CN110482550B - Device and method for self-activating and recycling porous carbon from waste electrode slurry of super capacitor - Google Patents
Device and method for self-activating and recycling porous carbon from waste electrode slurry of super capacitor Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/36—Reactivation or regeneration
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
Abstract
The invention relates to a device and a method for self-activating and recycling porous carbon from waste electrode slurry of a super capacitor. The method for recovering the porous carbon comprises the following steps: opening a waste material inlet valve, placing the waste electrode slurry in a horizontal reaction furnace, and closing the waste material inlet valve; opening an air inlet valve and an air outlet valve, introducing inert gas, and then closing the air inlet valve and the air outlet valve; turning on a traction motor to drive a stirring paddle to stir, then heating the horizontal reaction furnace to 120 ℃ for heat preservation for 1-3h, heating to 900 ℃ for heat preservation for 1-3h, and then stopping heating; opening an air inlet valve and an air outlet valve, introducing inert gas, and then closing the air inlet valve and the air outlet valve to naturally cool the horizontal reaction furnace to room temperature; opening a water inlet valve, a discharge valve and a discharge water pump, collecting materials, and closing the water inlet valve, the discharge valve and the discharge water pump after the solution has no black solid; and filtering the collected materials to obtain solid black porous carbon powder.
Description
Technical Field
The invention relates to the technical field of super capacitors, in particular to a device and a method for self-activating and recycling porous carbon from waste electrode slurry of a super capacitor.
Background
The super capacitor is widely applied by the advantages of super high power, super long service life, super wide high and low temperature characteristics and the like. The electrode of the super capacitor is formed by physically dispersing porous carbon, a binder and water into electrode slurry and uniformly coating the electrode slurry on an aluminum foil, but the electrode slurry is easy to remain in a stirring kettle and a conveying pipeline to form waste electrode slurry. At present, the treatment method of the waste electrode slurry mainly utilizes a sedimentation tank to extract precipitates (porous carbon and a binder) in the slurry, and the porous carbon is agglomerated under the action of the binder, and the specific surface area is reduced by 30%, so that the precipitates need to be treated by a burying or burning method, certain influence is caused on the environment, and the waste of electrode materials is caused.
Chinese patent publication No. 106207267a discloses a system and a method for recycling waste lithium ion battery positive electrode slurry, which relate to a method for recycling waste slurry, but are directed to recycling and storing of lithium ion battery positive electrode materials, and are not suitable for recycling of electrode materials of supercapacitors.
Disclosure of Invention
The invention provides a recycling method of the waste electrode slurry of the super capacitor, which is simple in recycling process and good in recycling material performance, aiming at the problems of recycling of the electrode slurry of the super capacitor in the prior art.
One purpose of the invention is realized by the following technical scheme: an apparatus for self-activating recovery of porous carbon from supercapacitor waste electrode slurry, the apparatus comprising:
the horizontal reaction furnace, the stirring paddle, blades on the stirring paddle, a traction motor, a heating sleeve, a flange, a plurality of air inlet valves, a plurality of feeding valves, a plurality of air outlet valves, a plurality of discharging valves and a discharging water pump.
Further preferably, the device comprises 1 intake valve; 1 discharge valve; 2 air outlet valves, wherein each air outlet valve comprises an air outlet valve 1 and an air outlet valve 2; 2 feeding valves, feeding valve includes the water inlet valve and advances the waste material valve.
