CN106564871A - Whisker-shaped thin film biochar material and preparation method thereof - Google Patents
Whisker-shaped thin film biochar material and preparation method thereof Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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Abstract
The invention discloses a whisker-shaped thin film biochar material and a preparation method thereof. The method comprises the steps that calcium carbonate whiskers are utilized as a template agent, and a polydopamine thin film is loaded, so that a CaCO3@PDA composite is formed; an intermediate product, namely CaO@W-HFGB, is formed through high-temperature carbonization; the intermediate product, namely CaO@W-HFGB, is immersed in water, so that Ca(OH)2@W-HFGB is formed; and secondary carbonization for pore expanding is conducted, so that the whisker-shaped thin film biochar material is obtained. According to the whisker-shaped thin film biochar material and the preparation method thereof, the green and environment-friendly template agent, namely the calcium carbonate whiskers, is utilized efficiently; meanwhile, W-HFGB serving as a pore expanding agent is subjected to double pore expanding physically and chemically; and a new pore expanding agent is prevented from being introduced; in addition, the whisker-shaped thin film biochar material and the preparation method thereof have the beneficial effects of being low in preparation cost, green and environment-friendly in process, novel in product structure and the like; and extremely high application potential is achieved with respect to industrialization.
Description
Technical field
The invention belongs to material chemistry technical field, and in particular to a kind of crystal whisker-shaped thin film bio material with carbon element and its preparation side
Method.
Background technology
In recent years extensive application of the porous carbon materials of special appearance in the fields such as absorption, separation and catalysis, causes
The increasing attention of people.Wherein preparing the common method of porous carbon materials has hard template method, soft template method, activation method.
Activation method is performed etching in high temperature environments for activator to carbon matrix precursor, produces a large amount of nanoscale cracks or less mesoporous.Often
The activating reagent seen has KOH, NaOH, ZnCl2、H3PO4Deng.
Dopamine (dopamine, 3,4- dihydroxy propyl benzene amine), is the important composition composition of marine mussel secretions, is had
The features such as nontoxic, good biocompatibility, strongly adherent, there is oxidation self-polymeric reaction easily under wet condition, in surface of solids shape
Into poly-dopamine (PDA, polydopamine) thin film.Poly-dopamine thin film can prepare the presoma of porous carbon materials, in height
It is carbonized under the conditions of temperature, forms the material with carbon element of dense non-porous, under the further etching carbonization of expanding agent, generates porous carbon materials.
In preparing the porous carbon materials of special appearance, generally there are template hardly possible and remove with high costs with expanding agent etc. asking
Topic.Calcium Carbonate is a kind of environmentally friendly inorganic raw material, with it is cheap, nontoxic, remove many advantages, such as.Can be with profit
With the calcium carbonate product of different-shape, it is applied in the preparation of the porous carbon materials of special appearance as template.
The disclosure of background above technology contents is only used for design and the technical scheme for aiding in understanding the present invention, and it is not necessarily
Belong to the prior art of present patent application, without tangible proof show the above present patent application the applying date
In the case of disclosed, above-mentioned background technology should not be taken to evaluate the novelty and creativeness of the application.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of crystal whisker-shaped thin film bio material with carbon element and preparation method thereof, to solve
Certainly existing template is difficult removes, the problems such as expanding agent is with high costs.The present invention enters to the template calcium carbonate crystal whisker of environmental protection
Efficient utilization is gone, while having carried out dual reaming from physics and chemically to W-HFGB as expanding agent, it is to avoid introduce new
Expanding agent；In addition advantage of the invention is that：The various features such as preparation cost is low, process environmental protection, product structure novelty,
There is great application potential in industrialization.
In order to solve above technical problem, the present invention is employed the following technical solutions：
For this purpose, the present invention proposes a kind of crystal whisker-shaped thin film bio material with carbon element, and it is to utilize calcium carbonate crystal whisker to be template, load
Poly-dopamine thin film, forms CaCO3@PDA composites, Jing high temperature cabonizations generate intermediate product CaO@W-HFGB, are soaked in water
Form Ca (OH)2Bis- carbonization reamings of@W-HFGB, Jing, are obtained crystal whisker-shaped thin film bio material with carbon element.
