CN116002668A - Batch purification method for carbon nanotubes and energy-saving device thereof - Google Patents
Batch purification method for carbon nanotubes and energy-saving device thereof Download PDFInfo
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- CN116002668A CN116002668A CN202310055698.6A CN202310055698A CN116002668A CN 116002668 A CN116002668 A CN 116002668A CN 202310055698 A CN202310055698 A CN 202310055698A CN 116002668 A CN116002668 A CN 116002668A
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Abstract
The invention discloses a batch purification method of carbon nanotubes and an energy-saving device thereof, relates to the technical field of energy-saving and emission-reducing furnaces, and aims to solve the problems of high energy consumption and high equipment requirement of devices in the existing method. The method comprises the following steps: step one: dividing a crude product of the carbon nano tube prepared by a chemical vapor deposition method into a plurality of batches; carrying out the same oxidation operation on each batch; the oxidant is one of hydrogen peroxide, ozone or hydroxyl free radicals; filtering to obtain a first filter cake; step two: the first filter cake obtained after the step one oxidation of each batch of carbon nano tube crude products is subjected to hydrochloric acid pickling for 5-8 hours; filtering to obtain a second filter cake; step three: the second filter cake obtained after the second acid washing of each batch of the crude carbon nano tube product needs to be washed for a plurality of times, the washing temperature is 80-90 ℃, and the pH value of the washed filtrate is about=5; and drying to obtain the pure carbon nanotube product.
Description
Technical Field
The invention relates to the technical field of energy-saving and emission-reduction reaction furnaces, in particular to a carbon nano tube batch purification method and an energy-saving device thereof.
Background
The furnace is a device for storing, processing and reacting materials in the modern industry, can operate carbon nano tube materials, is a novel carbon-based material with a complete molecular structure, structurally has the advantages of special hollow tubular configuration, good conductivity, high specific surface area, chemical stability, gaps suitable for electrolyte ion migration, nano-sized network structure formed by alternate winding and the like, and therefore, the furnace has wide application in the fields of new energy batteries, energy storage and semiconductors. At present, the preparation process of the carbon nano tube mainly comprises a graphite arc method, a chemical vapor deposition method, a laser evaporation method, an electrolysis method and the like, and the carbon nano tube is produced by the chemical vapor deposition method in industry. Because the transition metal catalyst is used when the carbon nano tube is prepared by the chemical vapor deposition method, the prepared carbon nano tube contains a large amount of metal impurities, such as iron, nickel, cobalt, aluminum and other impurities, and the self-discharge and internal micro-short circuit of the battery can be caused by the high metal content, so that certain potential safety hazard exists. Therefore, there is a need to provide an efficient and convenient purification process to overcome the above problems.
For example, application number "CN110104631B", entitled (purification method of carbon nanotubes and high purity carbon nanotubes), includes: at the treatment temperature of 90-150 ℃, firstly adopting an aqueous solution of industrial nitric acid to carry out first purification, and then carrying out second purification on the purified carbon nano tube by utilizing an aqueous solution of industrial hydrochloric acid, thereby obtaining the purified carbon nano tube. The method mainly adopts oxidative nitric acid for oxidation, the nitric acid can be replaced by sulfuric acid or hydrofluoric acid, and nickel cannot be treated to below 300ppm after purification. And a large amount of cleaning wastewater is generated, and the field operation environment is bad. The amount of clear water reaches 1/150 of the discharge amount.
The device in the method has the problems of high energy consumption and high equipment requirement, so that a simple, efficient and low-energy-consumption device and method for purifying the carbon nanotubes, which are suitable for production, need to be developed.
