CN114405827A - Wind power separation method for separating carbon materials in molten salt - Google Patents
Wind power separation method for separating carbon materials in molten salt Download PDFInfo
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- CN114405827A CN114405827A CN202210100091.0A CN202210100091A CN114405827A CN 114405827 A CN114405827 A CN 114405827A CN 202210100091 A CN202210100091 A CN 202210100091A CN 114405827 A CN114405827 A CN 114405827A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B9/00—Combinations of apparatus for screening or sifting or for separating solids from solids using gas currents; General arrangement of plant, e.g. flow sheets
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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
- B02C21/00—Disintegrating plant with or without drying of the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/08—Separating or sorting of material, associated with crushing or disintegrating
- B02C23/10—Separating or sorting of material, associated with crushing or disintegrating with separator arranged in discharge path of crushing or disintegrating zone
- B02C23/12—Separating or sorting of material, associated with crushing or disintegrating with separator arranged in discharge path of crushing or disintegrating zone with return of oversize material to crushing or disintegrating zone
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B11/00—Arrangement of accessories in apparatus for separating solids from solids using gas currents
- B07B11/02—Arrangement of air or material conditioning accessories
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B4/00—Separating solids from solids by subjecting their mixture to gas currents
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- Combined Means For Separation Of Solids (AREA)
Abstract
The invention provides a wind power separation method for separating carbon materials in molten salt, and belongs to the technical field of separation of carbon materials in a molten salt carbon preparation process. The method for sorting the mixed product of the fused salt and the carbon needs to be carried out by the following 5 steps: (1) and putting the salt-carbon mixed product into a crusher for crushing and powdering. (2) The crushed and powdered salt-carbon mixture is ground in a ball mill. (3) The milled salt-carbon mixture was placed on a porous sieve for sieving. (4) And placing the screened salt-carbon mixture on a wind power sorting platform to perform wind power sorting by adopting a certain wind speed and a certain sample platform height. (5) The carbon salt products in the two settling zones are collected respectively. The invention of the sorting method is that the sorting is carried out by different densities of the molten salt and the carbon material particles, and the carbon product with the carbon content of more than 93 percent and the salt content of less than 7 percent can be obtained in the carbon particle settling zone, which is important for promoting the recovery of the molten salt and improving the economic benefit of the molten salt carbon preparation process.
Description
Technical Field
The invention belongs to the technical field of separation of carbon materials and molten salts in a process of preparing carbon by electrolyzing molten salts, and particularly relates to a wind power separation method for separating a salt-carbon mixture.
Background
Since the beginning of the industrial revolution, with the rapid development of global economy, atmospheric carbon dioxide (CO)2) The concentration of (A) is increased from 270ppm at the beginning of the 20 th century to 400ppm at present, which can cause global warming and disastrous weather, and further influence human survival. In order to meet the challenge of the global climate problem, on one hand, a green emission reduction technology with low carbon, energy conservation, environmental protection and sustainable resource utilization needs to be developed; on the other hand, a certain method is needed to capture CO in the atmosphere2And is fixed and converted into a carbon material. Molten salt CO researched and developed by this subject group in recent years2The trapping and electrochemical conversion technology realizes the CO in the atmosphere2On the other hand, high value-added utilization of the converted carbon material is realized. The subject group has gradually scaled the technology from laboratory class A to Bai 'an and Qian' an. In the process of the stepwise amplification of the technology, as the technology is gradually amplified, new problems arise: the cathode product contains solidified electrolyte molten salt (95 wt.% to 97 wt.%) in a high proportion and a certain proportion of carbon material, so that the problem of separation of the carbon material from the molten salt needs to be solved urgently in order to efficiently and economically utilize the carbon material in the molten salt.
Molten salt CO capture2And various carbon materials (activated carbon, graphite carbon sheets, carbon nanotubes, carbon fibers and carbon microspheres) with high added values are prepared by an electrochemical conversion technology, and in the aspect of separation of the carbon materials and molten salt, a conventional method in a laboratory is to soak, wash to neutrality, filter and dry by a large amount of concentrated hydrochloric acid and pure water. Through calculation, in order to obtain 1kg of high-added-value carbon material, the amount of concentrated hydrochloric acid consumed by the traditional method is 34L, and the amount of pure water consumed for washing to be neutral is 2-4 m3Most importantly, this part of the accompanying molten salt is completely converted to chloride salt by reaction with concentrated hydrochloric acid, and cannot be achievedRecycling of the molten salt, which undoubtedly increases the process costs of the technique.