The other purpose of the invention is realized by the following technical scheme: a method for self-activating and recovering porous carbon from waste electrode slurry of a super capacitor by using the device comprises the following steps:
(1) opening a waste material inlet valve, placing the waste electrode slurry in a horizontal reaction furnace, and then closing the waste material inlet valve;
(2) opening the air inlet valve and the air outlet valve 2, introducing inert gas for 10-20min, and then closing the air inlet valve and the air outlet valve 2;
(3) turning on a traction motor, driving a stirring paddle to rotate and stir for 0.5-1h, heating the horizontal reaction furnace to 120 ℃ and preserving heat for 1-3h, then heating the horizontal reaction furnace to 900 ℃ and preserving heat for 1-3h, and then stopping heating;
(4) opening an air inlet valve, an air outlet valve 1 and an air outlet valve 2, introducing inert gas for 10-20min, and then closing the air inlet valve, the air outlet valve 1 and the air outlet valve 2 to naturally cool the horizontal reaction furnace to room temperature;
(5) opening a water inlet valve, a discharge valve and a discharge water pump, collecting materials, and closing the water inlet valve, the discharge valve and the discharge water pump until the solution in the horizontal reaction furnace has no black solid;
(6) and filtering the collected materials to obtain solid black porous carbon powder.
Preferably, the inert gas is one or more of nitrogen, argon and helium.
Preferably, the inert gas flow rate is 1 to 2L/min.
Preferably, the stirring speed is 900-.
Preferably, the horizontal reaction furnace is heated at a speed of 1-10 ℃/min during the heating process.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method for recovering the waste electrode slurry is simple and suitable for large-scale production.
(2) The porous carbon recovered by the method has high specific surface area and large pore volume, and has no difference compared with the performance of the original porous carbon.
(3) The porous carbon recycled by the invention can be used for water filtration, air filtration (mask) and the like, and can also be used as a super-capacitor energy storage material for continuous use.
Drawings
FIG. 1 is a schematic diagram of an apparatus for self-activating and recovering porous carbon from waste electrode slurry of a supercapacitor according to one embodiment of the invention.
In the figure, 1, a horizontal reaction furnace, 2, a stirring paddle, 21, blades, 3, a heating sleeve, 4, a flange, 5, an air inlet valve, 6, air outlet valves 1 and 7, air outlet valves 2 and 8, an water inlet valve, 9, a waste inlet valve, 10 and a discharge valve.
Detailed Description
The technical solution of the present invention will be further described and illustrated by the following specific embodiments in conjunction with the accompanying drawings. The raw materials used in the examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
As shown in fig. 1, the device for automatically recycling porous carbon in one embodiment of the present invention includes a horizontal reaction furnace (1), a stirring paddle (2), a paddle (21) on the stirring paddle, a traction motor (not shown), a heating jacket (3), a flange (4), an air inlet valve (5), an air inlet valve (8), a waste inlet valve (9), an air outlet valve (1), (6), an air outlet valve (2), (7), a discharging valve (10), and a discharging water pump (not shown).
The traction motor drives the stirring paddle (2) to rotate, the heating sleeve (3) heats the horizontal reaction furnace (1), the flange (4) is used for sealing the horizontal reaction furnace (1), and the discharging water pump extracts materials in the horizontal reaction furnace (1) for collection.
The horizontal reaction furnace (1) is made of steel or nickel metal or nickel alloy, the heating sleeve (3) is made of resistance wires (iron wires or copper wires) of the winding reaction furnace, and the stirring paddle (2) and the blades (21) are made of steel or nickel metal or nickel alloy.
The device in FIG. 1 is adopted to recover the porous carbon in the waste electrode slurry of the super capacitor, and the specific process comprises the following steps:
(1) and opening a waste material inlet valve (9), placing the waste electrode slurry into the horizontal reaction furnace (1), wherein the volume of the entered waste electrode slurry is less than or equal to 4/5 of the horizontal reaction furnace, and then closing the waste material inlet valve (9).
(2) Simultaneously or sequentially opening the air inlet valve (5) and the air outlet valve (2) (7), introducing inert gas for 10-20min, and then sequentially closing the air inlet valve (5) and the air outlet valve (2) (7); the introduced inert gas is one or more of nitrogen, argon and helium, and the flow rate of the inert gas is 1-2L/min. So that the horizontal reaction furnace (1) is filled with inert gas atmosphere.
