CN112250063A - Method for promoting graphitization of wood biochar at low temperature - Google Patents
Method for promoting graphitization of wood biochar at low temperature Download PDFInfo
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- CN112250063A CN112250063A CN202011094425.5A CN202011094425A CN112250063A CN 112250063 A CN112250063 A CN 112250063A CN 202011094425 A CN202011094425 A CN 202011094425A CN 112250063 A CN112250063 A CN 112250063A
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- 239000002023 wood Substances 0.000 title claims abstract description 136
- 238000005087 graphitization Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 42
- 230000001737 promoting effect Effects 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000005245 sintering Methods 0.000 claims abstract description 48
- 238000007598 dipping method Methods 0.000 claims abstract description 44
- 239000008367 deionised water Substances 0.000 claims abstract description 41
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 41
- 238000001035 drying Methods 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 29
- 239000002184 metal Substances 0.000 claims abstract description 29
- 150000003839 salts Chemical class 0.000 claims abstract description 27
- 239000012266 salt solution Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 230000007935 neutral effect Effects 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000007873 sieving Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 8
- 238000005470 impregnation Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 238000007781 pre-processing Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 5
- 235000009566 rice Nutrition 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical group Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 239000010902 straw Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000007246 mechanism Effects 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 229910052723 transition metal Inorganic materials 0.000 abstract description 2
- 150000003624 transition metals Chemical class 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000003575 carbonaceous material Substances 0.000 description 8
- 241000209094 Oryza Species 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000010903 husk Substances 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- 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
- C01B32/20—Graphite
- C01B32/205—Preparation
Abstract
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which comprises the following steps: firstly, preparing wood biochar and carrying out pretreatment, and dipping wood biochar powder into a salt solution, wherein the dipping salt solution is formed by mixing metal salt and deionized water; putting the wood-containing biochar composite material into a vacuum box for dipping, filtering, drying, and repeating for 1-3 times to obtain the dipped wood-containing biochar composite material; and finally, sintering the mixture in a vacuum sintering furnace to obtain the wood biochar with high graphitization degree. The method comprises the steps of tightly coating metal salt on the surface of the biochar by using an impregnation-drying method, and then reducing transition metal through carbothermic reduction, wherein the graphitization degree of the wooden biochar is improved by the metal at a low temperature through a catalytic mechanism. Compared with other graphitization promoting processes, the process can reach a certain graphitization degree without high temperature, the cost is reduced, the preparation process is simple, and no pollutant is generated.
Description
Technical Field
The invention belongs to the technical field of biochar graphitization, and particularly relates to a method for promoting graphitization of wooden biochar at a low temperature.
Background
Carbon materials have been used in a variety of materials due to their advantages of excellent electrical conductivity, low density, corrosion resistance, and the like. The performance of the carbon material has a great relationship with the graphitization degree, for example, carbon nanotubes, graphene and the like are common carbon materials with good graphitization at present, however, the preparation cost of the common carbon materials is high, and pollutants are generated in the preparation process, which limits the wide application of the materials. However, biochar has been regarded as a novel carbon material in recent years. The biological carbon has wide sources, is a renewable resource, has great future prospect, is simple in preparation process and free of harmful substances, can retain the unique structure of the biological carbon after the biological material is carbonized, and has great potential in the fields of batteries, adsorption materials, capacitors and the like. However, as an amorphous carbon, the graphitization of the biochar is difficult to meet the application requirement at a low temperature, and the carbonization temperature of the biochar is generally above 2500 ℃, so that the biochar with a good graphitization degree can be obtained, but the cost is greatly required. Therefore, in order to save the cost, a method for improving the graphitization degree of the biochar is explored at low temperature, and the method has great value for the application of the biochar in the future.
Disclosure of Invention
The invention aims to provide a method for promoting the graphitization of the wood biochar at low temperature, which improves the graphitization degree of the wood biochar under the low-temperature condition.
The technical scheme adopted by the invention is that the method for promoting the graphitization of the wooden biochar at low temperature is implemented according to the following steps:
step 1, preparing wood biochar;
step 2, preprocessing the wood biochar obtained in the step 1;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
step 4, dipping the wood biochar powder obtained in the step 2 into the salt solution obtained in the step 3, putting the wood biochar powder into a vacuum box for dipping, filtering out solid substances, drying, and repeating dipping, filtering and drying for 1-3 times to obtain a dipped wood biochar composite material;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The present invention is also characterized in that,
in the step 1, the method specifically comprises the following steps: and (3) putting the wood material into a vacuum sintering furnace for sintering, heating to 600-1000 ℃ at the speed of 10 ℃/min, preserving heat for 1.5-2 h, and cooling to room temperature along with the furnace to obtain the wood biochar.
