CN111704131A - Preparation method of carbon material prepared from bamboo - Google Patents
Preparation method of carbon material prepared from bamboo Download PDFInfo
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- CN111704131A CN111704131A CN202010672319.4A CN202010672319A CN111704131A CN 111704131 A CN111704131 A CN 111704131A CN 202010672319 A CN202010672319 A CN 202010672319A CN 111704131 A CN111704131 A CN 111704131A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C4/00—Crushing or disintegrating by roller mills
- B02C4/02—Crushing or disintegrating by roller mills with two or more rollers
- B02C4/08—Crushing or disintegrating by roller mills with two or more rollers with co-operating corrugated or toothed crushing-rollers
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Abstract
The invention discloses a preparation method of a bamboo prepared carbon material, belonging to the technical field of carbon material preparation, and the preparation method comprises the following steps: s1, preparing bamboo-based carbon: cutting moso bamboo stalks into segments, washing, drying, crushing into particles through a crushing device, placing the crushed moso bamboo particles into a tubular furnace, and calcining at the temperature of 600 ℃ in the nitrogen atmosphere and 400-; s2, preparation of an activated product: soaking the prepared bamboo-based carbon into a KOH solution, and performing soaking activation to obtain an activated product; s3, preparation of carbon material: the prepared activated product is placed in a tubular furnace, activated under the nitrogen atmosphere and at the temperature of 600-800 ℃, washed by dilute hydrochloric acid and distilled water until the solution is neutral, and then dried in vacuum at the temperature of 80 ℃ to obtain the porous carbon material.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a preparation method of a carbon material prepared by bamboo.
Background
The carbon material is an ancient and young material, namely, ancient products and products innovated by modern scientific and technical progress, and the novel carbon material mainly comprises activated carbon, carbon fiber, graphene, graphite, a carbon nanotube, diamond, fullerene and the like. The novel carbon material has a series of excellent characteristics of small density, high strength, good rigidity, high temperature resistance, chemical corrosion resistance, radiation resistance, fatigue resistance, high electric conductivity, high heat conductivity, ablation resistance, small thermal expansion and good physiological compatibility, and can be applied to the fields of metallurgy, chemical industry, machinery, automobiles, medical treatment, environmental protection, daily life of buildings and the like.
The traditional carbon material is mostly prepared from petroleum coke, coal coke and other disposable resources with high carbon content, the defects of long preparation period, low yield, environmental pollution and the like exist, and plant materials such as cellulose, hemicellulose, lignin and the like have rich sources, are renewable and are environment-friendly, so that the preparation of the carbon material by taking biomass such as pinecones, rapeseeds, oat hulls, corn stalks and the like as raw materials becomes a hotspot of research in recent years.
The moso bamboo has abundant natural cellulose resources, and compared with biomass such as pine cone, rapeseed, oat hull, corn stalk and the like, the moso bamboo has the advantages of easy reproduction, high growth speed, short mature period, high yield and the like. However, the preparation of carbon materials by using moso bamboos as carbon sources has not been applied and popularized yet, and therefore, the invention provides a preparation method of carbon materials by using moso bamboos.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a bamboo-made carbon material.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a bamboo prepared carbon material comprises the following steps:
s1 preparation of bamboo-based charcoal
Cutting moso bamboo stalks into sections, washing and drying each section, crushing the sections into particles through a crushing device, placing the crushed moso bamboo particles into a tubular furnace, and calcining the particles for 2-3h at the temperature of 600 ℃ in the atmosphere of nitrogen and 400-;
s2 preparation of activated product
Soaking the prepared bamboo-based carbon into 10mol/L KOH solution, and soaking and activating for 2-3h at the temperature of 40-60 ℃ under stirring to obtain an activated product;
s3 preparation of carbon material
And (3) placing the obtained activation product in a tubular furnace, activating for 2-3h under the nitrogen atmosphere and at the temperature of 600-800 ℃, washing by using dilute hydrochloric acid and distilled water until the solution is neutral, and then carrying out vacuum drying at the temperature of 80 ℃ to obtain the porous carbon material.
More preferably: in step S1, the mass ratio of the KOH solution to the bamboo-based charcoal is 2-4: 1.
more preferably: in steps S1 and S3, the flow rate of the nitrogen gas is 0.5 to 1L/min.
