CN114394593A - Method for preparing nitrogen-containing activated carbon by activating ammonia gas - Google Patents
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Abstract
A method for preparing nitrogen-containing activated carbon by ammonia activation belongs to the technical field of activated carbon modification, and comprises four steps of pretreatment, alkali treatment, impregnation and activation. According to the method, the activation temperature is relatively low (700-800 ℃), the operation is simple, and the nitrogen content of the surface of the prepared activated carbon is high (6.93-8.24%); the nitrogen-containing activated carbon prepared by the method has the nitrogen contents of 6.93 percent, 8.24 percent and 7.03 percent respectively and the yields of 85.2 percent, 78.9 percent and 63.7 percent respectively (the yield of the nitrogen-containing activated carbon after ammonia activation is calculated according to the mass ratio of the obtained nitrogen-containing activated carbon to the mass of the raw material activated carbon) at the activation temperature of 700 ℃, 750 ℃ and 800 ℃.
Description
Technical Field
The invention relates to a method for preparing nitrogen-containing activated carbon by activating ammonia gas, belonging to the technical field of activated carbon modification.
Background
The nitrogenous active carbon has the advantages of large specific surface area, developed pores, easily-regulated surface acid-base property, strong acid-base resistance, high-temperature hydrothermal environment resistance, no metal dissolution, environment friendliness and the like, and meanwhile, the existence of nitrogen in the active carbon can change the local electronic structure on the surface of the carbon material to form a local electron-rich area, so that the surface of the active carbon has the property of solid base, and certain catalytic activity is displayed, and the nitrogenous active carbon shows a certain application prospect in the field of catalysts. In addition, the special electrochemical performance of the nitrogenous activated carbon enables the nitrogenous activated carbon to be widely applied to the aspect of supercapacitors.
In the prior art, the method for preparing the nitrogen-containing activated carbon mainly adopts plasma treatment, nitrogen-containing compound impregnation and the like to modify the surface of the activated carbon so as to achieve the purpose of introducing nitrogen elements. However, the method has complex process operation and relatively high preparation cost, and the content of nitrogen elements on the surface of the prepared nitrogen-containing activated carbon is not high.
Chinese patent CN106629721A discloses a method for safely producing nitrogen-containing super activated carbon, which comprises the steps of introducing ammonia gas for activation in the KOH activation process, not only utilizing the reaction of the ammonia gas and the carbon at high temperature to generate a developed pore structure, but also utilizing the reaction of the ammonia gas and potassium to solve the problem of release of potassium in the KOH activation process, and simultaneously achieving the purpose of doping nitrogen elements on the surface of the activated carbon. The ammonia gas activation method disclosed in the patent only introduces ammonia gas in the activation step of the conventional preparation process of super activated carbon, and the KOH activation and the ammonia gas activation have competitive reaction, and the patent cannot obtain activated carbon with high surface nitrogen content.
Chinese patent CN105905895A discloses a preparation device and a preparation method of nitrogen-containing activated carbon, and the preparation process of the nitrogen-containing activated carbon comprises the following steps: carbonizing a precursor; and (4) activating the carbonized precursor by ammonia gas. The method disclosed by the patent activates carbonized activated carbon by using a mixture of ammonia and water vapor, so that the process requirement is harsh, the equipment is seriously corroded by high-temperature ammonia and water vapor, and the equipment cost is higher.
The problems of high activation temperature, complex operation, low nitrogen content on the surface of the activated carbon and the like still exist in the existing preparation method of the nitrogenous activated carbon, so that the development of the preparation method which has relatively low activation temperature and simple operation and can improve the nitrogen content on the surface of the activated carbon has great significance for improving the application quality of the nitrogenous activated carbon.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing nitrogen-containing activated carbon by activating ammonia gas, which realizes the following purposes: the preparation method of the nitrogenous activated carbon is relatively low in activation temperature and simple to operate, and the activated carbon prepared by the method is high in surface nitrogen content.
In order to realize the purpose, the invention adopts the following technical scheme:
a method for preparing nitrogen-containing activated carbon by activating ammonia gas comprises four steps of pretreatment, alkali treatment, impregnation and activation.
