material obtained by above-mentioned preparation method, and preferably, the specific surface area of described micro-meso-porous carbon material is 1056m
2/ g ~ 2950m
2/ g, mean pore size is 1.8nm ~ 4.0nm, and pore capacities is 0.521cc/g ~ 2.567cc/g, and wherein micropore hole content is 0.430cc/g ~ 1.125cc/g, and mesoporous hole content is 0.035cc/g ~ 0.980cc/g.
Compared with prior art, the invention has the advantages that: the present invention adopts polysiloxane as raw material, transform can obtain carbon matrix precursor by cracking; By controlling the factors such as cracking temperature mechanism, cracking atmosphere and polysiloxane kind further, ratio and the microtexture of each elemental composition in carbon matrix precursor can be regulated well, and then the microtexture such as specific surface, aperture of adjustment on a large scale, accurately control CDCs, and then realize the preparation of micro-meso-porous carbon material such as superhigh specific surface area, large pore volume.The present invention is by introducing polysiloxane conversion method, not only low raw-material cost, molecule can design, and processing step is simple and easy to do, preparation temperature is lower, formability is better, require lower to processing unit, therefore, technique of the present invention also easier low cost obtains the complex component of micro-meso-porous carbon material, for the Industry Promotion of CDC technique provides guarantee.
Accompanying drawing explanation
Fig. 1 is the adsorption/desorption curve of micro-meso-porous carbon material obtained in the embodiment of the present invention 1.
Fig. 2 is the adsorption/desorption curve of micro-meso-porous carbon material obtained in the embodiment of the present invention 2.
Fig. 3 is the adsorption/desorption curve of micro-meso-porous carbon material obtained in the embodiment of the present invention 3.
Fig. 4 is the adsorption/desorption curve of micro-meso-porous carbon material obtained in the embodiment of the present invention 4.
Fig. 5 is the adsorption/desorption curve of micro-meso-porous carbon material obtained in the embodiment of the present invention 5.
Embodiment
Below in conjunction with Figure of description and specific embodiment, the invention will be further described, but protection domain not thereby limiting the invention.
Embodiment 1:
Specific surface area of the present invention and the controlled micro-meso-porous carbon material preparation method of pore volume, comprise the following steps:
(1) preparation of carbon matrix precursor: polysiloxane precursor (all using the silicone resin containing Si-OH group in each embodiment) is heated to 250 DEG C and makes it that crosslinking reaction occur, after crosslinked 4h, cross-linking products is crushed to 150 μm ~ 250 μm, then the cross-linking products particle after fragmentation is placed in pyrolyzer, and at N
2atmosphere at high temperature cracking, cracking temperature is 1200 DEG C, and heat-up rate is 5 DEG C/min, pyrolysis time 2h, and the product furnace cooling after cracking is to room temperature, then ball milling 10h, obtains the carbon matrix precursor particle that particle size range is 0.1 μm ~ 50 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method to carry out chlorination etching to the carbon matrix precursor particle that above-mentioned steps (1) obtains, chlorination is etched in atmosphere tube type stove to be carried out, and etching temperature is 900 DEG C, and heat-up rate is 5 DEG C/min, etching time is 3h, and reaction atmosphere is Cl
2, logical N in whole chlorination etching process
2as carrier gas, cool to room temperature, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt NH
3what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl, and treatment temp is 600 DEG C, treatment time 2h, until removed by Cl element, obtains not containing micro-meso-porous carbon material of Cl.
The micro-meso-porous carbon material obtained to above-mentioned the present embodiment adopts gas adsorption (BET) method to analyze its pore structure, and adsorption/desorption curve as shown in Figure 1.Known after testing, the specific surface area of micro-meso-porous carbon material of the present embodiment is 2121m
2/ g, mean pore size is 3.1nm, and pore capacities is 1.668cc/g, and wherein micropore hole content is 1.045cc/g, and mesoporous hole content is 0.490cc/g.
Embodiment 2:
Specific surface area of the present invention and the controlled micro-meso-porous carbon material preparation method of pore volume, comprise the following steps:
(1) preparation of carbon matrix precursor: polysiloxane precursor is heated to 250 DEG C and makes it that crosslinking reaction occur, after crosslinked 4h, is crushed to 150 μm ~ 250 μm, then the cross-linking products particle after fragmentation is placed in pyrolyzer by cross-linking products, and at N
2atmosphere at high temperature cracking, cracking temperature is 1600 DEG C, and heat-up rate is 5 DEG C/min, pyrolysis time 2h, and the product furnace cooling after cracking is to room temperature, then ball milling 10h, obtains the carbon matrix precursor particle that particle size range is 0.1 μm ~ 50 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method to carry out chlorination etching to the carbon matrix precursor particle that above-mentioned steps (1) obtains, chlorination is etched in atmosphere tube type stove to be carried out, and etching temperature is 900 DEG C, and heat-up rate is 15 DEG C/min, etching time is 3h, and reaction atmosphere is Cl
2, logical N in whole chlorination etching process
2as carrier gas, cool to room temperature, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt NH
3what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl, and treatment temp is 600 DEG C, treatment time 2h, until removed by Cl element, obtains not containing micro-meso-porous carbon material of Cl.