(3) And (3) turning on a traction motor, driving the stirring paddle (2) to rotate at the speed of 900-.
(4) Simultaneously or sequentially opening an air inlet valve (5), an air outlet valve 1(6) and an air outlet valve 2(7), introducing inert gas for 10-20min at the flow rate of 1-2L/min, and then closing the air inlet valve (5), the air outlet valve 1(6) and the air outlet valve 2(7) to naturally cool the horizontal reaction furnace (1) to room temperature; gases formed after the reaction in the reaction furnace, including water vapor and carbon dioxide generated by the reaction, are removed.
(5) Opening a water inlet valve (8), a discharge valve (10) and a discharge water pump, pumping and collecting materials in the horizontal reaction furnace (1) through the discharge water pump, and closing the water inlet valve (8), the discharge valve (10) and the discharge water pump until the solution in the horizontal reaction furnace (1) is free of black solids;
(6) and filtering the collected materials to obtain solid black porous carbon powder.
The device is adopted to activate the waste electrode slurry of the super capacitor by water vapor to convert the waste electrode slurry into the porous carbon, the device and the method are simple, the waste electrode slurry is heated in a horizontal reaction furnace in an inert atmosphere step by step, and the waste electrode slurry is subjected to water activation and washing, so that the specific surface area and the pore volume of the recovered porous carbon are compared with the performance of the original porous carbon, and no difference exists.
Example 1
Opening a waste inlet valve (9), placing waste electrode slurry containing activated carbon and a binder into a horizontal reaction furnace (1), wherein the volume of the entered waste electrode slurry accounts for 2/3 of the horizontal reaction furnace, and then closing the waste inlet valve (9);
sequentially opening the air inlet valve (5) and the air outlet valve 2(7), introducing nitrogen inert gas for 15min, wherein the flow rate of the inert gas is 1.5L/min, and then sequentially closing the air inlet valve (5) and the air outlet valve 2 (7);
turning on a traction motor, driving a stirring paddle (2) to rotate by the traction motor, enabling the stirring speed to reach 1200r/min, stirring for 0.5h, heating the horizontal reaction furnace (1) to 120 ℃ at the speed of 8 ℃/min, and preserving heat for 2 h; heating the horizontal reaction furnace (1) to 800 ℃ at the speed of 3 ℃/min, preserving the heat for 2 hours, and then turning off the heating device;
simultaneously opening an air inlet valve (5), an air outlet valve 1(6) and an air outlet valve 2(7), keeping the flow rate of nitrogen inert gas at 1L/min for 10min, closing the air inlet valve (5), the air outlet valve 1(6) and the air outlet valve 2(7), and naturally cooling the horizontal reaction furnace (1) to room temperature;
opening a water inlet valve (8), a discharge valve (10) and a discharge water pump, pumping and collecting materials in the horizontal reaction furnace (1) through the discharge water pump, and closing the traction motor, the water inlet valve (8), the discharge valve (10) and the discharge water pump until the solution in the horizontal reaction furnace (1) is free of black solids;
and filtering the solution to obtain solid black activated carbon powder with high specific surface area and pore volume.