The following is a further improvement of the above technical solution:
step 1: pretreatment of
Dissolving water-soluble amide, a surfactant and a permeation promoter in deionized water to prepare a pretreatment solution, controlling the temperature to be 60-90 ℃, putting activated carbon into the solution, carrying out ultrasonic oscillation for 2-8 hours, filtering out the activated carbon, leaching the activated carbon with deionized water until the pH value is neutral, putting the activated carbon into an oven, and drying the activated carbon for 2-4 hours at 90-130 ℃ to obtain the pretreated activated carbon;
the particle size of the activated carbon is 5-30 meshes, the internal pore diameter is 50-150 nanometers, and the specific surface area is 700-950 m/g;
the mass ratio of the activated carbon to the pretreatment solution is 20-40: 100;
in the pretreatment solution, the mass ratio of water-soluble amide, a surfactant, a penetration enhancer and deionized water is 5-10: 1-2: 0.5-1.5: 50-80;
the water-soluble amide is one of cyanoacetamide, sulfonamide and methyl sulfonamide;
the surfactant is one of N, N, 4-trimethylaniline amine oxide, N-dimethyl decyl-N-amine oxide and tri (2-hydroxyethyl) methyl amine hydroxide;
the penetration enhancer is fatty alcohol-polyoxyethylene ether.
Step 2: alkali treatment
Dissolving quaternary ammonium salt and amine-containing phosphonic acid in an aqueous solution of sodium hydroxide to obtain an alkali treatment solution, controlling the temperature to be 40-70 ℃, putting the pretreated activated carbon into the alkali treatment solution, soaking for 40-50 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying at 90-130 ℃ for 1-4 hours to obtain the alkali-treated activated carbon;
the mass ratio of the pretreated activated carbon to the alkali treatment solution is 15-30: 100;
in the alkali treatment liquid, the mass ratio of the quaternary ammonium salt to the amine-containing phosphonic acid to the sodium hydroxide aqueous solution is 2-9: 0.8-2: 60-75;
the mass concentration of the sodium hydroxide aqueous solution is 10-16 wt%;
the quaternary ammonium salt is one of tetraethylammonium chloride, tetrapropylammonium chloride and tetrapropylammonium bromide;
the amine-containing phosphonic acid is one of hexamethylenediamine tetramethylene phosphonic acid, polyamino polyether methylene phosphonic acid and bis (1, 6-hexamethylene triamine pentamethylene phosphonic acid).
And step 3: impregnation
Dissolving hydrazine sulfate, sodium thiosulfate and thiourea dioxide in deionized water to obtain an impregnation liquid, controlling the temperature to be 50-70 ℃, putting the activated carbon subjected to alkali treatment into the impregnation liquid, impregnating for 24-48 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying at 100-140 ℃ for 1.5-3 hours to obtain the activated carbon subjected to impregnation treatment;
the mass ratio of the alkali-treated activated carbon to the impregnation liquid is 15-35: 100;
in the dipping solution, the mass ratio of hydrazine sulfate, sodium thiosulfate, thiourea dioxide and deionized water is 3-10: 2-9: 1-11: 70-95.
And 4, step 4: activation of
Putting the impregnated activated carbon into a vacuum tube furnace, introducing mixed gas of ammonia and nitrogen, heating to 700-800 ℃ at a heating rate of 2-8 ℃/min, keeping the temperature for 1-2.5 hours, continuing introducing the mixed gas, cooling to room temperature, and taking out to obtain nitrogen-containing activated carbon;
the volume ratio of ammonia gas to nitrogen gas in the mixed gas is 1: 0.5-2;
the introduction speed of the mixed gas is 0.5-3.5 mL/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the method for preparing the nitrogen-containing activated carbon has relatively low activation temperature (700-800 ℃), is simple to operate, and the nitrogen content of the surface of the prepared activated carbon is high (6.93-8.24%);
2. the nitrogen-containing activated carbon prepared by the method has the nitrogen contents of 6.93 percent, 8.24 percent and 7.03 percent respectively and the yields of 85.2 percent, 78.9 percent and 63.7 percent respectively at the activation temperature of 700 ℃, 750 ℃ and 800 ℃ (the yield of the nitrogen-containing activated carbon after ammonia activation is calculated according to the mass ratio of the obtained nitrogen-containing activated carbon to the raw material activated carbon);
3. according to the method for preparing the nitrogen-containing activated carbon, 750 ℃ is the optimal activation temperature, the nitrogen content of the nitrogen-containing activated carbon is the highest and reaches 8.24% at the temperature, and the yield of the activated carbon can reach 78.9% (the yield of the nitrogen-containing activated carbon after ammonia activation is calculated according to the mass ratio of the obtained nitrogen-containing activated carbon to the raw material activated carbon).