Disclosure of Invention
The invention aims to provide a batch purification method of carbon nanotubes and an energy-saving device thereof, which are used for solving the problems of high energy consumption and high equipment requirement of the device in the prior method in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: a batch purification method of carbon nanotubes, comprising the steps of:
step one: dividing a crude product of the carbon nano tube prepared by a chemical vapor deposition method into a plurality of batches; carrying out the same oxidation operation on each batch; the oxidant is one of hydrogen peroxide, ozone or hydroxyl free radicals; filtering to obtain a first filter cake;
step two: the first filter cake obtained after the step one oxidation of each batch of carbon nano tube crude products is subjected to hydrochloric acid pickling for 5-8 hours; filtering to obtain a second filter cake;
step three: the second filter cake obtained after the second acid washing of each batch of the crude carbon nano tube product needs to be washed for a plurality of times, the washing temperature is 80-90 ℃, and the pH value of the washed filtrate is about=5; and drying to obtain the pure carbon nanotube product.
Preferably, the concentration of the hydrogen peroxide is 8% -12%.
Preferably, the reaction temperature of the first step is 20-40 ℃, the oxidation reaction time is 5-8h, and the mass ratio of the crude carbon nano tube to the oxidant is 1:10-16.
Preferably, the specific steps of the second step are as follows: the first filter cake obtained in the first step of the crude product of the first batch of carbon nanotubes is subjected to reflux cleaning for a plurality of times by adopting clean dilute hydrochloric acid as a cleaning liquid, and the mass ratio of the first filter cake to the dilute hydrochloric acid is 1:10-16; the concentration of the dilute hydrochloric acid is 15-25%; when the first filter cake obtained in the first step of the crude product of each batch of carbon nanotubes after the first batch is subjected to acid washing, clean dilute hydrochloric acid is used as a cleaning liquid for the last acid washing; the nth acid washing before the last acid washing adopts the filtrate generated by the previous batch of the (n+1) th acid washing as a cleaning liquid.
Preferably, the times of pickling the first filter cake obtained in the first step for each batch of crude carbon nano tube are two times.
Preferably, the specific steps of the third step are as follows: the second filter cake obtained by the second step of the crude product of the first batch of carbon nano tubes is back-washed for a plurality of times by adopting clear water as a cleaning liquid, and when the second filter cake obtained by the second step of the crude product of each batch of carbon nano tubes after the first batch is water-washed, the clear water is used as the cleaning liquid for the last water washing; the M-th water washing before the last time adopts the filtrate generated by the M+1st water washing of the previous batch as the cleaning liquid.
Preferably, the number of times of washing the crude product of each batch of carbon nanotubes by the second filter cake generated in the second step is three.
Preferably, the batch purification energy-saving device for the carbon nanotubes is characterized by comprising an oxidation furnace, a first acidification furnace, a second acidification furnace, a first cleaning furnace, a second cleaning furnace and a third cleaning furnace, wherein one side of the oxidation furnace is provided with first filter pressing equipment, one side of the first acidification furnace is provided with second filter pressing equipment, one side of the second acidification furnace is provided with third filter pressing equipment, one side of the first cleaning furnace is provided with fourth filter pressing equipment, one side of the second cleaning furnace is provided with fifth filter pressing equipment, one side of the third cleaning furnace is provided with sixth filter pressing equipment, one side of the upper end face of the oxidation furnace is provided with a hydrogen peroxide filter pressing pipeline, the other side of the upper end face of the oxidation furnace is provided with a crude product conveying pipeline for the carbon nanotubes, the upper end face of the second acidification furnace is provided with a hydrochloric acid conveying pipeline, and the upper end face of the pure water conveying pipeline is provided with a pure water conveying pipeline.
Preferably, one side of the first filter pressing equipment is provided with a waste water pipeline, the other side of the first filter pressing equipment is connected with an oxidation furnace pipeline, the first filter pressing equipment is connected with a first acidification furnace pipeline, one side of the second filter pressing equipment is provided with a waste acid pipeline, the third filter pressing equipment is connected with the first acidification furnace pipeline through a first return pipeline, the third filter pressing equipment is connected with a second acidification furnace and a first cleaning furnace through pipelines, one side of the first cleaning furnace is provided with a cleaning water pipeline, the fifth filter pressing equipment is connected with the first cleaning furnace pipeline through a second return pipeline, the upper end face of the sixth filter pressing equipment is provided with a pure product conveying pipeline, and the sixth filter pressing equipment is connected with the second cleaning furnace pipeline through a third return pipeline.