Example 2
Opening a waste inlet valve (9), placing waste electrode slurry containing activated carbon and a binder into a horizontal reaction furnace (1), wherein the volume of the entered waste electrode slurry accounts for 2/3 of the horizontal reaction furnace, and then closing the waste inlet valve (9);
sequentially opening the air inlet valve (5) and the air outlet valve 2(7), introducing nitrogen inert gas for 10min at the inert gas flow rate of 1L/min, and then sequentially closing the air inlet valve (5) and the air outlet valve 2 (7);
turning on a traction motor, driving a stirring paddle (2) to rotate by the traction motor, enabling the stirring speed to reach 900r/min, stirring for 0.5h, heating the horizontal reaction furnace (1) to 100 ℃ at the speed of 1 ℃/min, and preserving heat for 1 h; heating the horizontal reaction furnace (1) to 700 ℃ at the speed of 1 ℃/min, preserving the heat for 1h, and then turning off the heating device;
simultaneously opening an air inlet valve (5), an air outlet valve 1(6) and an air outlet valve 2(7), keeping the flow rate of nitrogen inert gas at 1L/min for 10min, closing the air inlet valve (5), the air outlet valve 1(6) and the air outlet valve 2(7), and naturally cooling the horizontal reaction furnace (1) to room temperature;
opening a water inlet valve (8), a discharge valve (10) and a discharge water pump, pumping and collecting materials in the horizontal reaction furnace (1) through the discharge water pump, and closing the traction motor, the water inlet valve (8), the discharge valve (10) and the discharge water pump until the solution in the horizontal reaction furnace (1) is free of black solids;
and filtering the solution to obtain solid black activated carbon powder with high specific surface area and pore volume.
Example 3
Opening a waste inlet valve (9), placing waste electrode slurry containing activated carbon and a binder into a horizontal reaction furnace (1), wherein the volume of the entered waste electrode slurry accounts for 3/5 of the horizontal reaction furnace, and then closing the waste inlet valve (9);
sequentially opening the air inlet valve (5) and the air outlet valve 2(7), introducing nitrogen inert gas for 20min, and then sequentially closing the air inlet valve (5) and the air outlet valve 2(7) at the inert gas flow rate of 2L/min;
turning on a traction motor, driving a stirring paddle (2) to rotate by the traction motor, enabling the stirring speed to reach 1500r/min, stirring for 1h, heating the horizontal reaction furnace (1) to 110 ℃ at the speed of 10 ℃/min, and keeping the temperature for 3 h; heating the horizontal reaction furnace (1) to 900 ℃ at the speed of 10 ℃/min, preserving the heat for 3 hours, and then turning off the heating device;
simultaneously opening an air inlet valve (5), an air outlet valve 1(6) and an air outlet valve 2(7), keeping the flow rate of nitrogen inert gas at 2L/min for 20min, closing the air inlet valve (5), the air outlet valve 1(6) and the air outlet valve 2(7), and naturally cooling the horizontal reaction furnace (1) to room temperature;
opening a water inlet valve (8), a discharge valve (10) and a discharge water pump, pumping and collecting materials in the horizontal reaction furnace (1) through the discharge water pump, and closing the traction motor, the water inlet valve (8), the discharge valve (10) and the discharge water pump until the solution in the horizontal reaction furnace (1) is free of black solids;
and filtering the solution to obtain solid black activated carbon powder with high specific surface area and pore volume.
Example 4
Opening a waste inlet valve (9), placing waste electrode slurry containing activated carbon and a binder into a horizontal reaction furnace (1), wherein the volume of the entered waste electrode slurry accounts for 3/5 of the horizontal reaction furnace, and then closing the waste inlet valve (9);
sequentially opening the air inlet valve (5) and the air outlet valve 2(7), introducing nitrogen inert gas for 17min, wherein the flow rate of the inert gas is 1.8L/min, and then sequentially closing the air inlet valve (5) and the air outlet valve 2 (7);
turning on a traction motor, driving a stirring paddle (2) to rotate by the traction motor, enabling the stirring speed to reach 1000r/min, stirring for 1h, heating the horizontal reaction furnace (1) to 105 ℃ at the speed of 4 ℃/min, and keeping the temperature for 1.8 h; heating the horizontal reaction furnace (1) to 750 ℃ at the speed of 3 ℃/min, preserving heat for 2 hours, and then turning off the heating device;
simultaneously opening an air inlet valve (5), an air outlet valve 1(6) and an air outlet valve 2(7), keeping the flow rate of nitrogen inert gas at 2L/min for 20min, closing the air inlet valve (5), the air outlet valve 1(6) and the air outlet valve 2(7), and naturally cooling the horizontal reaction furnace (1) to room temperature;
opening a water inlet valve (8), a discharge valve (10) and a discharge water pump, pumping and collecting materials in the horizontal reaction furnace (1) through the discharge water pump, and closing the traction motor, the water inlet valve (8), the discharge valve (10) and the discharge water pump until the solution in the horizontal reaction furnace (1) is free of black solids;
and filtering the solution to obtain solid black activated carbon powder with high specific surface area and pore volume.
