CN110523376A - A kind of preparation method of the compound carbon felt of graphene - Google Patents
A kind of preparation method of the compound carbon felt of graphene Download PDFInfo
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- CN110523376A CN110523376A CN201910771592.XA CN201910771592A CN110523376A CN 110523376 A CN110523376 A CN 110523376A CN 201910771592 A CN201910771592 A CN 201910771592A CN 110523376 A CN110523376 A CN 110523376A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention belongs to the preparation fields of compound carbon felt, the preparation method of especially a kind of compound carbon felt of graphene, in the preparation for the compound carbon felt of existing graphene, the mixing velocity between liquid is slower, the problem for causing the preparation efficiency of the compound carbon felt of graphene lower, now propose following scheme, it is the following steps are included: S1: binder diaphragm being shredded, binder is put into n,N-Dimethylformamide with different positions, rabbling mechanism reciprocating motion stirs evenly, and mixed liquor is made；S2: graphene and organic solvent are mixed into mixed liquor with different positions, and rabbling mechanism reciprocating motion stirs evenly, and the second mixed liquor is made；S3: carbon felt slice, label are then immersed in the second mixed liquor；S4: finally taking out carbon felt, and the compound carbon felt of graphene is made in drying, and the present invention can effectively improve the mixing efficiency of solution, solution can be made to mix more uniform, improve the preparation efficiency of the compound carbon felt of graphene.
Description
Technical field
The present invention relates to the preparation sides of the preparation technical field of compound carbon felt more particularly to a kind of compound carbon felt of graphene
Method.
Background technique
Carbon fiber felt is a kind of felt made of carbon fiber, has absorption broad spectrum activity, and capacity is big, to gasoline, aldehydes,
Several times greater to tens times of the organic steams adsorbance specific activity charcoal such as phenols, alcohols, alkene (GAC), have well to inorganic gas
Extensive attention is prepared in adsorptivity (such as No, N, HF, HCl etc.), carbon fiber felt.
Through retrieving, application No. is 201811342101.1 patent documents to disclose a kind of preparation of compound carbon felt of graphene
Method, includes the following steps and process conditions: (1) shredding the binder diaphragm of 50~150mg, and be put into 100~300mL's
In n,N-Dimethylformamide, after stirring 2~5h under the conditions of 120~150 DEG C of temperature, diaphragm is completely dissolved in N, N- dimethyl
In formamide, mixed liquor is formed；Wherein, binder diaphragm is Nafion diaphragm, N-Methyl pyrrolidone NMP diaphragm, polyethylene
PE diaphragm, polytetrafluoroethylene PTFE particle gather inclined fluorine vinyl chloride PVDF powder, binder diaphragm with a thickness of 40~60 μm；
(2) 100~300mg graphene is put into the mixed liquor that step (1) obtains；(3) organic solvent of 400~500mL is mixed into
Step (2) resulting mixed liquor, and stir 8~20h, 500~700rpm/s of revolving speed；(4) it by carbon felt slice, label, and weighs
Original weight；(5) mixed liquor 5~25 times for obtaining carbon felt immersion step (3) of step (4), deposit graphite after immersing every time
The time of alkene is 2~5s；(6) carbon felt that step (5) obtains is put into baking oven, and 100~150 DEG C at a temperature of dry when
Between 8~20h, obtain the compound carbon felt of graphene, the graphene thicknesses of layers in carbon felt is 1~10 μm；(7) it takes out and corresponds to after drying
The carbon felt of label, and weight record is weighed, after weighing, seal carbon felt up for safekeeping, for use.
But the compound carbon felt of above-mentioned graphene is in the preparation, the mixing velocity between liquid is slower, causes graphene multiple
The preparation efficiency for closing carbon felt is lower, therefore we have proposed a kind of preparation methods of the compound carbon felt of graphene, above-mentioned for solving
Problem.
Summary of the invention
The purpose of the present invention is to solve the compound carbon felt of graphene exists in the prior art in the preparation, between liquid
Mixing velocity is slower, the disadvantage for causing the preparation efficiency of the compound carbon felt of graphene lower, and a kind of graphene composite carbon proposed
The preparation method of felt.