More preferably: in step S1, the crushing apparatus includes a body, a hole sealing mechanism, a sheet feeding mechanism, a double-roller type crushing mechanism, a positioning member, a cutting condition, and a strip cutting cylinder;
the machine body is provided with an insertion hole and a discharge hole, the hole sealing mechanism is positioned in the machine body and used for sealing the insertion hole, the positioning piece and the cutting condition are both positioned in the machine body, the positioning piece comprises a front end and a rear end, the front end of the positioning piece is close to the insertion hole, the hollow cylindrical moso bamboo is inserted in the positioning piece through the insertion hole, and the strip cutting cylinder is used for driving the cutting condition to horizontally move so as to cut the hollow cylindrical moso bamboo into strips;
the sheet discharging mechanism is used for driving the positioning piece and the cutting condition to rotate so that the cut strip moso bamboos fall downwards and are crushed through the double-roller type crushing mechanism.
More preferably: the positioning piece comprises an inserting piece, a slotted hole and a connecting ring;
the inserting pieces are arranged in a plurality and are enclosed to form a cylinder, hollow cylindrical moso bamboos are inserted into the outer surface of the cylinder, the outer diameter of the cylinder is smaller than the inner diameter of the hollow cylindrical moso bamboos, one end of the cylinder points to the inserting holes, a fixing ring is fixed at one end of the other end of the cylinder far away from the inserting holes, the connecting ring is fixed at the top in the machine body and sleeved on the outer surface of the fixing ring, and the fixing ring is embedded in the inner side of the connecting ring and is in rotating fit with the;
the slotted hole is positioned between the adjacent inserting sheets.
More preferably: the cutting conditions comprise a slitting knife, a driven gear and a fixed pipe;
the fixed pipe is positioned in the cylinder and is arranged in a sliding manner along the axial direction of the cylinder, one side of the strip cutter is fixed on the circumferential surface of the fixed pipe, the other side of the strip cutter penetrates through the slotted hole and extends outwards, and the end, pointing to the jack, of the strip cutter is an opening part;
the fixed pipe is kept away from one end of the jack and is fixedly provided with a connecting disc, and the slitting cylinder is installed on the machine body and is used for driving the connecting disc, the fixed pipe and the slitting knife to move back and forth along the axial direction of the cylinder.
More preferably: be fixed with driven gear on the connection pad, driven gear with the connection pad diameter all is less than the drum internal diameter, driven gear one side with the connection pad is fixed, and the mounting groove has been seted up to the opposite side, the slitting cylinder includes the piston rod, the piston rod end fixing has the connection minor axis, connect the minor axis and install in the mounting groove and with driven gear normal running fit, the slitting cylinder is installed on the organism.
More preferably: the slice feeding mechanism comprises a driving motor and a driving gear;
the driving motor is installed on the machine body, the driving gear is fixed on an output shaft of the driving motor, and the driving gear is meshed with the driven gear and is used for driving the fixed pipe, the slitting knife, the cylinder and the fixed ring to rotate on the connecting ring along the central axis of the cylinder.
More preferably: the hole sealing mechanism comprises a hole sealing plate, an abrasion-resistant plate and a lifting air cylinder;
the lifting cylinder is arranged at the bottom in the machine body, the hole sealing plate and the jack are positioned on the same side of the machine body, the hole sealing plate is in contact with the side wall of the machine body and is in up-and-down sliding fit with the side wall of the machine body, and the lifting cylinder is used for driving the hole sealing plate to move up and down;
the wear-resisting plate is fixed on the inner side of the hole sealing plate and used for tightly abutting against hollow cylindrical moso bamboos so as to be matched with the strip cutting knife for cutting strips.
More preferably: the double-roller type crushing mechanism comprises a crushing motor, a first crushing roller, a second crushing roller, a driving shaft and a driven shaft;
the crushing motor is installed in the organism outside, the driving shaft is fixed on the crushing motor output shaft, first crushing roller is fixed on the driving shaft and with the coaxial rotation setting of driving shaft, the driven shaft rotates to be connected on the organism, the second crushing roller is fixed on the driving shaft and with the coaxial rotation setting of driving shaft, the second crushing roller with first crushing roller meshing setting.