Disclosure of Invention
In order to solve the problems of environmental pollution and resource waste caused by the separation of the carbon material from the molten salt by the traditional method, the invention provides a method for separating the carbon material and the molten salt by utilizing different densities and particle shapes, and the core mechanism of the method is as follows: under high temperature conditions, the solid carbon is uniformly attached to the surface of the carbon particles due to the wetting effect of the liquid electrolyte on the solid carbon. The carbon material prepared by electrolysis in molten salt and the interface of two phases of electrolyte are only the interaction of Van der Waals force, under the mechanical crushing and ball milling, the Van der Waals force between the two phases of the carbon particles and the salt particles can be broken when the carbon particles and the salt particles are pulverized to a certain particle size due to different flexibility and hardness, and the carbon particles and the salt particles are settled to different areas under the action of wind power to realize the salt-carbon separation.
In order to realize the pneumatic separation method for separating the carbon material from the molten salt, the specific embodiment is as follows:
an air separation method for separating carbon materials in molten salt,
(1) and putting the salt-carbon mixed product into a sealed pulverizer, and crushing and pulverizing under the protection of inert gas atmosphere.
(2) The crushed and powdered salt-carbon mixture is put into a sealed ball mill and ground under the protection of inert gas atmosphere.
(3) The milled salt-carbon mixture was placed in a sieve through a porous sieve.
(4) And placing the salt-carbon mixture subjected to screening on a constant-temperature dry wind power separation platform, and performing wind power separation by adopting a certain wind speed and a certain sample platform height.
(5) And respectively collecting the salt and the carbon products.
Further, the salt in the step (1) is in a solidified state of a molten salt electrolyte in the process of preparing carbon by electrochemical conversion, and mainly relates to Li2CO3、Li2CO3-Na2CO3、Li2CO3-K2CO3、Li2CO3-Na2CO3-K2CO3、Li2CO3-Na2CO3-K2CO3-Li2SO4、Li2O-LiCl-KCl、LiCl-KCl-CaCO3And CaO-LiCl-KCl.
Further, the grinding chamber and the ball milling tank used in the steps (1) and (2) need to be designed in a sealing way, materials in the chamber and the tank do not contact with the outside air in the ball milling and screening processes, and the charged high-purity inert gas comprises: argon gas and nitrogen gas.
Furthermore, the mesh number of the porous sieve in the step (3) is 200 meshes, and for large particles which do not pass through the mesh of the porous sieve, the steps (1) and (2) need to be adopted again to continue crushing, pulverizing and ball milling.
Further, the wind speed of the wind power sorting platform in the step (4) is generally set to be 1-25 m.s-1。
Further, the height of the sample platform of the wind power separation platform in the step (4) is generally set to be 0.5-1.5 m away from the settlement plane.
Further, the length of the settling zone of the pneumatic separation platform in the step (4) is set to be 1-10 m.
Further, the constant-temperature drying wind power sorting platform in the step (4) comprises a sample feeding table, a liftable sample table, a temperature adjusting device, a drying device, a temperature and humidity sensor, a fan and a controller, wherein the temperature and humidity sensor transmits temperature information and humidity information to the controller, the controller controls the temperature adjusting device and the drying device to operate, the controller can control the fan to adjust wind speed, and a funnel-shaped sample inlet is formed in the sample feeding table.
Furthermore, an air inlet channel is formed between the sample feeding table and the sample table, and the fan is connected to an inlet of the air inlet channel.
Furthermore, the air inlet channel comprises a horizontal section and an upper inclined section, the upper inclined section is inclined upwards by 5-15 degrees, and the sample inlet is positioned above the horizontal section. Since the molten salt with higher density is more difficult to move upwards by wind power than to move horizontally by wind power, the upward inclination of the injection port is more beneficial to the separation of the molten salt with higher density and the carbon material with lower density. The inclination angle of 5-15 degrees can not only ensure that the air inlet channel keeps a certain inclination, but also avoid the phenomenon that the inclination is too large, and part of carbon materials are blocked and cannot be smoothly blown out.
Further, the air classification method can obtain carbon products with the carbon content of 93 wt.% to 99.5 wt.% and the salt content of less than 1.0 wt.% to 7.0 wt.% in the carbon particle settling zone.