The present invention also provides a kind of preparation method of crystal whisker-shaped thin film bio material with carbon element, comprises the following steps：
(1) synthesis of calcium carbonate crystal whisker
It is that raw material and tap water occur digestion reaction at 80 DEG C with calcium oxide, matches somebody with somebody after ageing, filtration, removal step
Ca (OH) processed2Suspension, in adding the circulation feed liquid kettle into supergravity reactor；Control Ca (OH)2Suspension total amount of feeding,
In CO2Gas flow is 50Lh-1, fluid flow is 530Lh-1, chemical additives addition is 7gL-1, carburizing temperature
For 60～85 DEG C, revolving bed rotating speed is 1000～1600rmin-1Preparation process condition under, Ca (OH)2Suspension and CO2Gas
Body contacts generation carburizing reagent in RPB and generates calcium carbonate crystal whisker；Reaction rear slurry is carried out sucking filtration, uses deionization
Water cyclic washing, 80 DEG C of vacuum drying 5h, is obtained calcium carbonate crystal whisker product；
(2)Ca(OH)2The preparation of@W-HFGB composites
Respectively compound concentration is 4～7gL-1Dopamine saline solution 100mL, concentration is 8gL-1Calcium carbonate crystal whisker water
Solution 50ml, and the alkaline solution prepared by 0.75mL ammonia, 40mL ethanol, 90mL deionized waters, three kinds of different solutions point
Mi Feng not stir；The calcium carbonate aqueous solution for having configured is added into DOPA amine salt aqueous solution, in bath temperature 15～25
DEG C, 150～300rmin of speed of agitator-1Under conditions of, react 0.5h；The alkaline solution for preparing is added to into above-mentioned DOPA
In amine salt mixed solution, reaction temperature keeps constant with rotating speed, reacts 20h；Reaction rear slurry is carried out into sucking filtration, deionized water
Washing, 80 DEG C of vacuum drying 5h, is obtained CaCO3@PDA composites；Weigh CaCO3@PDA samples are placed in tube furnace, in nitrogen
Protection under, carry out high temperature cabonization, obtain CaO@W-HFGB；CaO@W-HFGB, plus deionized water immersion are put in magnetic boat, it is quiet
Put, generate Ca (OH)2@W-HFGB, are vacuum dried at 70 DEG C to it, obtain Ca (OH)2@W-HFGB composite powders；
(3) preparation of crystal whisker-shaped thin film bio material with carbon element
Weigh Ca (OH)2@W-HFGB samples are placed in tube furnace, under the protection of nitrogen, carry out secondary high-temperature carbonization, its
Middle Ca (OH)2Reaming is performed etching to W-HFGB, deionized water is washed to neutrality after reaction, finally filter cake is put into into 80
DEG C vacuum drying oven in be dried 5h, obtain crystal whisker-shaped thin film bio material with carbon element.
Further, calcium oxide described in step (1) is technical grade.
Further, Ca (OH) described in step (1)2Concentration be 60～90gL-1。
Further, the Ca (OH) for controlling described in step (1)2Suspension total amount of feeding is 2.8L.
Further, chemical additives described in step (1) are phosphoric acid.
Further, DOPA amine salt is with the part by weight of calcium carbonate crystal whisker described in step (2)：1.00～1.75:
1.00。
Further, the ratio of CaO@W-HFGB and deionized water is described in step (2)：0.2～0.8g:10mL.
Further, time of repose described in step (2) is 6h.
Further, step (2) is identical with high temperature cabonization program described in (3), comprises the following steps：
(a) temperature-rise period：With 5～15 DEG C of min-1Speed sample is risen to into 700～900 DEG C from room temperature；
(b) thermostatic process：Sample keeps 1～3h at 700～900 DEG C；
(c) temperature-fall period：Sample naturally cools to room temperature from 700～900 DEG C.