To achieve the goals above, present invention employs following technical solutions:
A kind of preparation method of the compound carbon felt of graphene, comprising the following steps:
S1: binder diaphragm is shredded, and binder is put into n,N-Dimethylformamide with different positions, and rabbling mechanism is reciprocal
Movement stirs evenly, and mixed liquor is made；
S2: graphene and organic solvent are mixed into mixed liquor with different positions, and rabbling mechanism reciprocating motion stirs evenly, and are made
Obtain the second mixed liquor；
S3: carbon felt slice, label are then immersed in the second mixed liquor；
S4: finally taking out carbon felt, and the compound carbon felt of graphene is made in drying.
Preferably, in the S1, the binder diaphragm of 50-150mg is shredded, and is put into the N of 100-300mL, N- diformazan
In base formamide, after stirring 1-2h under the conditions of 120-150 DEG C of temperature, diaphragm is completely dissolved in n,N-Dimethylformamide,
Form mixed liquor.
Preferably, in the S1, n,N-Dimethylformamide is placed in agitator tank, and rabbling mechanism includes stirring rod, stirs
Motor and driving motor are mixed, stirring motor is used to that stirring rod is driven to rotate, and driving motor is used to drive stirring motor and stirring rod
Horizontal reciprocating movement.
Preferably, in the S2, the organic solvent of 100-300mg graphene and 400-500mL is mixed into mixed liquor, is stirred
4-8h is mixed, the second mixed liquor is made.
Preferably, the agitator tank is equipped with storage box, and the bottom of storage box offers multiple apertures, binder is first fallen
Into in storage box, binder enters in agitator tank by multiple apertures, and driving motor can also drive while driving stirring motor
Storage box horizontal reciprocating movement enables binder to be uniformly sprinkled upon in n,N-Dimethylformamide solution, accelerates mixing efficiency.
Preferably, in the S4, carbon felt is put into baking oven, when carbon felt is put into, is padded between carbon felt and carbon felt upper heat-resisting
Block, makes between carbon felt and carbon felt that there are gaps, hot gas is uniformly then blowed to carbon felt by fan, in 100-150 DEG C of temperature
Spend lower drying time 5-10h.
Preferably, in the S3, carbon felt immerses the second mixed liquor 5-25 times, and the time of deposition graphene is after immersion every time
2-5s。
Preferably, temperature controller is equipped in the baking oven, temperature controller is used to be monitored the temperature of baking oven.
Preferably, the side of the baking oven is equipped with exhaust outlet, and exhaust outlet is connected with heat-conducting mechanism, what carbon felt generated when drying
Hot gas is arranged from exhaust outlet to heat-conducting mechanism, and heat-conducting mechanism includes spiral heat conducting pipe, and spiral heat conducting pipe hovers above the outside of liquid reserve tank,
Spiral heat conducting pipe is made of copper, and when hot gas passes through spiral heat conducting pipe, heat is conducted through spiral heat conducting pipe to the liquid in liquid reserve tank
It is preheated, n,N-Dimethylformamide goods binder can be stored in liquid reserve tank.
Preferably, the spiral heat conducting pipe is connected with filter mechanism, and filter mechanism includes filter screen and active carbon, exhaust gas warp
It is discharged after filtering.