In conclusion, the invention has the following beneficial effects: the preparation method has the following characteristics:
1. the porous carbon material is prepared by taking natural biomass raw material moso bamboo as a carbon source, and has wide raw material source and high yield.
2. The carbonization-impregnation activation-carbonization and washing technologies are utilized to simultaneously carry out pore-forming and nitrogen doping.
3. KOH is used as a pore-forming agent to prepare the bamboo-based microporous carbon material with larger specific surface area.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment, which is mainly used for embodying the internal structure of a machine body;
FIG. 2 is a schematic structural diagram of an embodiment, which is mainly used for showing a matching structure among a hole sealing mechanism, a cutting condition and a positioning member;
FIG. 3 is a schematic structural diagram of an embodiment, which is mainly used for embodying the structure of the hole sealing mechanism;
FIG. 4 is a schematic structural diagram of an embodiment, which is mainly used for embodying the cutting conditions and the matching structure of the positioning members;
FIG. 5 is a schematic structural diagram of an embodiment, mainly used for embodying the structure of the cutting condition;
FIG. 6 is a schematic structural diagram of an embodiment, which is mainly used for embodying the structure of the positioning element;
fig. 7 is a schematic structural diagram of an embodiment, which is mainly used for showing a structure that a cutting condition moves to the front end of a positioning member.
In the figure, 1, a machine body; 2. a hole sealing mechanism; 21. sealing the hole plate; 22. a wear plate; 23. a lifting cylinder; 3. a slice discharging mechanism; 31. a drive motor; 32. a driving gear; 4. a first chute; 5. a jack; 6. a discharge hole; 71. a first crushing roller; 72. a second crushing roller; 73. a drive shaft; 74. a driven shaft; 8. a positioning member; 81. inserting sheets; 82. a fixing ring; 83. a slot; 84. a second chute; 85. a connecting ring; 9. cutting conditions; 91. a slitting knife; 92. a driven gear; 93. mounting grooves; 94. a fixed tube; 95. a second slide bar; 96. a connecting disc; 10. a slitting cylinder; 11. connecting the short shaft; 12. a material guiding sloping plate.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Example 1: a preparation method of a bamboo prepared carbon material comprises the following steps:
s1 preparation of bamboo-based charcoal
Cutting moso bamboo stalks into sections, wherein each section is in a hollow cylinder shape, and the length of each section of moso bamboo is not required to be all consistent and is generally about 20-30 cm; and washing, drying, crushing into particles by a crushing device, placing the crushed moso bamboo particles into a tubular furnace, and calcining for 2 hours at 400 ℃ in a nitrogen atmosphere to obtain the bamboo-based carbon.
Further preferably, the flow rate of nitrogen is 0.8L/min.
S2 preparation of activated product
Soaking the prepared bamboo-based carbon into 10mol/L KOH solution, wherein the mass ratio of the KOH solution to the bamboo-based carbon is 3: 1; dipping and activating for 2h at the temperature of 60 ℃ under stirring to obtain an activated product.
S3 preparation of carbon material
And (3) placing the obtained activated product in a tubular furnace, activating for 2h at 600 ℃ in a nitrogen atmosphere, washing for a plurality of times by using dilute hydrochloric acid and distilled water until the solution is neutral, and then performing vacuum drying at 80 ℃ to obtain the porous carbon material.
Further preferably, the flow rate of nitrogen is 0.8L/min.
In the technical scheme, the obtained porous carbon material is not screened and has different particle sizes, so that when the porous carbon material is used, the porous carbon material can be screened or graded according to application scenes to meet the requirements of different use environments. The invention utilizes ZnCl2KOH or H3PO4Chemically activating with isopore-forming agent, high-temp carbonizing and activating to obtain microporous carbon material2And H3PO4And KOH is used as a pore-foaming agent to obtain larger specific surface area.
The preparation method has the following characteristics:
1. the porous carbon material is prepared by taking natural biomass raw material moso bamboo as a carbon source, and has wide raw material source and high yield.
2. The carbonization-impregnation activation-carbonization and washing technologies are utilized to simultaneously carry out pore-forming and nitrogen doping.
3. KOH is used as a pore-forming agent to prepare the bamboo-based microporous carbon material with larger specific surface area.
