CN106744915A - A kind of cellulose base graphitized material and preparation method thereof - Google Patents
A kind of cellulose base graphitized material and preparation method thereof Download PDFInfo
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- CN106744915A CN106744915A CN201611169805.4A CN201611169805A CN106744915A CN 106744915 A CN106744915 A CN 106744915A CN 201611169805 A CN201611169805 A CN 201611169805A CN 106744915 A CN106744915 A CN 106744915A
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Abstract
The invention discloses a kind of biomass-based graphitized material and preparation method thereof, by biomass material charing process, product infusion process is obtained the biomass carbon of Ni loads afterwards.It is placed in again in high temperature resistant close crucible, graphitization reaction obtains final product after cooling with pickling.Degree of graphitization product higher is successfully obtained present invention employs Ni catalysis methods, has been substantially reduced than 2800 DEG C needed for ordinary graphite method with the graphite-structure more than 40 layers, and required temperature.Products therefrom electrical conductivity highest under 20MPa can exceed 60Scm‑1, conductive material, electromagnetic shielding material or Graphene can be further prepared, have a good application prospect.
Description
Technical field
The invention belongs to carbonaceous material applied technical field, a kind of preparation side of biomass-based graphitized material is related generally to
Method.
Technical field
Graphite has excellent thermal conductivity, all has in numerous areas such as electrode material, refractory material, steel-making etc.
It is widely used.But native graphite is nonrenewable resources, and synthetic graphite is needed convenient source such as petroleum coke, drip
Green grass or young crops etc. can just make its amorphous carbon structure be effectively converted into graphite-structure under excessive temperature (typically up to 2800 DEG C) treatment,
Therefore use reproducible biomass material --- cellulose be raw material prepare graphitized material with replace traditional petroleum coke with
The nonrenewable resourceses such as pitch have researching value very much.
But the product after the biomass material such as charing such as cellulose, lignin unlike petroleum coke, pitch etc.
The difficult graphited amorphous carbon of thing, even if being heated to 3000 DEG C is also still difficult to effective graphitization conversion
The content of the invention
It is an object of the invention to provide a kind of biomass-based graphitized material and preparation method thereof, with efficient, low energy
The characteristics of consumption.
The technical scheme is that：A kind of biomass-based graphitized material, biomass material is first carbonized, then by dipping
After method supported ni catalyst, under 1300~1600 DEG C of high-temperature closeds, under Ni catalyst actions, there is effective graphitization and turn
Change, obtain biomass-based graphitized material, the degree of graphitization of described biomass-based graphitized material reaches natural more than 50%
The crystallinity of graphite, with the graphite-structure more than 40 layers, electrical conductivity is more than 60Scm under 20MPa pressure-1。
Described biomass material includes any one in cellulose, lignin, coconut husk, wood chip, walnut shell, phoenix tree leaf
Or it is several.
The load capacity of Ni catalyst is 2~5mmol/g C.
A kind of method for preparing described biomass-based graphitized material, comprises the following steps：
The first step, the preparation of charcoal and the load of metallic catalyst：Biomass material is placed in close crucible and is carbonized
Treatment obtains charcoal, charcoal impregnated in and contain Ni2+The aqueous solution in overnight, be dried to obtain afterwards load Ni biology
Charcoal；
Second step, graphitization conversion：The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace anti-
Should, Ni2+Because the reduction of charcoal is changed into simple substance Ni, charcoal carries out graphitization conversion under the catalysis of simple substance Ni, finally uses
Acid elution obtains bio-based graphitized material after removing Ni.
Carbonization temperature is 350~500 DEG C.
The graphitization conversion reaction time is 2~5h.
Beneficial effect：
1. various conventional high temperature graphitizations can be made at 1300~1600 DEG C of relatively low temperature using Ni catalysis methods
Method is also still difficult to the graphited biomass material such as effective graphitization of the generation such as cellulose, coconut husk, walnut shell, wood chip
Conversion, 2800 DEG C needed for being significantly less than conventional graphite.
2. products therefrom degree of graphitization more than 50%, and can reach the crystallinity of native graphite.It is in 20MPa pressure
Lower electrical conductivity can exceed 60Scm-1, can further develop practical value for example as conductive material, electromagnetic shielding material or
Further prepare Graphene.
Brief description of the drawings
Fig. 1 is the XRD comparison diagrams after cellulose graphitization processing with natural graphite powder.
Fig. 2 is the TEM figures after cellulose graphitization processing, wherein, right figure is partial enlargement.
Fig. 3 is electrical conductivity and pressure dependence figure after different material graphitization processing.