The wood material is natural air-dried fir, straw or rice hull.
In the step 2, the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-50 mesh sieve is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
and 2.4, adding the wood biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min at 55 ℃ while continuously stirring, and washing the wood biochar powder to be neutral by using deionized water.
In step 3, the metal salt is NiCl2·6H2O、FeCl3·6H2O、CoCl2·6H2Any one of O; the concentration of the metal salt is 0.15-0.25 mol/L.
In the step 4, the dipping time is 12-24 hours, the drying temperature is 80 ℃, and the drying time is 8 hours.
In step 5, the sintering conditions are as follows: heating to 600-1000 ℃ at the speed of 10 ℃/min, and keeping the temperature for 1-2 h to cool to room temperature along with the furnace.
The method has the beneficial effects that the metal salt is tightly coated on the surface of the biochar by using an impregnation-drying method, and then the transition metal is reduced by carbothermic reduction, so that the graphitization degree of the wooden biochar is improved by a catalytic mechanism under the condition of low temperature by the metal. Compared with other graphitization promoting processes, the process can reach a certain graphitization degree without high temperature, the cost is reduced, the preparation process is simple, and no pollutant is generated.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which is implemented according to the following steps:
step 1, preparing wood biochar; the method specifically comprises the following steps:
putting the wood material into a vacuum sintering furnace for sintering, heating to 600-1000 ℃ at the speed of 10 ℃/min, preserving heat for 1.5-2 h, and cooling to room temperature along with the furnace to obtain the wood biochar;
the wood material is natural air-dried fir, straw or rice hull;
step 2, preprocessing the wood biochar obtained in the step 1; the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-50 mesh sieve is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
step 2.4, adding the wooden biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min under the heating temperature of 55 ℃ and continuously stirring, and then washing the wooden biochar powder to be neutral by using deionized water;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
the metal salt being NiCl2·6H2O、FeCl3·6H2O、CoCl2·6H2Any one of O;
the concentration of the metal salt is 0.15-0.25 mol/L;
step 4, soaking the wood biochar powder obtained in the step 2 in the soaking solution in the step 3, placing the wood biochar powder into a vacuum box for soaking, then filtering out solid substances, drying, and repeatedly soaking, filtering and drying for 1-3 times to obtain a soaked wood biochar composite material;
the dipping time is 12-24 h, the vacuum degree in a vacuum box is less than or equal to 10pa, the drying temperature is 80 ℃, and the drying time is 8 h;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The sintering conditions are as follows: heating to 600-1000 ℃ at the speed of 10 ℃/min, keeping the temperature for 1-2 h, and cooling to room temperature along with the furnace; the vacuum degree of the vacuum sintering furnace is less than or equal to 10 pa.
Example 1
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which is implemented according to the following steps:
step 1, preparing wood biochar; the method specifically comprises the following steps:
putting the wood material into a vacuum sintering furnace for sintering, heating to 600 ℃ at the speed of 10 ℃/min, preserving heat for 1.5h, and cooling to room temperature along with the furnace to obtain the wood biochar;
the wood material is natural air-dried fir;
step 2, preprocessing the wood biochar obtained in the step 1; the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-mesh screen is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
step 2.4, adding the wooden biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min under the heating temperature of 55 ℃ and continuously stirring, and then washing the wooden biochar powder to be neutral by using deionized water;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
the metal salt is CoCl2·6H2O; the concentration of the metal salt is 0.15 mol/L;
step 4, dipping the wood biochar powder obtained in the step 2 into the dipping solution in the step 3, putting the wood biochar powder into a vacuum box for dipping, filtering and drying, and repeating dipping, filtering and drying for 3 times to obtain a dipped wood biochar composite material;
the dipping time is 12h, the vacuum degree in the vacuum box is less than or equal to 20pa, the drying temperature is 80 ℃, and the drying time is 8 h;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The sintering conditions are as follows: heating to 600 ℃ at the speed of 10 ℃/min, keeping the temperature for 2h, and cooling to room temperature along with the furnace; the vacuum degree of the vacuum sintering furnace is less than or equal to 10 pa.