As shown in fig. 1 to 7, in step S1, the crushing apparatus includes a machine body 1, a hole sealing mechanism 2, a sheet feeding mechanism 3, a double-roller crushing mechanism, a positioning member 8, a slitting condition 9, and a slitting cylinder 10. The machine body 1 is provided with a jack 5 and a discharge hole 6, the jack 5 and the discharge hole 6 are respectively positioned at two opposite sides of the machine body 1, the jack 5 is positioned at one side of the upper part of the machine body 1, and the discharge hole 6 is positioned at one side of the lower part of the machine body 1.
Referring to fig. 1-7, the positioning member 8 and the cutting member 9 are both located in the machine body 1, the positioning member 8 includes a front end and a rear end, the front end of the positioning member 8 is close to the insertion hole 5, and the cut hollow cylindrical moso bamboo is inserted into the positioning member 8 through the insertion hole 5. The strip cutting cylinder 10 is used for driving the cutting condition 9 to move horizontally so as to cut the hollow cylindrical moso bamboo into a plurality of strip moso bamboo chips along the axial direction of the moso bamboo.
Referring to fig. 1-7, the positioning member 8 preferably includes a tab 81, a slot 83 and a coupling ring 85. The inserting pieces 81 are arranged in a plurality, the inserting pieces 81 are enclosed to form a cylinder, and the cylinder is horizontally arranged and is positioned above the inner part of the machine body 1. The hollow cylindrical moso bamboo is inserted into the outer surface of the cylinder, so that the hollow cylindrical moso bamboo is sleeved on the cylinder, and the outer diameter of the cylinder is smaller than the inner diameter of the hollow cylindrical moso bamboo. One end of the cylinder points to the jack 5, the other end of the cylinder is fixed with a fixing ring 82 at the end far away from the jack 5, and the connecting ring 85 is fixed at the inner top of the machine body 1 and sleeved on the outer surface of the fixing ring 82. Solid fixed ring 82 inlays at go-between 85 inboard and with go-between 85 normal running fit, for solid fixed ring 82 steady and smooth rotation in go-between 85, and prevent solid fixed ring 82 and break away from in the go-between 85, it is concrete, solid fixed ring 82 circumferential surface has seted up T type groove, go-between 85 inboard is fixed with round T type piece, T type piece inlays at T type inslot and rather than sliding fit, so that solid fixed ring 82 rotates along the drum center pin on T type piece. The centers of the connecting ring 85 and the fixing ring 82 are both located on the cylinder center axis. The slots 83 are located between adjacent tabs 81.
In the technical scheme, the cylinder plays a role in positioning and supporting, when the bamboo is crushed, the cut hollow cylindrical moso bamboos are inserted into the cylinder through the insertion holes 5, so that the moso bamboos are sleeved on the cylinder, and then the work of hole sealing, strip cutting and the like is carried out.
Referring to fig. 1 to 7, the strip cutting cylinder 10 is configured to drive the cutting member 9 to move horizontally, so as to cut the hollow cylindrical moso bamboo into a plurality of strip-shaped moso bamboo chips along the axial direction of the moso bamboo. Preferably, the cutting condition 9 includes a slitting knife 91, a driven gear 92, and a fixed pipe 94. The fixed tube 94 is located in the cylinder and is slidably disposed along the axial direction of the cylinder, and specifically, the outer diameter of the fixed tube 94 is the same as the inner diameter of the cylinder. The cylinder is provided with a second sliding groove 84 along the axial direction of the cylinder on the inner side, a second sliding strip 95 is provided on the circumferential surface of the fixed tube 94, and the second sliding strip 95 is embedded in the second sliding groove 84 and can slide in the second sliding groove 84. One side of the slitting knife 91 is fixed on the circumferential surface of the fixed pipe 94, the other side of the slitting knife 91 penetrates through the slotted hole 83 and extends outwards, the slitting knives 91 are arranged in a plurality, and the slitting knives 91 are uniformly distributed on the fixed pipe 94 and are distributed along the circle center of the fixed pipe 94 in a transmitting shape. Similarly, a plurality of slots 83 are provided, and the slots 83 correspond to the slitting knives 91 one by one. The slitting knife 91 is an opening part at one end directed to the insertion hole 5. The fixed tube 94 has a connecting plate 96 fixed to an end thereof remote from the insertion hole 5, and the diameter of the connecting plate 96 is the same as the outer diameter of the fixed tube 94. The slitting cylinder 10 is installed on the machine body 1 and is used for driving the connecting disc 96, the fixed pipe 94 and the slitting knife 91 to move back and forth along the axial direction of the cylinder, so that the hollow cylindrical moso bamboo can be conveniently cut into a plurality of strip moso bamboos.