The invention has the beneficial effects that: the wind power sorting method can greatly reduce or even eliminate the use of concentrated hydrochloric acid, pure water and the like; the inert gas atmosphere is adopted, so that the carbon material can be prevented from contacting with oxygen, and the safety is ensured; the constant-temperature drying wind power separation platform can avoid the melting of molten salt and the bonding of carbon materials in a humid environment.
Drawings
FIG. 1 is a salt-carbon mixture collected at the cathode in the example, the left figure is a carbon nanoparticle and salt mixture, and the right figure is a carbon sheet and salt mixture;
FIG. 2 is a flow diagram of an air classification process;
FIG. 3 is a schematic diagram of a laboratory wind sorting platform.
In the figure, 1, a settling zone, 2, a sample inlet, 3, a fan, 4 and a sample table.
Detailed Description
To more clearly illustrate the technical advantages of the air classification method in salt-carbon separation, the following description is given by way of specific examples, which are intended to be illustrative only and not limiting.
Example 1
All the salt-carbon mixtures used in the examples and comparative examples were electrolytically converted using a kilo-ampere electrolytic cell under the specific conditions: the temperature is 500 ℃, and the current density is 50mA cm-2The anode adopts an inert oxygen evolution anode, and the cathode adopts a high-purity nickel plate.
At 500 deg.C, the current density is 50mA cm-2，Li2CO3-Na2CO3-K2CO3The cathode salt-carbon mixture product electrolyzed in molten salt for 12h was collected and analyzed for initial salt to carbon ratio. Of carbonThe mass proportion was 3 wt.%, and the salt proportion was 97 wt.%. Placing the collected salt-carbon mixture into a high-speed crusher, crushing for 2min under the atmosphere of high-purity argon, then placing the crushed salt-carbon mixture into a ball milling tank filled with the high-purity argon, wherein the mass ratio of the crushed salt-carbon mixture to zirconia balls is 1:100, carrying out ball milling for 12h, placing the superfine salt-carbon mixture obtained by ball milling into a 200-mesh porous sieve for screening, collecting the salt-carbon mixture capable of passing through the 200-mesh porous sieve, and continuously crushing and ball milling large particles which do not pass through the porous sieve according to the conditions. Accurately weighing 5.0g of the sieved salt-carbon mixture, placing the salt-carbon mixture on a sample table of a wind power separation platform, and setting the working conditions of the platform to be room temperature and 10 m.s.-1The height of the sample table is 1.0m, the equipment is started, and 5.0g of sample is measured in 1 g.s-1And (4) the sampling speed is controlled, the fan is automatically stopped after the operation is carried out for 5s, and the waiting settling time is 20 min. And after the sedimentation is finished, observing and collecting the distribution condition of the salt and the carbon in the sedimentation area. The research shows that the length of the settling zone is 6.90m, a salt-carbon boundary line is obvious at the position of 1.3m, the mass content of salt in the salt zone is 99.0 percent, the carbon content in the carbon zone is 82.4 percent, the total mass of the sample collected in the carbon zone is 0.18g, and the separation effect is obvious.
Example 2
The salt-carbon mixture was prepared and the pulverizing and ball-milling steps were the same as in example 1 except that the air speed was set to 1 m.s-1. The study showed that the wind speed was set to 1 m.s-1In the case of (2), the length of the settling zone was 3.72m, the boundary between the salt zone and the carbon zone was about 0.90m, the total mass of the sample collected in the carbon zone was 0.30g, and the mass ratio of carbon was 40.0%.
Example 3
The salt-carbon mixture was prepared and the pulverizing and ball-milling steps were the same as in example 1 except that the air speed was set to 5 m.s-1. The study showed that at a wind speed of 25 m.s-1In the case of (2), the length of the settling zone was 8.72m, the boundary between the salt zone and the carbon zone was 3.17m, the total mass of the collected samples in the carbon zone was 0.16g, and the mass ratio of carbon was 95.2%.
Example 4
Preparation of salt-carbon mixture and the crushing and ball milling steps were the same as in example 1, except thatThe wind speed was set to 25 m.s during the wind sorting process-1The heights of the sample stages were set to 0.5m, respectively. It was found that under these conditions, the length of the settling zone was 5.24m, the boundary between the salt and carbon zones was about 2.16m, the total mass of the sample collected in the carbon zone was 0.20g, and the mass fraction of carbon was 76.4%.