Example 2
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which is implemented according to the following steps:
step 1, preparing wood biochar; the method specifically comprises the following steps:
putting the wood material into a vacuum sintering furnace for sintering, heating to 700 ℃ at the speed of 10 ℃/min, preserving heat for 1.5h, and cooling to room temperature along with the furnace to obtain the wood biochar;
the wood material is natural air-dried fir;
step 2, preprocessing the wood biochar obtained in the step 1; the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-mesh screen is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
step 2.4, adding the wooden biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min under the heating temperature of 55 ℃ and continuously stirring, and then washing the wooden biochar powder to be neutral by using deionized water;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
the metal salt is CoCl2·6H2Any one of O;
the concentration of the metal salt is 0.20 mol/L;
step 4, dipping the wood biochar powder obtained in the step 2 into the dipping solution in the step 3, putting the dipped solution into a vacuum box for dipping, then filtering and drying the dipped solution, and repeating dipping, filtering and drying for 3 times to obtain the dipped wood biochar composite material;
the dipping time is 14h, the vacuum degree in the vacuum box is less than or equal to 10pa, the drying temperature is 80 ℃, and the drying time is 8 h;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The sintering conditions are as follows: heating to 800 ℃ at the speed of 10 ℃/min, keeping the temperature for 2h, and cooling to room temperature along with the furnace; the vacuum degree of the vacuum sintering furnace is less than or equal to 10 pa.
Example 3
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which is implemented according to the following steps:
step 1, preparing wood biochar; the method specifically comprises the following steps:
putting the wood material into a vacuum sintering furnace for sintering, heating to 800 ℃ at the speed of 10 ℃/min, preserving heat for 2h, and cooling to room temperature along with the furnace to obtain the wood biochar;
the wood material is naturally air-dried rice husk;
step 2, preprocessing the wood biochar obtained in the step 1; the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-mesh screen is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
step 2.4, adding the wooden biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min under the heating temperature of 55 ℃ and continuously stirring, and then washing the wooden biochar powder to be neutral by using deionized water;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
the metal salt is CoCl2·6H2O；
The concentration of the metal salt is 0.25 mol/L;
step 4, dipping the wood biochar powder obtained in the step 2 into the dipping solution in the step 3, putting the dipped solution into a vacuum box for dipping, then filtering and drying the dipped solution, and repeating dipping, filtering and drying for 3 times to obtain the dipped wood biochar composite material;
the dipping time is 18h, the vacuum degree in the vacuum box is less than or equal to 10pa, the drying temperature is 80 ℃, and the drying time is 8 h;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The sintering conditions are as follows: heating to 800 ℃ at the speed of 10 ℃/min, keeping the temperature for 1h, and cooling to room temperature along with the furnace; the vacuum degree of the vacuum sintering furnace is less than or equal to 10 pa.
Example 4
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which is implemented according to the following steps:
step 1, preparing wood biochar; the method specifically comprises the following steps:
putting the wood material into a vacuum sintering furnace for sintering, heating to 1000 ℃ at the speed of 10 ℃/min, preserving heat for 1.5h, and cooling to room temperature along with the furnace to obtain the wood biochar;
the wood material is naturally air-dried rice husk;
step 2, preprocessing the wood biochar obtained in the step 1; the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 50-mesh sieve is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
step 2.4, adding the wooden biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min under the heating temperature of 55 ℃ and continuously stirring, and then washing the wooden biochar powder to be neutral by using deionized water;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
the metal salt being NiCl2·6H2O；
The concentration of the metal salt is 0.20 mol/L;
step 4, dipping the wood biochar powder obtained in the step 2 into the dipping solution in the step 3, putting the dipped solution into a vacuum box for dipping, then filtering and drying the dipped solution, and repeating dipping, filtering and drying for 2 times to obtain the dipped wood biochar composite material;
the dipping time is 24h, the vacuum degree in the vacuum box is less than or equal to 10pa, the drying temperature is 80 ℃, and the drying time is 8 h;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The sintering conditions are as follows: heating to 1000 ℃ at the speed of 10 ℃/min, keeping the temperature for 2h, and cooling to room temperature along with the furnace; the vacuum degree of the vacuum sintering furnace is less than or equal to 10 pa.