In the above technical solution, during slitting, under the action of the slitting cylinder 10, the connecting disc 96, the fixed pipe 94 and the slitting knife 91 move towards the direction close to the insertion hole 5, so that the moso bamboo sleeved on the cylinder is split into a plurality of independent strips. The effect of primary crushing is achieved, and the crushing pressure of a follow-up double-roller type crushing mechanism is reduced, so that the crushing efficiency and the crushing quality are improved.
Referring to fig. 1-7, driven gear 92 is fixed to coupling plate 96, and driven gear 92 and coupling plate 96 are both smaller in diameter than the inner diameter of the cylinder. Driven gear 92 one side is fixed with connection pad 96, and mounting groove 93 has been seted up to the opposite side, and slitting cylinder 10 includes the piston rod, and the piston rod end fixing has connection minor axis 11. The connecting stub shaft 11 is installed in the installation groove 93 and is in running fit with the driven gear 92, in order to enable the connecting stub shaft 11 to smoothly and stably rotate in the installation groove 93, and in order to prevent the connecting stub shaft 11 from being separated from the installation groove 93, specifically, the installation groove 93 is a T-shaped groove, and the longitudinal section of the connecting stub shaft 11 at one end connected with the installation groove 93 is a T-shaped section. The lower sheet mechanism 3 is used for driving the cylinder and the cutting condition 9 to rotate so that the cut strip moso bamboos fall downwards and are crushed by the double-roller type crushing mechanism. Preferably, the lower disc mechanism 3 includes a driving motor 31 and a driving gear 32. The driving motor 31 is installed on the shell of the machine body 1 and is positioned below the slitting cylinder 10, and the driving gear 32 is fixed on the output shaft of the driving motor 31. The driving gear 32 is located below the driven gear 92, and the driving gear 32 is engaged with the driven gear 92 and is used for driving the fixed tube 94, the slitting knife 91, the cylinder and the fixed ring 82 to rotate on the connecting ring 85 along the central axis of the cylinder. The central axis of the drive gear 32 is parallel to the central axis of the driven gear 92, and the central axis of the driven gear 92 coincides with the central axis of the cylinder. The drive gear 32 and the driven gear 92 are spur gears so that the driven gear 92 can move on the drive gear 32 in the cylindrical axial direction.
In the technical proposal, after the moso bamboos are split into a plurality of independent strips, the strip moso bamboos positioned at the lower part of the cylinder automatically fall down under the action of the self gravity, the strip moso bamboos on the upper part and two sides of the cylinder are blocked by the strip cutter 91 and the cylinder and can not fall off by self, in order to overcome the defects, the invention is provided with the slice discharging mechanism 3, and a driven gear 92 and a connecting stub shaft 11 are provided on the connecting disc 96, so that when the driving motor 31 is started, the driving gear 32 drives the driven gear 92 to rotate, since the connecting stub shaft 11 is rotationally connected to the driven gear 92, when the driven gear 92 rotates, the driven gear 92 will rotate on the connecting stub shaft 11, at the same time, the fixed tube 94, the slitting knife 91, the cylinder and the fixed ring 82 are driven to rotate on the connecting ring 85 along the central axis of the cylinder, and the strip moso bamboos on the upper part and two sides of the cylinder automatically fall down in the rotating process.
Referring to fig. 1-7, a hole sealing mechanism 2 is located in the machine body 1 and is used for sealing the insertion holes 5, and the hole sealing mechanism 2 comprises a hole sealing plate 21, a wear-resisting plate 22 and a lifting cylinder 23. The lifting cylinder 23 is arranged at the bottom in the machine body 1, the hole sealing plate 21 and the jack 5 are positioned at the same side of the machine body 1, and the hole sealing plate 21 is in contact with the side wall of the machine body 1 and is in up-and-down sliding fit with the side wall of the machine body 1. For the steady up-and-down slip of hole sealing plate 21, preferably, be fixed with first draw runner on the hole sealing plate 21, first spout 4 has been seted up to organism 1 inner wall, and lift cylinder 23 is used for driving hole sealing plate 21 and reciprocates to make first draw runner and first spout 4 up-and-down sliding fit. The wear-resisting plate 22 is fixed on the inner side of the hole sealing plate 21 and used for tightly abutting the hollow cylindrical moso bamboo to match with the strip cutting knife 91 to cut the moso bamboo.
