CN214829040U - Three-dimensional graphite alkene industrial production device - Google Patents
Three-dimensional graphite alkene industrial production device Download PDFInfo
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- CN214829040U CN214829040U CN202120446007.1U CN202120446007U CN214829040U CN 214829040 U CN214829040 U CN 214829040U CN 202120446007 U CN202120446007 U CN 202120446007U CN 214829040 U CN214829040 U CN 214829040U
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Abstract
The utility model discloses a three-dimensional graphite alkene industrial production device, the device are including the reation kettle, closed circulation formula centrifugation spray drier, rotary furnace, agitator tank, washing equipment, desiccator, demagnetization machine, fluid energy mill and the packagine machine that set gradually. The device has the advantages of continuous and continuous production, simple equipment, simple operation, energy conservation and environmental protection, is easy to realize automatic and batch industrial production, and can solve the problem of large-scale production of high-quality three-dimensional graphene.
Description
Technical Field
The utility model relates to a graphite alkene production facility technical field specifically is a three-dimensional graphite alkene industrial production device.
Background
Graphene is a two-dimensional material with a thickness of only one carbon atom consisting of carbon atoms arranged in a hexagonal honeycomb lattice with sp2 hybridized orbitals. The graphene has the thermal conductivity coefficient as high as 5300W/m.K, is higher than that of carbon nano tubes and diamond, has the electron mobility exceeding 15000cm2/(V.s) at normal temperature, is higher than that of carbon nano tubes or silicon crystals, has the resistivity of only about 10-6 omega.cm, is lower than that of copper or silver, and is a material with the minimum resistivity. Graphene has such excellent physicochemical properties, but has a fatal disadvantage of easy stacking and agglomeration, resulting in failure to sufficiently exert its properties.
The three-dimensional (3D) graphene material not only has inherent physicochemical properties of graphene, but also solves the problem of stacking and agglomeration of graphene. In addition, the three-dimensional porous micro/nano structure has excellent characteristics of large specific surface area, high mechanical strength and the like. These unique properties make three-dimensional graphene and its composites of great interest in the field of material science.
Chinese invention patent CN 106495134B, CN 102992306B, CN 106927451B discloses a preparation method of three-dimensional graphene. The production equipment of the graphene adopted by the three patents is basically laboratory equipment and is difficult to produce in batch. Particularly, the static sintering equipment causes the product to be hardened into blocks and adhered to the inner wall of the furnace body/saggar and other containers, and the products cannot be taken out normally.
In summary, the existing equipment and method for preparing three-dimensional graphene are basically laboratory-level equipment and method, and cannot process large-scale materials; and intermittent operation, particularly hardening and caking of products in a sintering process, can not be discharged normally, and seriously restricts the continuous and batch industrial production of the three-dimensional graphene.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome above-mentioned prior art's weak point, provide a novel three-dimensional graphite alkene high temperature sintering equipment of efficient.
In order to achieve the above object, the utility model provides a following technical scheme:
the utility model provides a three-dimensional graphite alkene industrial production device, includes reation kettle, closed cycle formula centrifugation spray drier, rotary furnace, agitator tank, washing equipment, desiccator, demagnetization machine, fluid energy mill and the packagine machine that sets gradually.
Preferably, an inert gas injection port is installed in the circulating centrifugal spray dryer.
Preferably, the circulating centrifugal spray dryer is provided with an organic solvent recovery device.
As a preferred scheme, the rotary furnace is provided with a furnace chamber main body, and the furnace chamber main body is made of stainless steel materials or ceramic materials.
Preferably, the material of the oven cavity body is 310S stainless steel
Preferably, the washing equipment is one or more of ceramic membrane equipment, a centrifuge and a plate-and-frame filter press.
As a preferable scheme, the washing equipment is provided with a pH detector and a conductivity detector.
Preferably, the dryer is one or more of a centrifugal spray dryer, a boiling dryer, a fluidized bed dryer, a mesh belt dryer and a vacuum dryer.
As a preferable scheme, a cyclone separator and a bag-type dust collector are arranged in the dryer.