The micro-meso-porous carbon material obtained to above-mentioned the present embodiment adopts gas adsorption (BET) method to analyze its pore structure, and adsorption/desorption curve as shown in Figure 2.Known after testing, the specific surface area of micro-meso-porous carbon material of the present embodiment is 1016m
2/ g, mean pore size is 9.4nm, and pore capacities is 2.398cc/g, and wherein micropore hole content is 0.161cc/g, and mesoporous hole content is 2.106cc/g.
Embodiment 3:
Specific surface area of the present invention and the controlled micro-meso-porous carbon material preparation method of pore volume, comprise the following steps:
(1) preparation of carbon matrix precursor: polysiloxane precursor is heated to 250 DEG C and makes it that crosslinking reaction occur, after crosslinked 4h, cross-linking products is crushed to 150 μm ~ 250 μm, then the cross-linking products particle after fragmentation is placed in pyrolyzer, and under vacuum atmosphere Pintsch process, cracking temperature is 1500 DEG C, heat-up rate is 5 DEG C/min, pyrolysis time 6h, product furnace cooling after cracking is to room temperature, ball milling 15h again, obtains the carbon matrix precursor particle that particle size range is 0.1 μm ~ 20 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method to carry out chlorination etching to the carbon matrix precursor particle that above-mentioned steps (1) obtains, chlorination is etched in atmosphere tube type stove to be carried out, and etching temperature is 900 DEG C, and heat-up rate is 5 DEG C/min, etching time is 3h, and reaction atmosphere is Cl
2, in whole chlorination etching process, logical Ar is as carrier gas, cool to room temperature, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt H
2what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl, and post-processing temperature is 600 DEG C, treatment time 2h, until removed by Cl element, obtains not containing micro-meso-porous carbon material of Cl.
The micro-meso-porous carbon material obtained to above-mentioned the present embodiment adopts gas adsorption (BET) method to analyze its pore structure, and adsorption/desorption curve as shown in Figure 3.Known after testing, the specific surface area of micro-meso-porous carbon material of the present embodiment is 1539m
2/ g, mean pore size is 1.9nm, and pore capacities is 0.726cc/g, and wherein micropore hole content is 0.571cc/g, and mesoporous hole content is 0.076cc/g.
Embodiment 4:
Specific surface area of the present invention and the controlled micro-meso-porous carbon material preparation method of pore volume, comprise the following steps:
(1) preparation of carbon matrix precursor: polysiloxane precursor is heated to 250 DEG C and makes it that crosslinking reaction occur, after crosslinked 4h, cross-linking products is crushed to 150 μm ~ 250 μm, then the cross-linking products particle after fragmentation is placed in pyrolyzer, and under vacuum atmosphere Pintsch process, cracking temperature is 1700 DEG C, heat-up rate is 5 DEG C/min, pyrolysis time 6h, product furnace cooling after cracking is to room temperature, ball milling 15h again, obtains the carbon matrix precursor particle that particle size range is 0.1 μm ~ 20 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method to carry out chlorination etching to the carbon matrix precursor particle that above-mentioned steps (1) obtains, chlorination is etched in atmosphere tube type stove to be carried out, and etching temperature is 900 DEG C, and heat-up rate is 5 DEG C/min, etching time is 3h, and reaction atmosphere is Cl
2, logical N in whole chlorination etching process
2as carrier gas, cool to room temperature, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt NH
3what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl, and treatment temp is 600 DEG C, treatment time 2h, until removed by Cl element, obtains not containing micro-meso-porous carbon material of Cl.
The micro-meso-porous carbon material obtained to above-mentioned the present embodiment adopts gas adsorption (BET) method to analyze its pore structure, and adsorption/desorption curve as shown in Figure 4.Known after testing, the specific surface area of micro-meso-porous carbon material of the present embodiment is 1168m
2/ g, mean pore size is 1.9nm, and pore capacities is 0.726cc/g, and wherein micropore hole content is 0.571cc/g, and mesoporous hole content is 0.076cc/g.
Embodiment 5:
Specific surface area of the present invention and the controlled micro-meso-porous carbon material preparation method of pore volume, comprise the following steps:
(1) preparation of carbon matrix precursor: polysiloxane precursor is heated to 250 DEG C and makes it that crosslinking reaction occur, after crosslinked 4h, is crushed to 150 μm ~ 250 μm, then the cross-linking products particle after fragmentation is placed in pyrolyzer by cross-linking products, and at N
2atmosphere at high temperature cracking, cracking temperature is 1200 DEG C, and heat-up rate is 5 DEG C/min, pyrolysis time 2h, and the product furnace cooling after cracking is to room temperature, then ball milling 15h, obtains the carbon matrix precursor particle that particle size range is 0.1 μm ~ 50 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method to carry out chlorination etching to the carbon matrix precursor particle that above-mentioned steps (1) obtains, chlorination is etched in atmosphere tube type stove to be carried out, and etching temperature is 1200 DEG C, and heat-up rate is 15 DEG C/min, etching time is 3h, and reaction atmosphere is Cl
2, in whole chlorination etching process, logical Ar is as carrier gas, cool to room temperature, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt H
2what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl, and treatment temp is 600 DEG C, treatment time 2h, until removed by Cl element, obtains not containing micro-meso-porous carbon material of Cl.