Compared with the prior art, the invention has the beneficial effects that:
1. the oxidation temperature is lower when the batch purification method of the carbon nano tube is adopted, and the conventional oxidation process needs to be carried out at 85-100 ℃; the oxidation temperature of the invention is between 20 and 40 ℃, and the energy consumption is lower.
2. In the traditional process, nitric acid or other oxidizing substances are used for oxidizing the carbon tube; wherein the residual other types of acidic oxides in the carbon nanotubes are mixed with hydrochloric acid in the subsequent acidification process in the post-treatment, so that sodium nitrate/sodium chloride or mixed salts of other sodium salts and sodium chloride are generated; can only be used as solid waste or general hazardous waste for treatment; the hydrogen peroxide, ozone or hydroxyl radical adopted in the process exists in the form of water or oxygen after oxidation, so that mixed salt is not generated, and only sodium chloride salt is used.
3. In the prior art, nitric acid, hydrofluoric acid and the like are adopted as oxidizing agents, the requirements on the materials of the equipment and the pipelines are high, PVDF special materials are required to be used as inner liners of the equipment, and the processing difficulty is high; after the purification method of the invention is adopted, the conventional stainless steel or plastic material is adopted
4. The batch purification method of the carbon nano tube has good purification effect and higher removal rate of the indexes such as iron, cobalt and the like in the crude product of the carbon nano tube.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a flow chart showing the operation of the reaction in example 1 of the present invention;
FIG. 3 is a flow chart showing the operation of the reaction in example 2 of the present invention;
FIG. 4 is a flow chart showing the operation of the reaction in example 3 of the present invention;
in the figure: 1. an oxidation furnace; 101. a first filter press device; 102. a waste water pipe; 103. a hydrogen peroxide delivery pipe; 104. a carbon nano tube crude product conveying pipeline; 2. a first acidification furnace; 201. a second filter pressing device; 202. a waste acid pipeline; 3. a second acidification furnace; 301. a third filter pressing device; 302. a first return conduit; 303. hydrochloric acid conveying pipeline; 4. a first cleaning furnace; 401. a fourth filter pressing device; 402. cleaning a water pipeline; 5. a second cleaning furnace; 501. a fifth filter pressing device; 502. a second return conduit; 6. a third cleaning furnace; 601. a sixth filter pressing device; 602. a pure product conveying pipeline; 603. a third return conduit; 604. pure water delivery pipe.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Example 1:
referring to fig. 1-4, an embodiment of the present invention is provided: a batch purification method of carbon nanotubes, comprising the steps of:
step one: oxidizing hydrogen peroxide; weighing 0.5kg of crude carbon nano tube, adding 8kg of 10% hydrogen peroxide into a glass reaction kettle, reacting for 6 hours at 20-40 ℃, and pressing into cakes through a high-pressure plate frame for later use;
step two: acid washing; placing the filter cake obtained by oxidation back to a reaction kettle, adding 20% clean hydrochloric acid for reflux pickling for 6 hours, pickling twice, wherein the consumption of the hydrochloric acid is 8kg each time, and pressing and filtering the filter cake into a filter cake through a high-pressure plate frame for later use; the filtrate subjected to the first acid washing enters waste liquid treatment, and the filtrate subjected to the second acid washing is collected and then is used for the next batch;
step three: washing with water; washing with clear water for three times at 85deg.C for 15min; washing until the pH is about 5; press-filtering to form cakes, drying and crushing the filter cakes to obtain a pure carbon nanotube product; the filtrate of the first water washing enters into the wastewater treatment, and the filtrate of the second water washing and the filtrate of the third water washing are collected separately and then are used for the next batch.