Example 5
The only difference from example 1 is that example 5 has a stirring speed of 1050 r/min.
Example 6
The difference from the example 1 is that in the example 6, the horizontal reaction furnace is heated to 120 ℃ at the speed of 8 ℃/min and is kept for 2 hours, and instead, the horizontal reaction furnace is heated to 120 ℃ at the speed of 4 ℃/min and is kept for 1 hour.
Example 7
The only difference from example 1 is that in example 7, inert gas is introduced for 15min at an inert gas flow rate of 1.5L/min, and inert gas is introduced for 20min at an inert gas flow rate of 1L/min.
Example 8
The difference from the example 1 is only that in the example 8, the horizontal reaction furnace is heated to 800 ℃ at the speed of 3 ℃/min and is kept for 2h, and instead, the horizontal reaction furnace is heated to 800 ℃ at the speed of 10 ℃/min and is kept for 2.5 h.
Example 9
The only difference from example 1 is that in example 9, the flow rate of inert gas is 1L/min and maintained for 10min, and the flow rate of inert gas is changed to 1.7L/min and maintained for 15 min.
Example 10
The only difference from example 1 is that in example 10, the horizontal reaction furnace is heated to 120 ℃ at a speed of 8 ℃/min and kept for 2h, and instead, the horizontal reaction furnace is heated to 115 ℃ at a speed of 8 ℃/min and kept for 1 h.
Comparative example 1
Comparative example 1 differs from example 1 only in that comparative example 1 does not go through the recovery system, but instead employs direct precipitation to obtain activated carbon using prior art techniques.
Comparative example 2
Comparative example 2 differs from example 1 only in that the horizontal reaction furnace (1) of example 1 was heated to 120 ℃ at a rate of 8 ℃/min and held for 2 h; then heating the horizontal reaction furnace (1) to 800 ℃ at the speed of 3 ℃/min, and preserving the heat for 2 hours; the horizontal reaction furnace (1) is heated to 800 ℃ at the speed of 8 ℃/min, and the temperature is kept for 2 h.
Comparative example 3
Comparative example 3 differs from example 1 only in that the horizontal reactor (1) of example 1 was heated to 120 ℃ at a rate of 8 ℃/min and held for 2 h; then heating the horizontal reaction furnace (1) to 800 ℃ at the speed of 3 ℃/min, and preserving the heat for 2 hours; heating the horizontal reaction furnace (1) to 120 ℃ at the speed of 15 ℃/min, and preserving heat for 2 hours; then the horizontal reaction furnace (1) is heated to 800 ℃ at the speed of 15 ℃/min and is kept warm for 2 h.
The activated carbons obtained in examples 1 to 10 and comparative examples 1 to 3 and the raw activated carbon in the waste electrode slurry were subjected to the test of specific surface area and pore volume, and the results are shown in table 1.