The present invention compared with prior art, has the advantages that：
(1) present invention resolves into calcium oxide and carbon dioxide using calcium carbonate crystal whisker as template after high temperature cabonization, uses water
Calcium oxide is can remove, is solved the problems, such as that later stage template is difficult and is removed；
(2) calcium carbonate crystal whisker used by the present invention, in first time carbonisation, it decomposes the CO of release2With efficient
Reaming effect；
(3) calcium carbonate crystal whisker pyrolytic of the invention, the Ca (OH) formed after soaking2, in secondary carbonisation
In can realize the efficient utilization to calcium carbonate crystal whisker as expanding agent.
Description of the drawings
Fig. 1 is the SEM and TEM figure of the calcium carbonate crystal whisker of the embodiment of the present invention one and W-HFGB；
Fig. 2 is the calcium carbonate crystal whisker of the embodiment of the present invention one, the XRD figure of CaO@W-HFGB and W-HFGB；
Fig. 3 is the calcium carbonate crystal whisker of the embodiment of the present invention one, CaCO3The TG figures of@PDA；
Fig. 4 is the N of the W-HFGB of the embodiment of the present invention one2Adsorption-desorption figure.
Specific embodiment
With reference to specific embodiment and compare accompanying drawing the present invention is described in further detail.It is emphasized that
What the description below was merely exemplary, rather than in order to limit the scope of the present invention and its application.
Embodiment 1
A kind of preparation method of crystal whisker-shaped thin film bio material with carbon element, comprises the following steps：
(1) synthesis of calcium carbonate crystal whisker
With technical grade calcium oxide (quick lime) as raw material and tap water, there is digestion reaction at 80 DEG C, through ageing, mistake
Concentration is configured to after the steps such as filter, remove impurity for 80gL-1Ca (OH)2Suspension, adds the circulation into supergravity reactor
In feed liquid kettle；The Ca (OH) of control2Suspension total amount of feeding is 2.8L, in CO2Gas flow is 50Lh-1, fluid flow is
530L·h-1, chemical additives phosphoric acid addition is 7gL-1, carburizing temperature is 70 DEG C, and revolving bed rotating speed is 1400rmin-1
Preparation process condition under, Ca (OH)2Suspension and CO2Gas contacts generation carburizing reagent in RPB and generates carbonic acid
Calcium pyroborate；
(2)Ca(OH)2The preparation of@W-HFGB composites
Compound concentration is 5gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, i.e. part by weight are 1.25DA/1.0CaCO3DOPA amine salt and calcium carbonate crystal whisker, and by 0.75mL ammonia, 40mL
Ethanol, the alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；By the Calcium Carbonate for having configured
Aqueous solution is added into DOPA amine salt aqueous solution, is 20 DEG C in bath temperature, and speed of agitator is 200rmin-1Under conditions of, instead
Answer 0.5h；The alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature keeps constant with rotating speed,
Reaction 20h, is obtained CaCO3@PDA composites；
(3) preparation of crystal whisker-shaped thin film bio material with carbon element
Weigh the CaCO of certain mass3@PDA samples are placed in tube furnace, under the protection of nitrogen, carry out high temperature cabonization,
Carbonization Conditions are：With 5 DEG C of min-1Speed by CaCO3@PDA samples rise to 700 DEG C from room temperature, constant temperature 1h, then natural cooling
To room temperature, CaO@W-HFGB are obtained.0.4g CaO@W-HFGB are put in magnetic boat, plus go 10mL ionized waters to soak, stand 6h,
Generate Ca (OH)2@W-HFGB, are vacuum dried at 70 DEG C to it, obtain Ca (OH)2@W-HFGB powder；Weigh certain mass
Ca (OH)2@W-HFGB samples are placed in tube furnace, under the protection of nitrogen, carry out secondary high-temperature carbonization, and carbodiimide procedure is not
Become, wherein Ca (OH)2Reaming is performed etching to W-HFGB, deionized water is washed to neutrality after reaction, finally obtains carbon
Material W-HFGB-1.
Embodiment 2
Become outside the pale of civilization except following, remaining is with embodiment 1.