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1: method for preparing nitrogen-containing activated carbon by activating ammonia gas
The method comprises the following steps:
1. pretreatment of
Dissolving water-soluble amide, a surfactant and a permeation promoter in deionized water to prepare a pretreatment solution, controlling the temperature at 80 ℃, putting activated carbon into the solution, ultrasonically oscillating for 4 hours, filtering out the activated carbon, leaching the activated carbon with deionized water until the pH value is neutral, putting the activated carbon into an oven, and drying for 3 hours at 110 ℃ to obtain the pretreated activated carbon;
the particle size of the activated carbon is 15 meshes, the internal pore diameter is 90 nanometers, and the specific surface area is 850 m/g;
the mass ratio of the activated carbon to the pretreatment solution is 30: 100;
in the pretreatment solution, the mass ratio of water-soluble amide to surfactant to penetration aid to deionized water is 8:1.5:1.0: 70;
the water-soluble amide is cyanoacetamide;
the surfactant is N, N, 4-trimethylaniline amine oxide;
the penetration enhancer is fatty alcohol-polyoxyethylene ether.
2. Alkali treatment
Dissolving quaternary ammonium salt and amine-containing phosphonic acid in an aqueous solution of sodium hydroxide to obtain an alkali treatment solution, controlling the temperature to be below 50 ℃, putting the pretreated activated carbon into the alkali treatment solution, soaking for 44 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying for 2.5 hours at 100 ℃ to obtain the alkali-treated activated carbon;
the mass ratio of the pretreated active carbon to the alkali treatment solution is 20: 100;
in the alkali treatment liquid, the mass ratio of the quaternary ammonium salt to the amine-containing phosphonic acid to the sodium hydroxide aqueous solution is 5:1.2: 68;
the mass concentration of the sodium hydroxide aqueous solution is 14 wt%;
the quaternary ammonium salt is tetraethylammonium chloride;
the amine-containing phosphonic acid is hexamethylenediamine tetramethylidene phosphonic acid.
3. Impregnation
Dissolving hydrazine sulfate, sodium thiosulfate and thiourea dioxide in deionized water to obtain an impregnation solution, controlling the temperature to be 60 ℃, putting the alkali-treated activated carbon into the impregnation solution, impregnating for 36 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying for 2 hours at 120 ℃ to obtain the impregnated activated carbon;
the mass ratio of the alkali-treated activated carbon to the impregnation liquid is 25: 100;
in the impregnation liquid, the mass ratio of hydrazine sulfate, sodium thiosulfate, thiourea dioxide and deionized water is 6:7:6: 80.
4. Activation of
Putting the impregnated activated carbon into a vacuum tube furnace, introducing mixed gas of ammonia and nitrogen, heating to 750 ℃ at the heating rate of 5 ℃/min, preserving the temperature for 2 hours, continuously introducing the mixed gas, cooling to room temperature, and taking out to obtain nitrogen-containing activated carbon;
the volume ratio of ammonia gas to nitrogen gas in the mixed gas is 1: 1.5;
the introduction speed of the mixed gas is 2 mL/min.
Example 2: method for preparing nitrogen-containing activated carbon by activating ammonia gas
The method comprises the following steps:
1. pretreatment of
Dissolving water-soluble amide, a surfactant and a permeation promoter in deionized water to prepare a pretreatment solution, controlling the temperature at 60 ℃, putting activated carbon into the solution, ultrasonically oscillating for 2 hours, filtering out the activated carbon, leaching the activated carbon with deionized water until the pH value is neutral, putting the activated carbon into an oven, and drying for 2 hours at 90 ℃ to obtain the pretreated activated carbon;
the particle size of the activated carbon is 5 meshes, the internal pore diameter is 50 nanometers, and the specific surface area is 700 m/g;
the mass ratio of the activated carbon to the pretreatment solution is 20: 100;
in the pretreatment solution, the mass ratio of water-soluble amide to surfactant to penetration aid to deionized water is 5:1:0.5: 50;
the water-soluble amide is sulfonamide;
the surfactant is N, N-dimethyl decyl-N-amine oxide;
the penetration enhancer is fatty alcohol-polyoxyethylene ether.