Preferably, the stirring tank is made of PP, PVDF or PTFE material.
Compared with the prior art, the utility model discloses following beneficial effect has:
1. the device has the advantages of continuous production, simple equipment, simplicity in operation, energy conservation, environmental friendliness, easiness in realization of automatic and batch industrial production, and capability of solving the problem of large-scale production of high-quality three-dimensional graphene;
2. the device adopts a closed-loop circulating centrifugal spray dryer, and takes inert gas (such as nitrogen) as drying circulating gas, thereby not only avoiding the moisture absorption and water absorption of strong alkali, but also playing an explosion-proof function and avoiding the explosion of organic solvents such as ethanol and the like. Meanwhile, an organic solvent recovery device is arranged, so that a large amount of organic solvent is recovered and reused, and the energy is saved and the environment is protected;
3. the device adopts a rotary furnace for dynamic sintering, the material is heated uniformly, and the consistency/stability of the product is higher; the materials are granulated in the rotary motion and are changed into small balls (or small particles), the product has good fluidity, and the materials cannot be hardened and agglomerated, so that continuous automatic discharging can be realized;
4. the device adopts washing equipment, especially ceramic membrane equipment, can realize 100% continuous automated production, has reduced the risk that operating personnel is hurt by strong alkali strong acid. And the conductivity meter can more accurately detect the conductivity of the filtrate and can control the purity of the product to the maximum extent.
5. The device adopts a drier, particularly a centrifugal spray drier and a boiling drier, and the dried product is directly granular powder, so that the trouble that the conventional drying agglomeration needs to be crushed again is solved. And the cyclone separator and the bag-type dust collector (or water curtain dust collection) which are equipped with the drying equipment have good functions of dust collection/powder recovery, and the environmental protection of the process is realized.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a medium-three-dimensional graphene industrial production device of the present invention;
in the figure, 1-a reaction kettle, 2-a closed-loop circulating centrifugal spray dryer, 3-a rotary furnace, 4-washing equipment, 5-a dryer, 6-a demagnetizer, 7-a jet mill, 8-a packaging machine and 9-a stirring tank.
Detailed Description
For the purpose of promoting a better understanding of the objects, structures, features, and functions of the invention, reference should now be made to the drawings and detailed description of the invention. It should be noted that the features illustrated in the drawings are not necessarily drawn to scale. Moreover, the described embodiments are only some of the described embodiments of the present invention, and not all of them. All other embodiments, which can be obtained by a person skilled in the art without any inventive work based on the described embodiments of the present invention, belong to the protection scope of the present invention.
Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this disclosure belongs. The use of "first," "second," and similar terms in this disclosure is not intended to indicate any order, quantity, or importance, but rather is used to distinguish one element from another. The terms "connected" or "coupled" and the like are not restricted to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", "front", "rear", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships may also be changed accordingly. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
As shown in fig. 1, the utility model provides a three-dimensional graphite alkene industrial production device, including reation kettle 1, closed circulation formula centrifugal spray drier 2, rotary furnace 3, agitator tank 9, washing equipment 4, desiccator 5, except that magnetic separator 6, fluid energy mill 7, packagine machine 8, feed bin and the conveying equipment that sets gradually. Wherein, the reaction kettle 1 is used for stirring and mixing materials to form mixed slurry. The mixed slurry is sent to a closed-cycle centrifugal spray dryer 2 by pump driving to dry the mixture powder. A feeding machine is arranged between the rotary furnace 3 and the closed-loop circulating centrifugal spray dryer, the mixture powder is transferred into the rotary furnace 3 through the feeding machine to carry out high-temperature reaction, a three-dimensional graphene (3DG) sintering product is generated, dynamic sintering is carried out by adopting the rotary furnace, the material is uniformly heated, and the product consistency/stability is high; the materials are granulated in the rotary motion and are changed into small balls (or small particles), the product has good fluidity, the materials are not hardened and agglomerated, and the continuous automatic discharging can be realized. The stirring tank is connected with the rotary furnace. Discharging the three-dimensional graphene (3DG) sintering product from the rotary furnace into a stirring tank 9 for stirring, and stirring the mixed solution by using the stirring tank 9 to obtain the mixed solution. The washing equipment is used for receiving the mixed solution, carrying out acid washing (hydrochloric acid) to remove alkali and metal simple substances, and then carrying out pure water washing to remove impurity ions (the filtrate requires that the pH is 7 and the conductivity is less than 10us/cm) to obtain 3DG aqueous slurry. And drying the 3DG slurry into powder (3DG powder) by using a dryer 5, removing magnetic substances by using a demagnetizer 6, crushing and grading by using an airflow crusher 7, and finally packaging by using a packaging machine 8 to obtain the final three-dimensional graphene (3 DG).