TABLE 1 Properties of activated carbon and raw activated carbon in examples 1 to 10 and comparative examples 1 to 3
| Specific surface area (m)2/g) | Pore volume (cm)3/g) | |
| Example 1 | 1730 | 0.94 |
| Example 2 | 1690 | 0.99 |
| Example 3 | 1680 | 0.95 |
| Example 4 | 1720 | 0.94 |
| Example 5 | 1692 | 0.95 |
| Example 6 | 1712 | 0.98 |
| Example 7 | 1708 | 0.98 |
| Example 8 | 1696 | 0.94 |
| Example 9 | 1699 | 0.94 |
| Example 10 | 1723 | 0.98 |
| Raw activated carbon | 1705 | 0.96 |
| Comparative example 1 | 1210 | 0.62 |
| Comparative example 2 | 1420 | 0.75 |
| Comparative example 3 | 1589 | 0.86 |
As can be seen from table 1, the activated carbon recovered in the example of the present invention has a high specific surface area and pore volume, which are not significantly different from those of the original activated carbon in the waste electrode slurry. The stepwise temperature rise and the temperature rise speed in the present invention have a large influence on the specific surface area and the pore volume of the recovered activated carbon, and as can be seen from comparative examples 2 to 3, the specific surface area and the pore volume of the recovered activated carbon are reduced by the one-step temperature rise and the rapid temperature rise.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (1)
1. A method for self-activating and recovering porous carbon by using super capacitor waste electrode slurry is characterized in that a device for self-activating and recovering porous carbon by using the super capacitor waste electrode slurry is used, and the device comprises a horizontal reaction furnace, a stirring paddle, blades on the stirring paddle, a traction motor, a heating sleeve, a flange, a plurality of air inlet valves, a plurality of feeding valves, a plurality of air outlet valves, a plurality of discharging valves and a discharging water pump; the device comprises 1 intake valve; 1 discharge valve; 2 air outlet valves, wherein each air outlet valve comprises an air outlet valve 1 and an air outlet valve 2; 2 feeding valves, wherein the feeding valves comprise a water inlet valve and a waste inlet valve; the method comprises the following steps:
(1) opening a waste material inlet valve, placing the waste electrode slurry in a horizontal reaction furnace, and then closing the waste material inlet valve;
(2) opening the air inlet valve and the air outlet valve 2, introducing inert gas for 10-20min, and then closing the air inlet valve and the air outlet valve 2;
(3) turning on a traction motor, driving a stirring paddle to rotate and stir for 0.5-1h, heating the horizontal reaction furnace to 120 ℃ and preserving heat for 1-3h, then heating the horizontal reaction furnace to 900 ℃ and preserving heat for 1-3h, and then stopping heating;
(4) opening an air inlet valve, an air outlet valve 1 and an air outlet valve 2, introducing inert gas for 10-20min, and then closing the air inlet valve, the air outlet valve 1 and the air outlet valve 2 to naturally cool the horizontal reaction furnace to room temperature;
(5) opening a water inlet valve, a discharge valve and a discharge water pump, collecting materials, and closing the water inlet valve, the discharge valve and the discharge water pump until the solution in the horizontal reaction furnace has no black solid;
(6) filtering the collected materials to obtain solid black porous carbon powder;
heating at the speed of 1-10 ℃/min in the heating process of the horizontal reaction furnace;
the inert gas is one or more of nitrogen, argon and helium;
the flow rate of the inert gas is 1-2L/min; the stirring speed is 900-1500 r/min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101592439A (en) * | 2009-06-03 | 2009-12-02 | 淮北市协力重型机器有限责任公司 | Active carbon horizontal converter |
| CN102530939A (en) * | 2012-02-28 | 2012-07-04 | 宜兴市昌华过滤器材有限公司 | Active carbon recycling device and recycling technology |
| CN103936001A (en) * | 2013-01-18 | 2014-07-23 | 沈善明 | Horizontal thermal regeneration furnace for waste powdered activated carbon |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101592439A (en) * | 2009-06-03 | 2009-12-02 | 淮北市协力重型机器有限责任公司 | Active carbon horizontal converter |
| CN102530939A (en) * | 2012-02-28 | 2012-07-04 | 宜兴市昌华过滤器材有限公司 | Active carbon recycling device and recycling technology |
| CN103936001A (en) * | 2013-01-18 | 2014-07-23 | 沈善明 | Horizontal thermal regeneration furnace for waste powdered activated carbon |
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