Specific embodiment
A kind of preparation method of biomass-based graphitized material, comprises the following steps that：
(1) raw material cellulose, lignin, coconut husk, wood chip, walnut shell, phoenix tree leaf etc. are fully dried at 140 DEG C
After be placed in close crucible (if feed particulate material then carries out pulverization process before charing), in charing process 1h at 400 DEG C.Will
Product after charing impregnated in containing a certain amount of Ni2+The aqueous solution in overnight, obtain certain Ni load capacity after drying at 140 DEG C
Charcoal, it is stand-by.
(2) graphitization conversion：The charcoal for loading Ni is placed in high temperature resistant close crucible, being placed in carries out graphitization in high temperature furnace
Reaction certain hour, washing is impregnated until maceration extract is in colourless to remove metal catalytic after cooling repeatedly with concentrated hydrochloric acid (37%)
Agent, is finally washed with distilled water to neutral and dries, and obtains final product.
W metal carrying capacity is 2~5mmol/g C；
Graphitization reaction temperature is 1300~1600 DEG C；
The graphitization reaction time is 2~5h.
The present invention is difficult to, by this problem of conventional method generation graphitization, employ Ni and urge for various biomass materials
Change method has successfully been obtained degree of graphitization product higher, is significantly less than often with the graphite-structure more than 40 layers, and temperature
2800 DEG C needed for rule graphitization.In addition products therefrom has preferable electrical conductivity, and it can in electrical conductivity highest under 20MPa pressure
More than 60Scm-1, had a good application prospect the fields such as conductive material, electromagnetic shielding material are prepared.
Embodiment 1：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 6mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 3h is reacted at being warming up to 1300 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 27.6% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
36.83S·cm-1。
Embodiment 2：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 6mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 3h is reacted at being warming up to 1400 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 46.5% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
54.05S·cm-1。
Embodiment 3：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 6mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 3h is reacted at being warming up to 1600 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 54.6% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
62.96S·cm-1。
Embodiment 4：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 4mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 3h is reacted at being warming up to 1400 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 31.4% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
45.02S·cm-1。
Embodiment 5：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 10mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 3h is reacted at being warming up to 1400 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 48.4% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
55.21S·cm-1。
Embodiment 6：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 6mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 2h is reacted at being warming up to 1400 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 30.2% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
43.28S·cm-1。
Embodiment 7：
Cellulose is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 6mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 5h is reacted at being warming up to 1400 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 47.2% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
53.78S·cm-1。
Embodiment 8：
Lignin is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings and impregnated in and contain
A certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is 6mmol in charcoal sample.Will
The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, and 3h is reacted at being warming up to 1400 DEG C, and dense salt is used after cooling
Dipping washing, up to maceration extract is in colourless to remove metallic catalyst, is finally washed with distilled water to neutrality simultaneously repeatedly for acid (37%)
Drying, obtains final product.It is 24.4% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
31.19S·cm-1。
Embodiment 9：
Walnut shell after crushing is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings
Impregnated in containing a certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is in charcoal sample
6mmol.The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, 3h is reacted at being warming up to 1400 DEG C, cooled down
Washing is impregnated repeatedly with concentrated hydrochloric acid (37%) afterwards until maceration extract finally uses distillation water washing in colourless to remove metallic catalyst
To neutral and dry, final product is obtained.It is 43.0% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
It is 54.20Scm-1。
Embodiment 10：
Coconut husk after crushing is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product leaching after 2g charings
Stain is in containing a certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is in charcoal sample
6mmol.The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, 3h is reacted at being warming up to 1400 DEG C, cooled down
Washing is impregnated repeatedly with concentrated hydrochloric acid (37%) afterwards until maceration extract finally uses distillation water washing in colourless to remove metallic catalyst
To neutral and dry, final product is obtained.It is 37.2% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
It is 44.84Scm-1。
Embodiment 11：
Wood chip after crushing is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product leaching after 2g charings
Stain is in containing a certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, Ni carrying capacity is now born in charcoal sample is
6mmol.The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, 3h is reacted at being warming up to 1400 DEG C, cooled down
Washing is impregnated repeatedly with concentrated hydrochloric acid (37%) afterwards until maceration extract finally uses distillation water washing in colourless to remove metallic catalyst
To neutral and dry, final product is obtained.It is 22.8% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
It is 45.04Scm-1。
Embodiment 12：
Phoenix tree leaf after crushing is placed in close crucible, in charing process 1h at 400 DEG C.Weigh the product after 2g charings
Impregnated in containing a certain amount of Ni2+The aqueous solution in overnight, the dried for standby at 140 DEG C afterwards, now Ni load capacity is in charcoal sample
6mmol.The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace, 3h is reacted at being warming up to 1400 DEG C, cooled down
Washing is impregnated repeatedly with concentrated hydrochloric acid (37%) afterwards until maceration extract finally uses distillation water washing in colourless to remove metallic catalyst
To neutral and dry, final product is obtained.It is 24.6% to be computed the product degree of graphitization, and it is in electrical conductivity under 20MPa pressure
It is 29.24Scm-1。
Claims (6)
1. a kind of biomass-based graphitized material, it is characterised in that biomass material is first carbonized, then Ni is loaded by infusion process urge
After agent, under 1300~1600 DEG C of high-temperature closeds, under Ni catalyst actions, there is effective graphitization conversion, given birth to
Material base graphitized material, the degree of graphitization of described biomass-based graphitized material reaches the knot of native graphite more than 50%
Brilliant degree, with the graphite-structure more than 40 layers, electrical conductivity is more than 60Scm under 20MPa pressure-1。
2. biomass-based graphitized material as claimed in claim 1, it is characterised in that described biomass material includes fiber
Any one or a few in element, lignin, coconut husk, wood chip, walnut shell, phoenix tree leaf.