Compound concentration is 6gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, i.e. part by weight are 1.50DA/1.0CaCO3DOPA amine salt and calcium carbonate crystal whisker, and by 0.75mL ammonia, 40mL
Ethanol, the alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；By the Calcium Carbonate for having configured
Aqueous solution is added into DOPA amine salt aqueous solution, in 25 DEG C of bath temperature, speed of agitator 250rmin-1Under conditions of, reaction
0.5h；The alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature keeps constant with rotating speed, instead
Answer 20h that intermediate product CaCO is obtained3@PDA；
Weigh the CaCO of certain mass3@PDA samples are placed in tube furnace, under the protection of nitrogen, carry out high temperature cabonization,
Carbonization Conditions are：With 10 DEG C of min-1Speed by CaCO3@PDA samples rise to 800 DEG C from room temperature, constant temperature 2h, then natural cooling
To room temperature；Obtain intermediate product CaO@W-HFGB；0.6g CaO@W-HFGB are put in magnetic boat, plus go 10mL ionized waters to soak,
6h is stood, Ca (OH) is generated2@W-HFGB, are vacuum dried at 70 DEG C to it, obtain Ca (OH)2@W-HFGB powder.Keep carbon
Change program is constant to carry out secondary carbonization, and deionized water is washed to neutrality after reaction, final to obtain material with carbon element W-HFGB-2.
Embodiment 3
Become outside the pale of civilization except following, remaining is with embodiment 1.
Compound concentration is 7gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, i.e. part by weight are 1.75DA/1.0CaCO3DOPA amine salt and calcium carbonate crystal whisker, and by 0.75mL ammonia, 40mL
Ethanol, the alkaline solution that 90mL deionized waters are prepared, three kinds of different solutions seal stir respectively；By the Calcium Carbonate for having configured
Aqueous solution is added into DOPA amine salt aqueous solution, in 15 DEG C of bath temperature, speed of agitator 300rmin-1Under conditions of, reaction
0.5h；The alkaline solution for preparing is added in above-mentioned dopamine mixed salt solution, reaction temperature keeps constant with rotating speed, instead
Answer 20h that intermediate product CaCO is obtained3@PDA；
Weigh the CaCO of certain mass3@PDA samples are placed in tube furnace, under the protection of nitrogen, carry out high temperature cabonization,
Carbonization Conditions are：With 15 DEG C of min-1Speed by CaCO3@PDA samples rise to 900 DEG C from room temperature, constant temperature 3h, then natural cooling
To room temperature；Obtain intermediate product CaO@W-HFGB；0.8g CaO@W-HFGB are put in magnetic boat, plus go 10mL ionized waters to soak,
6h is stood, Ca (OH) is generated2@W-HFGB, are vacuum dried at 70 DEG C to it, obtain Ca (OH)2@W-HFGB powder；Keep carbon
Change program is constant to carry out secondary carbonization, and deionized water is washed to neutrality after reaction, final to obtain material with carbon element W-HFGB-3.
Instance analysis
As shown in figure 1, W-HFGB porous carbon materials prepared by the present invention, the appearance structure with whisker film like shows
Template Calcium Carbonate has resolved into completely calcium oxide and has been washed with water removal, and pattern caves in after wash water.Wherein SEM charts are bright
The minor axis of t calcium carbonate crystal whiskers is 140～180nm, and draw ratio is 17～20.
As shown in Fig. 2 it is aragonitic that the present invention prepares calcium carbonate crystal whisker, and the XRD spectrum of intermediate product CaO@W-HFGB
Without the characteristic peak of Calcium Carbonate aragonitic, show CaCO3Calcium Carbonate in@PDA has resolved into completely calcium oxide.Wherein W-HFGB
XRD figure, there is graphitization characteristic peak on 26 ° and 44 °, (002) and (100) crystal face shows that W-HFGB has part graphite
Change structure.
As shown in figure 3, the calcium carbonate crystal whisker and CaCO of present invention preparation3@PDA decomposition temperatures, respectively 586 DEG C and 673
DEG C, wherein CaCO3@PDA weight-loss ratios under conditions of greenhouse rises to 900 DEG C are about 57%.
As shown in figure 4, the N of the W-HFGB of present invention preparation2Adsorption/desorption figure, and its thus obtain the pore structure of material
As shown in table 1.Understand that W-HFGB has high-specific surface area and big micro-diplopore structure, BET and Langmuir specific surface areas are respectively
707.4m2·g-1, 843.9m2·g-1, wherein micropore ratio is 38.38%.