Example 5
The invention discloses a method for promoting graphitization of wooden biochar at low temperature, which is implemented according to the following steps:
step 1, preparing wood biochar; the method specifically comprises the following steps:
putting the wood material into a vacuum sintering furnace for sintering, heating to 1000 ℃ at the speed of 10 ℃/min, preserving heat for 1.5h, and cooling to room temperature along with the furnace to obtain the wood biochar;
the wood material is naturally air-dried straw;
step 2, preprocessing the wood biochar obtained in the step 1; the method specifically comprises the following steps:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-mesh screen is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
step 2.4, adding the wooden biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min under the heating temperature of 55 ℃ and continuously stirring, and then washing the wooden biochar powder to be neutral by using deionized water;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
the metal salt being FeCl3·6H2O；
The concentration of the metal salt is 0.20 mol/L;
step 4, dipping the wood biochar powder obtained in the step 2 into the dipping solution in the step 3, putting the dipped solution into a vacuum box for dipping, then filtering and drying the dipped solution, and repeating dipping, filtering and drying for 1 time to obtain the dipped wood biochar composite material;
the dipping time is 12h, the vacuum degree in the vacuum box is less than or equal to 10pa, the drying temperature is 80 ℃, and the drying time is 8 h;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
The sintering conditions are as follows: heating to 1000 ℃ at the speed of 10 ℃/min, keeping the temperature for 2h, and cooling to room temperature along with the furnace; the vacuum degree of the vacuum sintering furnace is less than or equal to 10 pa.
TABLE 1 conductivity of the samples prepared
| Untreated biochar | Fe catalyzed biochar | Co-catalyzed biochar | |
| Conductivity (S/m) | 0.441895572 | 1.749498507 | 1.679788358 |
The conductivity of the carbon material is closely related to the graphitization degree of the carbon material, and the carbon material with higher graphitization degree has more free electrons to move inside the material, thereby showing good conductivity. The conductivity of the prepared sample is tested, as shown in table 1, it can be seen that the conductivity of the untreated biochar is 0.441895572S/m, while the conductivities of the biochar catalyzed by Fe and Co according to the method of the present invention reach 1.749498507S/m and 1.679788358S/m, respectively, and are increased by nearly 5 times compared with the previous conductivities, which indicates that the graphitization degree of the biochar is obviously increased.
Claims (7)
1. A method for promoting graphitization of wooden biochar at low temperature is characterized by comprising the following steps:
step 1, preparing wood biochar;
step 2, preprocessing the wood biochar obtained in the step 1;
step 3, preparing a dipping salt solution; the impregnation salt solution is formed by mixing metal salt and deionized water;
step 4, dipping the wood biochar powder obtained in the step 2 into the salt solution obtained in the step 3, putting the wood biochar powder into a vacuum box for dipping, filtering out solid substances, drying, and repeating dipping, filtering and drying for 1-3 times to obtain a dipped wood biochar composite material;
and 5, putting the impregnated wood biochar composite material into a vacuum sintering furnace for sintering to obtain the wood biochar with high graphitization degree.
2. The method for promoting graphitization of wooden biochar by low temperature according to claim 1, wherein in the step 1, the steps are as follows: and (3) putting the wood material into a vacuum sintering furnace for sintering, heating to 600-1000 ℃ at the speed of 10 ℃/min, preserving heat for 1.5-2 h, and cooling to room temperature along with the furnace to obtain the wood biochar.
3. The method for promoting graphitization of wooden biochar at low temperature according to claim 2, wherein the wooden material is naturally air-dried fir, straw or rice hull.
4. The method for promoting graphitization of wooden biochar by low temperature according to claim 1, wherein in the step 2, the steps are as follows:
step 2.1, crushing and sieving the wood biochar to obtain wood biochar powder;
when sieving, a 40-50 mesh sieve is adopted;
step 2.2, carrying out ultrasonic cleaning on the wood biological carbon powder for 5min by using cleaning fluid; then washing the wood biological carbon powder to be neutral by using deionized water;
the volume ratio of the cleaning liquid is 1: 1C2H5OH and deionized water are mixed;
step 2.3, soaking the wood biochar powder in NaOH solution with the mass concentration of 2.0g/L, continuously stirring for 10min, and then washing the wood biochar powder to be neutral by using deionized water;
and 2.4, adding the wood biochar powder into a nitric acid solution with the volume fraction of 20%, heating in a constant-temperature water bath for 20min at 55 ℃ while continuously stirring, and washing the wood biochar powder to be neutral by using deionized water.
5. The method for promoting graphitization of wooden biochar at low temperature according to claim 1, wherein in the step 3, the metal salt is NiCl2·6H2O、FeCl3·6H2O、CoCl2·6H2Any one of O; the concentration of the metal salt is 0.15-0.25 mol/L.
6. The method for promoting graphitization of wooden biochar at low temperature according to claim 1, wherein in the step 4, the soaking time is 12-24 hours, the drying temperature is 80 ℃, and the drying time is 8 hours.
7. The method for promoting graphitization of wooden biochar by low temperature according to claim 1, wherein in the step 5, sintering conditions are as follows: heating to 600-1000 ℃ at the speed of 10 ℃/min, and keeping the temperature for 1-2 h to cool to room temperature along with the furnace.
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