In the above technical scheme, after the moso bamboo is sleeved on the cylinder through the insertion hole 5, the insertion hole 5 needs to be plugged, and then slitting is performed. During plugging, only the air cylinder needs to be started, so that the air cylinder drives the hole sealing plate 21 to slide upwards until the hole sealing plate 21 and the wear-resisting plate 22 in the insertion hole 5 are plugged.
Referring to fig. 1 to 7, the double roller crushing mechanism includes a crushing motor, a first crushing roller 71, a second crushing roller 72, a driving shaft 73, and a driven shaft 74. The crushing motor is arranged outside the machine body 1, and the driving shaft 73 is fixed on the output shaft of the crushing motor. The first crushing roller 71 is fixed to the driving shaft 73 and is provided to rotate coaxially with the driving shaft 73, and the driven shaft 74 is rotatably connected to the machine body 1. The second crushing roller 72 is fixed to the drive shaft 73 and is provided coaxially with the drive shaft 73 so as to be rotatable, and the second crushing roller 72 is provided in mesh with the first crushing roller 71. The double-roller type crushing mechanism is the prior art, and the specific structure and the working principle thereof are not described in detail herein. In order to guide the moso bamboos to fall, specifically, a material guiding sloping plate 12 is fixed in the machine body 1, the upper side of the material guiding sloping plate 12 is fixed on the inner wall of the machine body 1, and the lower side is close to the space between the second crushing roller 72 and the first crushing roller 71. The first crushing roller 71 and the second crushing roller 72 are both positioned below the cylinder, and the material guide sloping plate 12 is positioned between the second crushing roller 72 and the cylinder.
In the technical scheme, during crushing, firstly, the cut hollow cylindrical moso bamboos are inserted into the cylinder through the insertion holes 5, so that the moso bamboos are sleeved on the cylinder, and then the hole sealing plate 21 and the wear-resisting plate 22 are moved to the insertion holes 5 through the lifting cylinder 23, so that the hole sealing effect is realized. After the jack 5 is plugged, the slitting cylinder 10 is started to move the fixed pipe 94 and the slitting knife 91 towards the direction close to the jack 5, so that the hollow cylindrical moso bamboo is cut into strips, after slitting is completed, the slitting cylinder 10 drives the fixed pipe 94 and the slitting knife 91 to reset, and at the moment, the driving gear 32 and the driven gear 92 keep a meshing state again. After the fixed pipe 94 and the slitting knife 91 are reset, the driving motor 31 is started to rotate the fixed pipe 94, the slitting knife 91 and the cylinder on the connecting ring 85, so that the moso bamboos cut into strips fall downwards, and then the moso bamboos are crushed by the first crushing roller 71 and the second crushing roller 72.
Example 2: the difference between the preparation method of the carbon material prepared by the moso bamboo and the embodiment 1 is that the preparation method of the carbon material prepared by the moso bamboo comprises the following steps:
s1 preparation of bamboo-based charcoal
Cutting moso bamboo stalks into sections, wherein each section is in a hollow cylinder shape, and the length of each section of moso bamboo is not required to be all consistent and is generally about 20-30 cm; and washing, drying, crushing into particles by a crushing device, placing the crushed moso bamboo particles into a tubular furnace, and calcining for 2 hours at 600 ℃ in a nitrogen atmosphere to obtain the bamboo-based carbon.
Further preferably, the flow rate of nitrogen is 0.5L/min.
S2 preparation of activated product
Soaking the prepared bamboo-based carbon into 10mol/L KOH solution, wherein the mass ratio of the KOH solution to the bamboo-based carbon is 2: 1; soaking and activating for 2h at 40 ℃ under stirring to obtain an activated product.
S3 preparation of carbon material
And (3) placing the obtained activated product in a tubular furnace, activating for 2h at 700 ℃ in the nitrogen atmosphere, washing for a plurality of times by using dilute hydrochloric acid and distilled water until the solution is neutral, and then carrying out vacuum drying at 80 ℃ to obtain the porous carbon material.