The pore structure parameter of the W-HFGB of table 1
It would be recognized by those skilled in the art that it is possible that numerous accommodations are made to above description, so embodiment and attached
Figure is intended merely to describe one or more particular implementations.
Although having been described above and describing the example embodiment for being counted as the present invention, it will be apparent to those skilled in the art that
It can be variously modified and be replaced, without departing from the spirit of the present invention.Furthermore it is possible to make many modifications with by spy
Condition of pledging love is fitted to the religious doctrine of the present invention, without departing from invention described herein central concept.So, the present invention is unrestricted
May also include belonging to all embodiments and its equivalent of the scope of the invention in specific embodiment disclosed here, but the present invention
Thing.
Claims (10)
1. a kind of crystal whisker-shaped thin film bio material with carbon element, it is characterised in that using calcium carbonate crystal whisker be template, loads poly-dopamine
Thin film, forms CaCO3@PDA composites, Jing high temperature cabonizations generate intermediate product CaO@W-HFGB, are soaked in water to form Ca
(OH)2Bis- carbonization reamings of@W-HFGB, Jing, are obtained crystal whisker-shaped thin film bio material with carbon element.
2. a kind of preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 1, it is characterised in that include with
Lower step：
(1) synthesis of calcium carbonate crystal whisker
It is that raw material and tap water occur digestion reaction at 80 DEG C with calcium oxide, after ageing, filtration, removal step Ca is prepared
(OH)2Suspension, in adding the circulation feed liquid kettle into supergravity reactor；Control Ca (OH)2Suspension total amount of feeding, in CO2
Gas flow is 50Lh-1, fluid flow is 530Lh-1, chemical additives addition is 7gL-1, carburizing temperature be 60～
85 DEG C, revolving bed rotating speed is 1000～1600rmin-1Preparation process condition under, Ca (OH)2Suspension and CO2Gas is in rotation
Turn contact in packed bed and carburizing reagent generation calcium carbonate crystal whisker occurs；Reaction rear slurry is carried out into sucking filtration, deionized water repeatedly
Washing, 80 DEG C of vacuum drying 5h, is obtained calcium carbonate crystal whisker product；
(2)Ca(OH)2The preparation of@W-HFGB composites
Respectively compound concentration is 4～7gL-1Dopamine saline solution 100mL, concentration is 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, and the alkaline solution prepared by 0.75mL ammonia, 40mL ethanol, 90mL deionized waters, three kinds of different solutions difference are close
Envelope stirs；The calcium carbonate aqueous solution for having configured is added into DOPA amine salt aqueous solution, in 15～25 DEG C of bath temperature, is stirred
150～300rmin of mix rotating speed-1Under conditions of, react 0.5h；The alkaline solution for preparing is added to into above-mentioned DOPA amine salt to mix
In closing solution, reaction temperature keeps constant with rotating speed, reacts 20h；Reaction rear slurry is carried out sucking filtration, is washed with deionized,
80 DEG C of vacuum drying 5h, are obtained CaCO3@PDA composites；Weigh CaCO3@PDA samples are placed in tube furnace, in the guarantor of nitrogen
Under shield, high temperature cabonization is carried out, obtain CaO@W-HFGB；CaO@W-HFGB, plus deionized water immersion are put in magnetic boat, are stood,
Generate Ca (OH)2@W-HFGB, are vacuum dried at 70 DEG C to it, obtain Ca (OH)2@W-HFGB composite powders；
(3) preparation of crystal whisker-shaped thin film bio material with carbon element
Weigh Ca (OH)2@W-HFGB samples are placed in tube furnace, under the protection of nitrogen, carry out secondary high-temperature carbonization, wherein Ca
(OH)2Reaming is performed etching to W-HFGB, deionized water is washed to neutrality after reaction, finally filter cake is put into into 80 DEG C
5h is dried in vacuum drying oven, crystal whisker-shaped thin film bio material with carbon element is obtained.
3. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that in step (1)
The calcium oxide is technical grade.
4. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that in step (1)
The Ca (OH)2Concentration be 60～90gL-1。
5. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that in step (1)
The Ca (OH) of the control2Suspension total amount of feeding is 2.8L.
6. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that in step (1)
The chemical additives are phosphoric acid.
7. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that：In step (2)
The DOPA amine salt is with the part by weight of calcium carbonate crystal whisker：1.00～1.75:1.00.
8. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that：In step (2)
The ratio of the CaO@W-HFGB and deionized water is：0.2～0.8g:10mL.
9. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 2, it is characterised in that：In step (2)
The time of repose is 6h.
10. the preparation method of crystal whisker-shaped thin film bio material with carbon element according to claim 1, it is characterised in that：Step (2) and
(3) high temperature cabonization program described in is identical, comprises the following steps：
(a) temperature-rise period：With 5～15 DEG C of min-1Speed sample is risen to into 700～900 DEG C from room temperature；
(b) thermostatic process：Sample keeps 1～3h at 700～900 DEG C；
(c) temperature-fall period：Sample naturally cools to room temperature from 700～900 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053938A (en) * | 2018-09-21 | 2018-12-21 | 黑龙江大学 | A kind of charcoal/composite membrane of polymer preparation method applied to solar energy evaporation water |
| CN111968862A (en) * | 2020-08-07 | 2020-11-20 | 苏州科技大学 | Method for synthesizing MnO-Co/biochar electrode material |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005022970A (en) * | 1995-02-23 | 2005-01-27 | Okura Ind Co Ltd | Manufacturing method of silicon nitride whisker |
| CN103072970A (en) * | 2013-02-04 | 2013-05-01 | 河北科技大学 | Spherical hollow mesoporous carbon shell and preparing method thereof |
| JP2014047087A (en) * | 2012-08-30 | 2014-03-17 | Aomori Prefectural Industrial Technology Research Center | Method of producing chemical-carrying active carbon, chemical-carrying active carbon and filter using the carbon |
| CN104085877A (en) * | 2014-06-30 | 2014-10-08 | 湖北工程学院 | Porous carbon electrode material based on chitosan and derivative of chitosan thereof as well as preparation method and application of porous carbon electrode material |
| CN104310368A (en) * | 2014-08-11 | 2015-01-28 | 常州大学 | Hollow carbon sphere preparing method |
| CN105502342A (en) * | 2016-01-07 | 2016-04-20 | 上海工程技术大学 | Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source |
| CN105621386A (en) * | 2014-10-30 | 2016-06-01 | 中国石油化工股份有限公司 | Method for preparing carbon material |
-
2016
- 2016-11-08 CN CN201610979838.9A patent/CN106564871B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005022970A (en) * | 1995-02-23 | 2005-01-27 | Okura Ind Co Ltd | Manufacturing method of silicon nitride whisker |
| JP2014047087A (en) * | 2012-08-30 | 2014-03-17 | Aomori Prefectural Industrial Technology Research Center | Method of producing chemical-carrying active carbon, chemical-carrying active carbon and filter using the carbon |
| CN103072970A (en) * | 2013-02-04 | 2013-05-01 | 河北科技大学 | Spherical hollow mesoporous carbon shell and preparing method thereof |
| CN104085877A (en) * | 2014-06-30 | 2014-10-08 | 湖北工程学院 | Porous carbon electrode material based on chitosan and derivative of chitosan thereof as well as preparation method and application of porous carbon electrode material |
| CN104310368A (en) * | 2014-08-11 | 2015-01-28 | 常州大学 | Hollow carbon sphere preparing method |
| CN105621386A (en) * | 2014-10-30 | 2016-06-01 | 中国石油化工股份有限公司 | Method for preparing carbon material |
| CN105502342A (en) * | 2016-01-07 | 2016-04-20 | 上海工程技术大学 | Method for preparing nanometer hollow carbon spheres with dopamine serving as carbon source |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109053938A (en) * | 2018-09-21 | 2018-12-21 | 黑龙江大学 | A kind of charcoal/composite membrane of polymer preparation method applied to solar energy evaporation water |
| CN111968862A (en) * | 2020-08-07 | 2020-11-20 | 苏州科技大学 | Method for synthesizing MnO-Co/biochar electrode material |
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