Compared with prior art, the beneficial effects of the present invention are:
(1) this programme is by the way that binder to be put into n,N-Dimethylformamide with different positions, by graphene and organic molten
Agent is mixed into mixed liquor with different positions, so that binder is uniformly spilt in the solution, is accelerated mixing efficiency；
(2) this programme drives stirring rod rotation by stirring motor, and driving motor drives stirring motor and stirring rod horizontal reciprocating
Movement, so as to so as to be mixed between liquid more uniform thorough；
(3) this programme is recycled by the heat to exhaust gas, can be preheated to solution；
(4) present invention can effectively improve the mixing efficiency of solution, solution can be made to mix more uniform, improve graphene
The preparation efficiency of compound carbon felt.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment one
A kind of preparation method of the compound carbon felt of graphene, comprising the following steps:
S1: the binder diaphragm of 50mg is shredded, and is put into the n,N-Dimethylformamide of 100mL, in 120 DEG C of temperature strip
After stirring 1h under part, diaphragm is completely dissolved in n,N-Dimethylformamide, and binder is put into N, N- dimethyl with different positions
In formamide, rabbling mechanism reciprocating motion is stirred evenly, and mixed liquor is made, and n,N-Dimethylformamide is placed in agitator tank,
Rabbling mechanism includes stirring rod, stirring motor and driving motor, and stirring motor is used to that stirring rod is driven to rotate, and driving motor is used to
Stirring motor and stirring rod horizontal reciprocating movement are driven, agitator tank is equipped with storage box, and the bottom of storage box offers multiple small
Hole first pours binder in storage box into, and binder enters in agitator tank by multiple apertures, and driving motor drives stirring motor
While can also drive storage box horizontal reciprocating movement, so that binder is uniformly sprinkled upon n,N-Dimethylformamide solution
In, accelerate mixing efficiency；
S2: the organic solvent of 100mg graphene and 400mL is mixed into mixed liquor, stirs 4h, graphene and organic solvent be not with
Same position is mixed into mixed liquor, and rabbling mechanism reciprocating motion stirs evenly, and the second mixed liquor is made,；
S3: by carbon felt slice, label, carbon felt immerses the second mixed liquor 5 times, and the time that graphene is deposited after immersing every time is 2s；
S4: carbon felt is put into baking oven, and when carbon felt is put into, upper resistance to heat block is padded between carbon felt and carbon felt, make carbon felt and carbon felt it
Between there are gaps, hot gas is uniformly then blowed to by carbon felt by fan, in 100 DEG C of at a temperature of drying time 5h, stone is made
The black compound carbon felt of alkene, the baking oven is interior to be equipped with temperature controller, and temperature controller is used to be monitored the temperature of baking oven, described
The side of baking oven is equipped with exhaust outlet, and exhaust outlet is connected with heat-conducting mechanism, and the hot gas that carbon felt generates when drying arranges guide by exhaust outlet
Heat engine structure, heat-conducting mechanism include spiral heat conducting pipe, and spiral heat conducting pipe hovers above the outside of liquid reserve tank, and spiral heat conducting pipe is by copper
At when hot gas passes through spiral heat conducting pipe, heat preheats the liquid in liquid reserve tank through the conduction of spiral heat conducting pipe, in liquid reserve tank
N,N-Dimethylformamide goods binder can be stored, the spiral heat conducting pipe is connected with filter mechanism, and filter mechanism includes filtering
Net and active carbon, exhaust gas are discharged after filtering.
Embodiment two
A kind of preparation method of the compound carbon felt of graphene, comprising the following steps:
S1: the binder diaphragm of 100mg is shredded, and is put into the n,N-Dimethylformamide of 200mL, in 130 DEG C of temperature
Under the conditions of stir 1.5h after, diaphragm is completely dissolved in n,N-Dimethylformamide, and binder is put into N, N- bis- with different positions
In methylformamide, rabbling mechanism reciprocating motion is stirred evenly, and mixed liquor is made, and n,N-Dimethylformamide is placed on agitator tank
Interior, rabbling mechanism includes stirring rod, stirring motor and driving motor, and stirring motor is used to that stirring rod is driven to rotate, driving motor
For driving stirring motor and stirring rod horizontal reciprocating movement, agitator tank is equipped with storage box, and the bottom of storage box offers more
A aperture first pours binder in storage box into, and binder enters in agitator tank by multiple apertures, driving motor driving stirring
Storage box horizontal reciprocating movement can be also driven while motor, so that binder is uniformly sprinkled upon n,N-Dimethylformamide molten
In liquid, accelerate mixing efficiency；
S2: the organic solvent of 200mg graphene and 450mL is mixed into mixed liquor, stirs 4-8h, graphene and organic solvent with
Different positions are mixed into mixed liquor, and rabbling mechanism reciprocating motion stirs evenly, and the second mixed liquor is made,；
S3: by carbon felt slice, label, carbon felt immerses the second mixed liquor 15 times, and the time that graphene is deposited after immersing every time is 3s；
S4: carbon felt is put into baking oven, and when carbon felt is put into, upper resistance to heat block is padded between carbon felt and carbon felt, make carbon felt and carbon felt it
Between there are gaps, hot gas is uniformly then blowed to by carbon felt by fan, in 130 DEG C of at a temperature of drying time 7h, stone is made
The black compound carbon felt of alkene, the baking oven is interior to be equipped with temperature controller, and temperature controller is used to be monitored the temperature of baking oven, described
The side of baking oven is equipped with exhaust outlet, and exhaust outlet is connected with heat-conducting mechanism, and the hot gas that carbon felt generates when drying arranges guide by exhaust outlet
Heat engine structure, heat-conducting mechanism include spiral heat conducting pipe, and spiral heat conducting pipe hovers above the outside of liquid reserve tank, and spiral heat conducting pipe is by copper
At when hot gas passes through spiral heat conducting pipe, heat preheats the liquid in liquid reserve tank through the conduction of spiral heat conducting pipe, in liquid reserve tank
N,N-Dimethylformamide goods binder can be stored, the spiral heat conducting pipe is connected with filter mechanism, and filter mechanism includes filtering
Net and active carbon, exhaust gas are discharged after filtering.