Example 2:
a batch purification method of carbon nanotubes, comprising the steps of:
step one: performing ozone oxidation; weighing 0.5kg of carbon nano tube crude product, putting the crude product into a gas-liquid mixing reaction kettle, adding 8kg of pure water, introducing ozone at 20-40 ℃ for reaction for 6 hours, and performing filter pressing through a high-pressure plate frame to form cakes for later use;
step two: acid washing; placing the filter cake obtained by oxidation back to a reaction kettle, adding 20% clean hydrochloric acid for reflux pickling for 6 hours, pickling twice, wherein the consumption of the hydrochloric acid is 8kg each time, and pressing and filtering the filter cake into a filter cake through a high-pressure plate frame for later use;
step three: washing with water; washing with clear water for three times; the washing temperature is 85 ℃ and the washing time is 15min; washing until the pH value is about 5, press-filtering to form cakes, drying the filter cakes, and crushing to obtain the pure carbon nano tube product.
Example 3:
a batch purification method of carbon nanotubes, comprising the steps of:
step one: oxidizing hydroxyl radicals; weighing 0.5Kg of crude carbon nano tube, adding 8Kg of pure water into a hydroxyl radical generator (electro Fenton device), starting radical generating equipment to react for 6 hours, and performing filter pressing through a high-pressure plate frame to form cakes for later use;
step two: acid washing; placing the filter cake obtained by oxidation back to a reaction kettle, adding 20% clean hydrochloric acid for reflux pickling for 6 hours, pickling twice, wherein the consumption of the hydrochloric acid is 8kg each time, and pressing and filtering the filter cake into a filter cake through a high-pressure plate frame for later use;
step three: washing with water; washing with clear water for three times; the washing temperature is 85 ℃ and the washing time is 15min; washing until the pH value is about 5, press-filtering to form cakes, drying the filter cakes, and crushing to obtain the pure carbon nano tube product.
The concentration of the hydrogen peroxide is 8% -12%, the reaction temperature of the first step is 20-40 ℃, the oxidation reaction time is 5-8h, the mass ratio of the crude carbon nano tube to the oxidant is 1:10-16, and the specific steps of the second step are as follows: the first filter cake obtained in the first step of the crude product of the first batch of carbon nanotubes is subjected to reflux cleaning for a plurality of times by adopting clean dilute hydrochloric acid as a cleaning liquid, and the mass ratio of the first filter cake to the dilute hydrochloric acid is 1:10-16; the concentration of the dilute hydrochloric acid is 15-25%; when the first filter cake obtained in the first step of the crude product of each batch of carbon nanotubes after the first batch is subjected to acid washing, clean dilute hydrochloric acid is used as a cleaning liquid for the last acid washing; the Nth pickling before the last pickling adopts the filtrate generated by the previous batch of (n+1) th pickling as a cleaning liquid, the times of pickling the first filter cake obtained by the step one of each batch of crude carbon nano tube product are two times, and the specific steps of the step three are as follows: the second filter cake obtained by the second step of the crude product of the first batch of carbon nano tubes is back-washed for a plurality of times by adopting clear water as a cleaning liquid, and when the second filter cake obtained by the second step of the crude product of each batch of carbon nano tubes after the first batch is water-washed, the clear water is used as the cleaning liquid for the last water washing; the M-th washing before the last time adopts filtrate generated by the previous M+1st washing as a cleaning solution, and the times of washing each batch of crude carbon nano tube products by the second filter cake generated in the second step are all three times.