Example 5
The salt-carbon mixture was prepared and pulverized and ball-milled in the same manner as in example 1 except that the air speed was set to 25 m.s in the air classification process-1The height of the sample stage was set to 1.5 m. It was found that under these conditions the length of the settling zone was 9.99m, the boundary between the salt and carbon zones was about 3.54m, the total mass of the sample collected in the carbon zone was 0.15g, and the mass fraction of carbon was 96.9%.
Example 6
The salt-carbon mixture preparation conditions, crushing and ball milling steps were the same as in example 1, except that the molten salt used was CaCO3-LiCl-KCl, the initial salt mass ratios determined to be 95.8% respectively. The air sorting process was the same as in example 1, except that the wind speed was set to 25m · s-1And observing and collecting the distribution of the salt and the carbon in the settling zone. Research shows that CaCO3The length of the settling zone of the LiCl-KCl molten salt is 8.40m, the boundary between the salt zone and the carbon zone is about 3.04m, the mass of the carbon zone is 0.26g, and the mass proportion of carbon is 98.05%.
Claims (10)
1. An air separation method for separating carbon materials in molten salt is characterized by comprising the following steps:
(1) putting the salt-carbon mixed product into a closed pulverizer, and crushing and pulverizing under the protection of inert gas atmosphere;
(2) placing the crushed and powdered salt-carbon mixture into a closed ball mill for levigating, and adopting inert gas atmosphere protection in the ball mill chamber;
(3) sieving the milled salt-carbon mixture through a porous sieve;
(4) placing the salt-carbon mixture passing through the porous sieve on a constant-temperature dry air sorting platform, performing air sorting by adopting constant air speed and sample platform height, and repeating the steps (1), (2) and (3) on the large-particle salt-carbon mixture not passing through the porous sieve;
(5) and (4) carrying out partition collection on the salt carbon product in the settling zone.
2. An air classification method for carbon material separation in molten salt according to claim 1, characterized in that the salt in step (1) is Li2CO3、Na2CO3、K2CO3、Li2SO4、Li2O、LiCl、KCl、CaCO3And CaO in a mixed form.
3. The pneumatic separation method for separating carbon materials in molten salt according to claim 1, wherein the inert gas in step (1) (2) is any one of argon and nitrogen.
4. An air classification method for carbon material separation in molten salt according to claim 1, characterized in that the mesh number of the porous screen in step (3) is 200 meshes.
5. The pneumatic separation method for separating carbon materials in molten salt according to claim 1, wherein the humidity of the constant-temperature drying pneumatic separation platform in the step (4) is lower than 0.1%.
6. An air classification method for carbon material separation in molten salt according to claim 1, characterized in that the constant wind speed in step (4) is 1-25 m-s-1。
7. The wind power separation method for separating carbon materials in molten salt according to claim 1, wherein the constant-temperature drying wind power separation platform in the step (4) comprises a sample feeding table, a liftable sample table, a temperature adjusting device, a drying device, a temperature and humidity sensor, a fan and a controller, the temperature and humidity sensor transmits temperature information and humidity information to the controller, the controller controls the temperature adjusting device and the drying device to operate, the controller can control the fan to adjust the wind speed, and a funnel-shaped sample inlet is formed in the sample feeding table.
8. The wind power separation method for separating the carbon materials in the molten salt according to claim 7, wherein an air inlet channel is formed between the sample feeding table and the sample table, and a fan is connected to an inlet of the air inlet channel.
9. The wind power separation method for separating the carbon materials in the molten salt according to claim 1, wherein the height of the sample platform of the wind power separation platform in the step (4) is 0.1-1.5 m.
10. The wind power separation method for separating the carbon materials in the molten salt according to claim 1, wherein the length of a settling zone of the wind power separation platform is 1-10 m.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024083786A1 (en) | 2022-10-21 | 2024-04-25 | Shell Internationale Research Maatschappij B.V. | Apparatus for separating a solids-containing and molten salt containing stream |
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| CN201774951U (en) * | 2010-08-06 | 2011-03-30 | 福建中烟工业公司 | Automatic air quantity and humidity control device of winnowing and air conveying appliance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2024083786A1 (en) | 2022-10-21 | 2024-04-25 | Shell Internationale Research Maatschappij B.V. | Apparatus for separating a solids-containing and molten salt containing stream |
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