Embodiment three
A kind of preparation method of the compound carbon felt of graphene, comprising the following steps:
S1: the binder diaphragm of 150mg is shredded, and is put into the n,N-Dimethylformamide of 300mL, in 150 DEG C of temperature
Under the conditions of stir 2h after, diaphragm is completely dissolved in n,N-Dimethylformamide, and binder is put into N, N- diformazan with different positions
In base formamide, rabbling mechanism reciprocating motion is stirred evenly, and mixed liquor is made, and n,N-Dimethylformamide is placed on agitator tank
Interior, rabbling mechanism includes stirring rod, stirring motor and driving motor, and stirring motor is used to that stirring rod is driven to rotate, driving motor
For driving stirring motor and stirring rod horizontal reciprocating movement, agitator tank is equipped with storage box, and the bottom of storage box offers more
A aperture first pours binder in storage box into, and binder enters in agitator tank by multiple apertures, driving motor driving stirring
Storage box horizontal reciprocating movement can be also driven while motor, so that binder is uniformly sprinkled upon n,N-Dimethylformamide molten
In liquid, accelerate mixing efficiency；
S2: the organic solvent of 300mg graphene and 500mL is mixed into mixed liquor, stirs 8h, graphene and organic solvent be not with
Same position is mixed into mixed liquor, and rabbling mechanism reciprocating motion stirs evenly, and the second mixed liquor is made,；
S3: by carbon felt slice, label, carbon felt immerses the second mixed liquor 25 times, and the time that graphene is deposited after immersing every time is 5s；
S4: carbon felt is put into baking oven, and when carbon felt is put into, upper resistance to heat block is padded between carbon felt and carbon felt, make carbon felt and carbon felt it
Between there are gaps, hot gas is uniformly then blowed to by carbon felt by fan, in 150 DEG C of at a temperature of drying time 10h, stone is made
The black compound carbon felt of alkene, the baking oven is interior to be equipped with temperature controller, and temperature controller is used to be monitored the temperature of baking oven, described
The side of baking oven is equipped with exhaust outlet, and exhaust outlet is connected with heat-conducting mechanism, and the hot gas that carbon felt generates when drying arranges guide by exhaust outlet
Heat engine structure, heat-conducting mechanism include spiral heat conducting pipe, and spiral heat conducting pipe hovers above the outside of liquid reserve tank, and spiral heat conducting pipe is by copper
At when hot gas passes through spiral heat conducting pipe, heat preheats the liquid in liquid reserve tank through the conduction of spiral heat conducting pipe, in liquid reserve tank
N,N-Dimethylformamide goods binder can be stored, the spiral heat conducting pipe is connected with filter mechanism, and filter mechanism includes filtering
Net and active carbon, exhaust gas are discharged after filtering.
By the preparation method for the compound carbon felt of graphene that embodiment one, two, three proposes, solution can be effectively improved
Mixing efficiency can be such that solution mixes more uniform, improve the preparation efficiency of the compound carbon felt of graphene, and embodiment two is most
Good embodiment.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of the compound carbon felt of graphene, comprising the following steps:
S1: binder diaphragm is shredded, and binder is put into n,N-Dimethylformamide with different positions, and rabbling mechanism is reciprocal
Movement stirs evenly, and mixed liquor is made；
S2: graphene and organic solvent are mixed into mixed liquor with different positions, and rabbling mechanism reciprocating motion stirs evenly, and are made
Obtain the second mixed liquor；
S3: carbon felt slice, label are then immersed in the second mixed liquor；
S4: finally taking out carbon felt, and the compound carbon felt of graphene is made in drying.