Referring to fig. 1, a batch purification energy-saving device for carbon nanotubes is characterized by comprising an oxidation furnace 1, a first acidification furnace 2, a second acidification furnace 3, a first cleaning furnace 4, a second cleaning furnace 5 and a third cleaning furnace 6, wherein one side of the oxidation furnace 1 is provided with a first filter pressing device 101, one side of the first acidification furnace 2 is provided with a second filter pressing device 201, one side of the second acidification furnace 3 is provided with a third filter pressing device 301, one side of the first cleaning furnace 4 is provided with a fourth filter pressing device 401, one side of the second cleaning furnace 5 is provided with a fifth filter pressing device 501, one side of the third cleaning furnace 6 is provided with a sixth filter pressing device 601, one side of the upper end face of the oxidation furnace 1 is provided with a hydrogen peroxide conveying pipeline 103, the other side of the upper end face of the oxidation furnace 1 is provided with a carbon nanotube crude product conveying pipeline 104, the upper end face of the second acidification furnace 3 is provided with a hydrochloric acid conveying pipeline 303, and the upper end face of the pure water conveying pipeline 604 is provided with a pure water conveying pipeline 604.
Referring to fig. 1, a waste water pipe 102 is disposed on one side of a first filter pressing device 101, the other side of the first filter pressing device 101 is connected with an oxidation furnace 1 through a pipe, the first filter pressing device 101 is connected with a first acidification furnace 2 through a pipe, a waste acid pipe 202 is disposed on one side of a second filter pressing device 201, a third filter pressing device 301 is connected with the first acidification furnace 2 through a first return pipe 302, the third filter pressing device 301 is connected with a second acidification furnace 3 and a first cleaning furnace 4 through a pipe, a cleaning water pipe 402 is disposed on one side of the first cleaning furnace 4, a fifth filter pressing device 501 is connected with the first cleaning furnace 4 through a second return pipe 502 through a pipe, a pure product conveying pipe 602 is disposed on the upper end face of a sixth filter pressing device 601, and the sixth filter pressing device 601 is connected with the second cleaning furnace 5 through a third return pipe 603.
In the embodiments provided in the present application, it should be understood that the disclosed apparatus and method may be implemented in other manners. The above-described apparatus embodiments are merely illustrative, for example, the division of the units is merely a logical function division, and there may be other manners of division in actual implementation, and for example, multiple units or components may be combined or integrated into another system, or some features may be omitted, or not performed. Alternatively, the coupling or direct coupling or communication connection shown or discussed with each other may be through some communication interface, device or unit indirect coupling or communication connection, which may be in electrical, mechanical or other form.
Finally, it should be noted that: the above examples are only specific embodiments of the present invention, and are not intended to limit the scope of the present invention, but it should be understood by those skilled in the art that the present invention is not limited thereto, and that the present invention is described in detail with reference to the foregoing examples: any person skilled in the art may modify or easily conceive of the technical solution described in the foregoing embodiments, or perform equivalent substitution of some of the technical features, while remaining within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (9)
1. A batch purification method of carbon nanotubes, comprising the steps of:
step one: dividing a crude product of the carbon nano tube prepared by a chemical vapor deposition method into a plurality of batches; carrying out the same oxidation operation on each batch; the oxidant is one of hydrogen peroxide, ozone or hydroxyl free radicals; filtering to obtain a first filter cake;
step two: the first filter cake obtained after the step one oxidation of each batch of carbon nano tube crude products is subjected to hydrochloric acid pickling for 5-8 hours; filtering to obtain a second filter cake;
step three: the second filter cake obtained after the second acid washing of each batch of the crude carbon nano tube product needs to be washed for a plurality of times, the washing temperature is 80-90 ℃, and the pH value of the washed filtrate is about=5; and drying to obtain the pure carbon nanotube product.
2. The method for batch purification of carbon nanotubes of claim 1, wherein: the concentration of the hydrogen peroxide is 8% -12%.
3. The method for batch purification of carbon nanotubes of claim 1, wherein: the reaction temperature of the first step is 20-40 ℃, the oxidation reaction time is 5-8h, and the mass ratio of the crude carbon nano tube to the oxidant is 1:10-16.