The circulating centrifugal spray dryer is internally provided with an inert gas jet orifice for jetting inert gas (such as nitrogen). The closed-loop circulating centrifugal spray dryer is adopted, and inert gas is used as drying circulating gas, so that the moisture absorption and water absorption of strong alkali are avoided, the explosion-proof function is achieved, and the explosion of organic solvents such as ethanol and the like can be avoided.
The circulating centrifugal spray dryer is provided with an organic solvent recovery device, so that a large amount of organic solvent is recovered and reused, and the circulating centrifugal spray dryer is energy-saving and environment-friendly.
The rotary furnace is provided with a furnace chamber main body, and the furnace chamber main body is made of stainless steel materials or ceramic materials, preferably 310S stainless steel.
The washing equipment is one or more of ceramic membrane equipment, a centrifugal machine and a plate-and-frame filter press, preferably ceramic membrane equipment, the ceramic membrane equipment can realize 100% continuous automatic production, and the risk that operators are injured by strong alkali and strong acid is reduced.
The washing equipment is provided with a pH detector and a conductivity detector. The conductivity meter can be configured to more accurately detect the conductivity of the filtrate, and the purity of the product can be controlled to the greatest extent.
The dryer is one or more of a centrifugal spray dryer, a boiling dryer, a fluidized bed dryer, a mesh belt dryer and a vacuum dryer. The dried product is directly granular powder, thus solving the problem that the conventional drying agglomeration needs to be crushed again.
The dryer is internally provided with the cyclone separator and the bag-type dust collector, so that the dryer has good dust collection/powder recovery effects, and environmental protection of the process is realized.
The stirring tank is made of PP, PVDF or PTFE materials.
Example 1:
as shown in FIG. 1, in a reaction vessel 1, ion exchange resin powder and an alkali raw material (KOH, Ca (OH)) are sequentially added2) Ethanol solvent, metal ion catalyst (NiSO)4) After long-time stirring and mixing, the resin/alkali/NiSO which is uniformly mixed is formed4And (3) slurry. The slurry enters a closed-loop circulating centrifugal spray dryer 2 (protected by high-purity nitrogen) through a pump and is dried into powder (resin/alkali/NiSO)4Mixture powder), ethanol solvent is recovered.
resin/base/NiSO obtained after drying4The mixture powder enters a rotary furnace 3 for high-temperature reaction through a feeding machine. At high temperature of about 900 deg.C, resin and alkali (KOH, Ca (OH)2) In the presence of catalyst (NiSO)4) To produce three-dimensional graphene (3 DG). The sintered product (mixture of 3 DG/alkali/metal salt, etc.) was discharged from the rotary kiln to a stirring tank 9, and water was added thereto, and stirring was started to dissolve/disperse the sintered product, thereby obtaining a mixed solution. And (3) subjecting the mixed solution to washing by a washing device 4 (ceramic membrane), removing alkali and metal simple substances by acid washing (hydrochloric acid), and then washing by pure water to remove impurity ions (the filtrate requires that the pH is 7 and the conductivity is less than 10us/cm) to obtain the 3DG aqueous slurry. Drying the 3DG slurry into powder (3DG powder) by a dryer 5 (centrifugal spray dryer), removing magnetic substances by a demagnetizer 6, crushing and grading by an airflow crusher 7, and finally packaging by a packaging machine 8 to obtain the final three-dimensional graphene (3 DG).