2. a kind of preparation method of the compound carbon felt of graphene according to claim 1, which is characterized in that, will in the S1
The binder diaphragm of 50-150mg shreds, and is put into the n,N-Dimethylformamide of 100-300mL, in 120-150 DEG C of temperature
After stirring 1-2h under the conditions of degree, diaphragm is completely dissolved in n,N-Dimethylformamide, forms mixed liquor.
3. a kind of preparation method of the compound carbon felt of graphene according to claim 1, which is characterized in that in the S1, N,
Dinethylformamide is placed in agitator tank, and rabbling mechanism includes stirring rod, stirring motor and driving motor, and stirring motor is used
Stirring rod is driven to rotate, driving motor is used to drive stirring motor and stirring rod horizontal reciprocating movement.
4. a kind of preparation method of the compound carbon felt of graphene according to claim 1, which is characterized in that, will in the S2
The organic solvent of 100-300mg graphene and 400-500mL are mixed into mixed liquor, stir 4-8h, and the second mixed liquor is made.
5. a kind of preparation method of the compound carbon felt of graphene according to claim 3, which is characterized in that on the agitator tank
Equipped with storage box, the bottom of storage box offers multiple apertures, and binder is first poured into storage box, and binder is by multiple small
Hole enters in agitator tank, and driving motor can also drive storage box horizontal reciprocating movement while driving stirring motor, makes binder
It can uniformly be sprinkled upon in n,N-Dimethylformamide solution, accelerate mixing efficiency.
6. a kind of preparation method of the compound carbon felt of graphene according to claim 1, which is characterized in that, will in the S4
Carbon felt is put into baking oven, and when carbon felt is put into, upper resistance to heat block is padded between carbon felt and carbon felt, makes the presence of seam between carbon felt and carbon felt
Then hot gas is uniformly blowed to carbon felt by fan by gap, in 100-150 DEG C of at a temperature of drying time 5-10h.
7. a kind of preparation method of the compound carbon felt of graphene according to claim 1, which is characterized in that in the S3, carbon
Felt immerses the second mixed liquor 5-25 times, and the time that graphene is deposited after immersing every time is 2-5s.
8. a kind of preparation method of the compound carbon felt of graphene according to claim 6, which is characterized in that set in the baking oven
There is temperature controller, temperature controller is used to be monitored the temperature of baking oven.
9. a kind of preparation method of the compound carbon felt of graphene according to claim 6, which is characterized in that the one of the baking oven
Side is equipped with exhaust outlet, and exhaust outlet is connected with heat-conducting mechanism, and the hot gas that carbon felt generates when drying is arranged to heat-conducting mechanism from exhaust outlet, led
Heat engine structure includes spiral heat conducting pipe, and spiral heat conducting pipe hovers above the outside of liquid reserve tank, and spiral heat conducting pipe is made of copper, and hot gas passes through
When spiral heat conducting pipe, heat preheats the liquid in liquid reserve tank through the conduction of spiral heat conducting pipe, and N, N- can be stored in liquid reserve tank
Dimethylformamide goods binder.
10. a kind of preparation method of the compound carbon felt of graphene according to claim 9, which is characterized in that the spiral is led
Heat pipe is connected with filter mechanism, and filter mechanism includes filter screen and active carbon, and exhaust gas is discharged after filtering.
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| CN109473685A (en) * | 2018-11-12 | 2019-03-15 | 湖南国昶能源科技有限公司 | A kind of preparation method of the compound carbon felt of graphene |
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| CN107873175A (en) * | 2017-11-21 | 2018-04-06 | 湖南辉讯企业管理有限公司 | One kind is based on reciprocating seed dresser |
| CN207815847U (en) * | 2017-12-15 | 2018-09-04 | 婺源县林香实业有限公司 | A kind of energy-saving folium cortex eucommiae drying unit |
| CN208106911U (en) * | 2018-04-13 | 2018-11-16 | 四川省江油润生石墨毡有限公司 | A kind of automatic forming equipment making hard carbon felt and graphite felt letter material |
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Application publication date: 20191203 |