4. A method for batch purification of carbon nanotubes as claimed in claim 3, wherein: the specific steps of the second step are as follows: the first filter cake obtained in the first step of the crude product of the first batch of carbon nanotubes is subjected to reflux cleaning for a plurality of times by adopting clean dilute hydrochloric acid as a cleaning liquid, and the mass ratio of the first filter cake to the dilute hydrochloric acid is 1:10-16; the concentration of the dilute hydrochloric acid is 15-25%; when the first filter cake obtained in the first step of the crude product of each batch of carbon nanotubes after the first batch is subjected to acid washing, clean dilute hydrochloric acid is used as a cleaning liquid for the last acid washing; the nth acid washing before the last acid washing adopts the filtrate generated by the previous batch of the (n+1) th acid washing as a cleaning liquid.
5. The method for batch purification of carbon nanotubes of claim 4, wherein: and (3) carrying out acid washing on the first filter cake obtained in the first step on each batch of crude carbon nano tube product twice.
6. The method for batch purification of carbon nanotubes of claim 4, wherein: the specific steps of the third step are as follows: the second filter cake obtained by the second step of the crude product of the first batch of carbon nano tubes is back-washed for a plurality of times by adopting clear water as a cleaning liquid, and when the second filter cake obtained by the second step of the crude product of each batch of carbon nano tubes after the first batch is water-washed, the clear water is used as the cleaning liquid for the last water washing; the M-th water washing before the last time adopts the filtrate generated by the M+1st water washing of the previous batch as the cleaning liquid.
7. The method for batch purification of carbon nanotubes of claim 6, wherein: and (3) washing the crude carbon nano tube products of each batch with water for three times through the second filter cake generated in the second step.
8. The utility model provides a batched purification economizer of carbon nanotube, its characterized in that, including oxidation furnace (1), first acidizing stove (2), second acidizing stove (3), first washery (4), second washery (5) and third washery (6), oxidation furnace (1) one side is provided with first filter-pressing equipment (101), one side of first acidizing stove (2) is provided with second filter-pressing equipment (201), one side of second acidizing stove (3) is provided with third filter-pressing equipment (301), one side of first washery (4) is provided with fourth filter-pressing equipment (401), one side of second washery (5) is provided with fifth filter-pressing equipment (501), one side of third washery (6) is provided with sixth filter-pressing equipment (601), one side of oxidation furnace (1) up end is provided with pipeline (103), the opposite side of oxidation furnace (1) up end is provided with carbon nanotube crude conveying pipeline (104), one side of second acidizing stove (3) is provided with fourth filter-pressing equipment (604), one side of second acidizing stove (4) is provided with pure water (604), one side (604) is provided with pure water (604).
9. The energy-saving device for batch purification of carbon nanotubes of claim 8, wherein: one side of first filter-pressing equipment (101) is provided with waste water pipeline (102), first filter-pressing equipment (101) opposite side and oxidation stove (1) pipe connection, first filter-pressing equipment (101) and first acidizing stove (2) pipe connection, one side of second filter-pressing equipment (201) is provided with waste acid pipeline (202), pass through first returning pipeline (302) and first acidizing stove (2) pipe connection of third filter-pressing equipment (301), third filter-pressing equipment (301) all pass through pipe connection with second acidizing stove (3) and first washing stove (4), one side of first washing stove (4) is provided with washing water pipeline (402), fifth filter-pressing equipment (501) pass through second returning pipeline (502) and first washing stove (4) pipe connection, the up end of sixth filter-pressing equipment (601) is provided with pure product conveying pipeline (602), sixth filter-pressing equipment (601) pass through third pipeline (603) and second washing stove (5) pipe connection.
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2023
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| JP2003089510A (en) * | 2001-09-11 | 2003-03-28 | Denso Corp | Method for refining carbon nanotube |
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