Further preferably, the flow rate of nitrogen is 0.5L/min.
Example 3: the difference between the preparation method of the carbon material prepared by the moso bamboo and the embodiment 1 is that the preparation method of the carbon material prepared by the moso bamboo comprises the following steps:
s1 preparation of bamboo-based charcoal
Cutting moso bamboo stalks into sections, wherein each section is in a hollow cylinder shape, and the length of each section of moso bamboo is not required to be all consistent and is generally about 20-30 cm; and washing, drying, crushing into particles by a crushing device, placing the crushed moso bamboo particles into a tubular furnace, and calcining for 3 hours at 500 ℃ in a nitrogen atmosphere to obtain the bamboo-based carbon.
Further preferably, the flow rate of nitrogen is 1L/min.
S2 preparation of activated product
Soaking the prepared bamboo-based carbon into 10mol/L KOH solution, wherein the mass ratio of the KOH solution to the bamboo-based carbon is 4: 1; and (3) soaking and activating for 3 hours at the temperature of 50 ℃ under stirring to obtain an activated product.
S3 preparation of carbon material
And (3) placing the obtained activated product in a tubular furnace, activating for 3h at 800 ℃ in a nitrogen atmosphere, washing for a plurality of times by using dilute hydrochloric acid and distilled water until the solution is neutral, and then performing vacuum drying at 80 ℃ to obtain the porous carbon material.
Further preferably, the flow rate of nitrogen is 1L/min.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that several improvements and modifications without departing from the principle of the present invention will occur to those skilled in the art, and such improvements and modifications should also be construed as within the scope of the present invention.
Claims (10)
1. A preparation method of a bamboo prepared carbon material is characterized by comprising the following steps: the method comprises the following steps:
s1 preparation of bamboo-based charcoal
Cutting moso bamboo stalks into sections, washing and drying each section, crushing the sections into particles through a crushing device, placing the crushed moso bamboo particles into a tubular furnace, and calcining the particles for 2-3h at the temperature of 600 ℃ in the atmosphere of nitrogen and 400-;
s2 preparation of activated product
Soaking the prepared bamboo-based carbon into 10mol/L KOH solution, and soaking and activating for 2-3h at the temperature of 40-60 ℃ under stirring to obtain an activated product;
s3 preparation of carbon material
And (3) placing the obtained activation product in a tubular furnace, activating for 2-3h under the nitrogen atmosphere and at the temperature of 600-800 ℃, washing by using dilute hydrochloric acid and distilled water until the solution is neutral, and then carrying out vacuum drying at the temperature of 80 ℃ to obtain the porous carbon material.
2. The method for preparing a carbon material by bamboo as claimed in claim 1, wherein: in step S1, the mass ratio of the KOH solution to the bamboo-based charcoal is 2-4: 1.
3. the method for preparing a carbon material by bamboo as claimed in claim 1, wherein: in steps S1 and S3, the flow rate of the nitrogen gas is 0.5 to 1L/min.
4. The method for preparing a carbon material by bamboo as claimed in claim 1, wherein: in step S1, the crushing apparatus includes a machine body (1), a hole sealing mechanism (2), a sheet discharging mechanism (3), a double-roller crushing mechanism, a positioning member (8), a cutting condition (9), and a strip cutting cylinder (10);
the machine body (1) is provided with a jack (5) and a discharge hole (6), the hole sealing mechanism (2) is located in the machine body (1) and used for sealing the jack (5), the positioning piece (8) and the cutting condition (9) are both located in the machine body (1), the positioning piece (8) comprises a front end and a rear end, the front end of the positioning piece (8) is close to the jack (5), hollow cylindrical moso bamboos are inserted into the positioning piece (8) through the jack (5), and the cutting cylinder (10) is used for driving the cutting condition (9) to horizontally move so as to cut the hollow cylindrical moso bamboos into strips;
and the sheet discharging mechanism (3) is used for driving the positioning piece (8) and the cutting condition (9) to rotate so that the cut strip moso bamboos fall downwards and are crushed by the double-roller crushing mechanism.