3. biomass-based graphitized material as claimed in claim 1, it is characterised in that the load capacity of Ni catalyst is 2~
5mmol/g C。
4. a kind of method for preparing any described biomass-based graphitized material of claims 1 to 3, it is characterised in that including
Following steps：
The first step, the preparation of charcoal and the load of metallic catalyst：Biomass material is placed in charing process in close crucible
Charcoal is obtained, charcoal be impregnated in and contained Ni2+The aqueous solution in overnight, be dried to obtain afterwards load Ni charcoal；
Second step, graphitization conversion：The charcoal for loading Ni is placed in high temperature resistant close crucible, is placed in high temperature furnace and is reacted,
Ni2+Because the reduction of charcoal is changed into simple substance Ni, charcoal carries out graphitization conversion under the catalysis of simple substance Ni, finally uses pickling
Bio-based graphitized material is obtained after washing away Ni.
5. the method for preparing biomass-based graphitized material as claimed in claim 4, it is characterised in that carbonization temperature is 350
~500 DEG C.
6. the method for preparing biomass-based graphitized material as claimed in claim 4, it is characterised in that graphitization conversion reaction
Time is 2~5h.
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Cited By (7)
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| CN107799771A (en) * | 2017-11-16 | 2018-03-13 | 湖州创亚动力电池材料有限公司 | A kind of carbon negative pole material for lithium ion battery and preparation method thereof |
| CN108479782A (en) * | 2018-04-09 | 2018-09-04 | 北京化工大学 | P-nitrophenol adds hydrogen support type yolk-eggshell nano-structured calalyst and preparation method |
| CN109603810A (en) * | 2018-12-28 | 2019-04-12 | 湖南大学 | Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and its preparation method and application |
| CN110085863A (en) * | 2019-04-26 | 2019-08-02 | 桑顿新能源科技有限公司 | Graphite cathode material and preparation method thereof, battery |
| CN111892048A (en) * | 2020-06-29 | 2020-11-06 | 中合天成科技发展(北京)有限公司 | Palm-based artificial graphite and preparation method thereof |
| CN112624104A (en) * | 2021-01-08 | 2021-04-09 | 中国林业科学研究院林产化学工业研究所 | Preparation method of wood fiber-based high-conductivity carbon material |
| CN112788934A (en) * | 2020-12-18 | 2021-05-11 | 中国林业科学研究院林产化学工业研究所 | Preparation method of wood fiber-based electromagnetic shielding carbon material |
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| CN107799771A (en) * | 2017-11-16 | 2018-03-13 | 湖州创亚动力电池材料有限公司 | A kind of carbon negative pole material for lithium ion battery and preparation method thereof |
| CN108479782A (en) * | 2018-04-09 | 2018-09-04 | 北京化工大学 | P-nitrophenol adds hydrogen support type yolk-eggshell nano-structured calalyst and preparation method |
| CN109603810A (en) * | 2018-12-28 | 2019-04-12 | 湖南大学 | Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and its preparation method and application |
| CN109603810B (en) * | 2018-12-28 | 2020-08-07 | 湖南大学 | Molybdenum disulfide nanosheet/porous graphitized biochar composite material and preparation method and application thereof |
| CN110085863A (en) * | 2019-04-26 | 2019-08-02 | 桑顿新能源科技有限公司 | Graphite cathode material and preparation method thereof, battery |
| CN110085863B (en) * | 2019-04-26 | 2024-03-12 | 桑顿新能源科技有限公司 | Graphite negative electrode material, preparation method thereof and battery |
| CN111892048A (en) * | 2020-06-29 | 2020-11-06 | 中合天成科技发展(北京)有限公司 | Palm-based artificial graphite and preparation method thereof |
| CN112788934A (en) * | 2020-12-18 | 2021-05-11 | 中国林业科学研究院林产化学工业研究所 | Preparation method of wood fiber-based electromagnetic shielding carbon material |
| CN112624104A (en) * | 2021-01-08 | 2021-04-09 | 中国林业科学研究院林产化学工业研究所 | Preparation method of wood fiber-based high-conductivity carbon material |
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