Example 2:
as shown in FIG. 1, ion exchange resin powder, alkali raw material (KOH), ethanol solvent, and metal ion catalyst (NiCl) are sequentially added into a reaction vessel 12) After long-time stirring and mixing, the resin/alkali/NiCl is formed and mixed evenly2And (3) slurry. The slurry enters a closed-loop circulating centrifugal spray dryer 2 (protected by high-purity nitrogen) through a pump and is dried into powder (resin/alkali/NiCl)2Mixture powder), ethanol solvent is recovered.
resin/base/NiCl obtained after drying2The mixture powder enters a rotary furnace 3 for high-temperature reaction through a feeding machine. At high temperature of about 950 ℃, resin and alkali (KOH) are added in a catalyst (NiCl)2) Is moved downwardsThe reaction was carried out sufficiently to produce three-dimensional graphene (3 DG). The sintered product (mixture of 3 DG/alkali/metal salt, etc.) is discharged from the rotary kiln 3 into a stirring tank, water is added, stirring is started, and dissolution/dispersion is carried out to obtain a mixed solution. And (3) subjecting the mixed solution to acid washing (hydrochloric acid) to remove alkali and metal simple substances by a washing device 4 (a centrifugal machine), and then washing the mixed solution with pure water (the filtrate requires that the pH is 7 and the conductivity is less than 10us/cm) to obtain 3DG aqueous slurry. And drying the 3DG slurry into powder (3DG powder) by a dryer 5 (a boiling dryer), removing magnetic substances by a demagnetizer 6, crushing and grading by an airflow crusher 7, and finally packaging by a packaging machine 8 to obtain the final three-dimensional graphene (3 DG).
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described in the foregoing embodiments, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A three-dimensional graphene industrial production device is characterized by comprising a reaction kettle, a closed-loop circulating centrifugal spray dryer, a rotary furnace, a stirring tank, a washing device, a dryer, a demagnetizer, a jet mill and a packaging machine which are sequentially arranged; the circulating centrifugal spray dryer is provided with an organic solvent recovery device; the washing equipment is one or more of ceramic membrane equipment, a centrifugal machine and a plate-and-frame filter press; the dryer is one or more of a centrifugal spray dryer, a boiling dryer, a fluidized bed dryer, a mesh belt dryer and a vacuum dryer.
2. The industrial production device of three-dimensional graphene according to claim 1, wherein an inert gas injection port is installed in the circulating centrifugal spray dryer.
3. The industrial production device of three-dimensional graphene according to claim 1, wherein the rotary furnace is provided with a furnace chamber main body, and the furnace chamber main body is made of stainless steel materials or ceramic materials.
4. The industrial production device of three-dimensional graphene according to claim 3, wherein the furnace chamber main body is made of 310S stainless steel.
5. The industrial production device of three-dimensional graphene according to claim 1, wherein the washing apparatus is equipped with a pH detector and a conductivity detector.
6. The industrial production device of three-dimensional graphene according to claim 5, wherein a cyclone separator and a bag-type dust collector are arranged in the dryer.
7. The industrial production device of three-dimensional graphene as claimed in claim 6, wherein the stirring tank is made of PP, PVDF or PTFE material.
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| CN202120446007.1U CN214829040U (en) | 2021-03-02 | 2021-03-02 | Three-dimensional graphite alkene industrial production device |
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| CN202120446007.1U CN214829040U (en) | 2021-03-02 | 2021-03-02 | Three-dimensional graphite alkene industrial production device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449346A (en) * | 2022-08-31 | 2022-12-09 | 广东工业大学 | Preparation method and device of ferroferric oxide composite particles for magnetorheological polishing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449346A (en) * | 2022-08-31 | 2022-12-09 | 广东工业大学 | Preparation method and device of ferroferric oxide composite particles for magnetorheological polishing |
| CN115449346B (en) * | 2022-08-31 | 2024-05-24 | 广东工业大学 | Preparation method and device of ferroferric oxide composite particles for magnetorheological polishing |
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