5. The method for preparing a carbon material by bamboo as claimed in claim 4, wherein: the positioning piece (8) comprises an inserting piece (81), a slotted hole (83) and a connecting ring (85);
the inserting pieces (81) are arranged in a plurality, the inserting pieces (81) are enclosed to form a cylinder, hollow cylindrical moso bamboos are inserted into the outer surface of the cylinder, the outer diameter of the cylinder is smaller than the inner diameter of the hollow cylindrical moso bamboos, one end of the cylinder points to the inserting hole (5), a fixing ring (82) is fixed at one end, far away from the inserting hole (5), of the other end of the cylinder, the connecting ring (85) is fixed at the inner top of the machine body (1) and sleeved on the outer surface of the fixing ring (82), and the fixing ring (82) is embedded in the inner side of the connecting ring (85) and is in running fit;
the slotted hole (83) is positioned between the adjacent inserting sheets (81).
6. The method for preparing a carbon material by bamboo as claimed in claim 5, wherein: the cutting condition (9) comprises a slitting knife (91), a driven gear (92) and a fixed pipe (94);
the fixed pipe (94) is positioned in the cylinder and is arranged in a sliding manner along the axial direction of the cylinder, one side of the slitting knife (91) is fixed on the circumferential surface of the fixed pipe (94), the other side of the slitting knife penetrates through the slotted hole (83) and extends outwards, and one end, pointing to the jack (5), of the slitting knife (91) is an opening part;
fixed pipe (94) is keeping away from jack (5) one end is fixed with connection pad (96), slitting cylinder (10) are installed on organism (1) and be used for the drive connection pad (96), fixed pipe (94) and slitting sword (91) are followed drum axial direction round trip movement.
7. The method for preparing a carbon material by bamboo as claimed in claim 6, wherein: be fixed with driven gear (92) on connection pad (96), driven gear (92) with connection pad (96) diameter all is less than the drum internal diameter, driven gear (92) one side with connection pad (96) are fixed, and mounting groove (93) have been seted up to the opposite side, slitting cylinder (10) includes the piston rod, the piston rod end fixing has connection minor axis (11), install connection minor axis (11) in mounting groove (93) and with driven gear (92) normal running fit, slitting cylinder (10) are installed on organism (1).
8. The method for preparing a carbon material by bamboo as claimed in claim 7, wherein: the slice feeding mechanism (3) comprises a driving motor (31) and a driving gear (32);
the driving motor (31) is installed on the machine body (1), the driving gear (32) is fixed on an output shaft of the driving motor (31), and the driving gear (32) is meshed with the driven gear (92) and is used for driving the fixed pipe (94), the slitting knife (91), the cylinder and the fixed ring (82) to rotate on the connecting ring (85) along the central axis of the cylinder.
9. The method for preparing a carbon material by bamboo as claimed in claim 5, wherein: the hole sealing mechanism (2) comprises a hole sealing plate (21), an abrasion-resistant plate (22) and a lifting cylinder (23);
the lifting cylinder (23) is installed at the bottom in the machine body (1), the hole sealing plate (21) and the jack (5) are located on the same side of the machine body (1), the hole sealing plate (21) is in contact with the side wall of the machine body (1) and is in up-and-down sliding fit with the side wall of the machine body (1), and the lifting cylinder (23) is used for driving the hole sealing plate (21) to move up and down;
the wear-resisting plate (22) is fixed on the inner side of the hole sealing plate (21) and used for tightly abutting against hollow cylindrical moso bamboos so as to be matched with the strip cutting knife (91) for cutting strips.
10. The method for preparing a carbon material by bamboo as claimed in claim 5, wherein: the double-roller crushing mechanism comprises a crushing motor, a first crushing roller (71), a second crushing roller (72), a driving shaft (73) and a driven shaft (74);
the crushing motor is installed on the outer side of the machine body (1), the driving shaft (73) is fixed on an output shaft of the crushing motor, the first crushing roller (71) is fixed on the driving shaft (73) and coaxially and rotatably arranged with the driving shaft (73), the driven shaft (74) is rotatably connected to the machine body (1), the second crushing roller (72) is fixed on the driving shaft (73) and coaxially and rotatably arranged with the driving shaft (73), and the second crushing roller (72) is meshed with the first crushing roller (71).
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| CN114293364A (en) * | 2022-01-28 | 2022-04-08 | 华北电力大学（保定） | Carbon fiber activation method and apparatus |
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Application publication date: 20200925 |