The micro-meso-porous carbon material obtained to above-mentioned the present embodiment adopts gas adsorption (BET) method to analyze its pore structure, and adsorption/desorption curve as shown in Figure 5.Known after testing, the specific surface area of micro-meso-porous carbon material of the present embodiment is 2869m
2/ g, mean pore size is 3.2nm, and pore capacities is 1.869cc/g, and wherein micropore hole content is 1.045cc/g, and mesoporous hole content is 0.824cc/g.
Claims (7)
1. specific surface area and the controlled micro-meso-porous carbon material preparation method of pore volume, comprises the following steps:
(1) preparation of carbon matrix precursor: make it that crosslinking reaction occur after polysiloxane precursor being heated, cross-linking products is carried out fragmentation, then the cross-linking products particle after fragmentation is placed in Pintsch process under inert atmosphere or vacuum atmosphere, product cool to room temperature after cracking, obtains the carbon matrix precursor that particle size range is 0.1 μm ~ 50 μm after ball milling;
(2) chlorination etching: utilize carbide-derived carbon method to carry out chlorination etching to the carbon matrix precursor that above-mentioned steps (1) obtains, obtains containing the micro-meso-porous carbon material of Cl;
(3) aftertreatment: adopt NH
3or H
2what obtain above-mentioned steps (2) carries out aftertreatment containing the micro-meso-porous carbon material of Cl, until removed by Cl element, obtains not containing micro-meso-porous carbon material of Cl;
In described step (1), described polysiloxane precursor is the silicone resin containing Si-OH group; In described step (1), inert atmosphere is nitrogen atmosphere or Ar atmosphere, and under described inert atmosphere, the cracking temperature of Pintsch process controls at 1600 DEG C ~ 1700 DEG C; Under described vacuum atmosphere, the cracking temperature of Pintsch process controls at 1400 DEG C ~ 2000 DEG C; Heat-up rate during Pintsch process is 5 DEG C/min ~ 20 DEG C/min.
2. micro-meso-porous carbon material preparation method according to claim 1, is characterized in that: in described step (1), and the temperature of described crosslinking reaction is 150 DEG C ~ 300 DEG C, and the time of crosslinking reaction is 2h ~ 6h.
3. micro-meso-porous carbon material preparation method according to claim 1 and 2, is characterized in that: in described step (1), the particle size distribution range of the cross-linking products particle after fragmentation controls at 150 μm ~ 250 μm.
4. micro-meso-porous carbon material preparation method according to claim 3, is characterized in that: the time controling of described Pintsch process is 1h ~ 6h, and the time controling of described ball milling is 5h ~ 40h.
5. the micro-meso-porous carbon material preparation method according to claim 1,2 or 4, is characterized in that: in described step (2), and the etching temperature of chlorination etching is 750 DEG C ~ 1200 DEG C, heat-up rate is 5 DEG C/and min ~ 20 DEG C/min, reaction atmosphere is Cl
2, logical N in whole chlorination etching process
2or Ar is as carrier gas.
6. micro-meso-porous carbon material preparation method according to claim 5, is characterized in that: the time of described chlorination etching is 1h ~ 5h.
7. the micro-meso-porous carbon material preparation method according to claim 1,2 or 4, is characterized in that: in described step (3), and the treatment temp of aftertreatment is 400 DEG C ~ 800 DEG C; The treatment time of described aftertreatment is 0.5h ~ 4h.
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| CN104058387B (en) * | 2014-07-11 | 2016-06-22 | 武汉工程大学 | A kind of preparation method of hollow meso-porous carbon material |
| CN104529401B (en) * | 2015-01-14 | 2017-08-15 | 景德镇陶瓷大学 | A kind of preparation method of the micro/meso porous silicon-oxygen-carbon ceramic material of high-specific surface area |
| CN111389357B (en) * | 2020-03-24 | 2021-03-23 | 中国科学院化学研究所 | Mesoporous multilevel structure carbon microsphere and preparation method thereof |
| CN111850600A (en) * | 2020-07-17 | 2020-10-30 | 西安怡速安智能科技有限公司 | Formula of anode coating for removing peculiar smell of electrochemical electrode |
| DE102021107429A1 (en) * | 2021-03-24 | 2022-09-29 | Skeleton Technologies GmbH | Method of making microporous carbon material |
| CN113546584A (en) * | 2021-07-14 | 2021-10-26 | 中天超容科技有限公司 | Mesoporous carbon pressurized fluidization production system and production method |
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