2. Alkali treatment
Dissolving quaternary ammonium salt and amine-containing phosphonic acid in an aqueous solution of sodium hydroxide to obtain an alkali treatment solution, controlling the temperature at 40 ℃, putting the pretreated activated carbon into the alkali treatment solution, soaking for 40 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying at 90 ℃ for 1 hour to obtain the alkali-treated activated carbon;
the mass ratio of the pretreated active carbon to the alkali treatment solution is 15: 100;
in the alkali treatment liquid, the mass ratio of the quaternary ammonium salt to the amine-containing phosphonic acid to the sodium hydroxide aqueous solution is 2:0.8: 60;
the mass concentration of the sodium hydroxide aqueous solution is 10 wt%;
the quaternary ammonium salt is tetrapropylammonium chloride;
the amine-containing phosphonic acid is polyamino polyether methylene phosphonic acid.
3. Impregnation
Dissolving hydrazine sulfate, sodium thiosulfate and thiourea dioxide in deionized water to obtain an impregnation solution, controlling the temperature to be 50 ℃, putting the alkali-treated activated carbon into the impregnation solution, impregnating for 24 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying at 100 ℃ for 1.5 hours to obtain the impregnated activated carbon;
the mass ratio of the alkali-treated activated carbon to the impregnation liquid is 15: 100;
in the impregnation liquid, the mass ratio of hydrazine sulfate, sodium thiosulfate, thiourea dioxide and deionized water is 3:2:1: 70.
4. Activation of
Putting the impregnated activated carbon into a vacuum tube furnace, introducing mixed gas of ammonia and nitrogen, heating to 700 ℃ at the heating rate of 2 ℃/min, preserving the temperature for 1 hour, continuing introducing the mixed gas, cooling to room temperature, and taking out to obtain nitrogen-containing activated carbon;
the volume ratio of ammonia gas to nitrogen gas in the mixed gas is 1: 0.5;
the introduction speed of the mixed gas is 0.5 mL/min.
Example 3: method for preparing nitrogen-containing activated carbon by activating ammonia gas
The method comprises the following steps:
1. pretreatment of
Dissolving water-soluble amide, a surfactant and a permeation promoter in deionized water to prepare a pretreatment solution, controlling the temperature at 90 ℃, putting activated carbon into the solution, ultrasonically oscillating for 8 hours, filtering out the activated carbon, leaching the activated carbon with deionized water until the pH value is neutral, putting the activated carbon into an oven, and drying for 4 hours at 130 ℃ to obtain the pretreated activated carbon;
the particle size of the activated carbon is 30 meshes, the internal pore diameter is 150 nanometers, and the specific surface area is 950 m/g;
the mass ratio of the activated carbon to the pretreatment solution is 40: 100;
in the pretreatment solution, the mass ratio of water-soluble amide to surfactant to penetration aid to deionized water is 10:2:1.5: 80;
the water-soluble amide is methyl sulfonamide;
the surfactant is tris (2-hydroxyethyl) methyl ammonium hydroxide;
the penetration enhancer is fatty alcohol-polyoxyethylene ether.
2. Alkali treatment
Dissolving quaternary ammonium salt and amine-containing phosphonic acid in an aqueous solution of sodium hydroxide to obtain an alkali treatment solution, controlling the temperature at 70 ℃, putting pretreated activated carbon into the alkali treatment solution, soaking for 50 hours, taking out, rinsing with deionized water until the pH of an eluate is neutral, and drying at 130 ℃ for 4 hours to obtain alkali-treated activated carbon;
the mass ratio of the pretreated active carbon to the alkali treatment solution is 30: 100;
in the alkali treatment liquid, the mass ratio of the quaternary ammonium salt to the amine-containing phosphonic acid to the sodium hydroxide aqueous solution is 9:2: 75;
the mass concentration of the sodium hydroxide aqueous solution is 16 wt%;
the quaternary ammonium salt is tetrapropyl ammonium bromide;
the amine-containing phosphonic acid is bis-1, 6-hexylidene triamine pentamethylene phosphonic acid.
3. Impregnation
Dissolving hydrazine sulfate, sodium thiosulfate and thiourea dioxide in deionized water to obtain an impregnation solution, controlling the temperature to be 70 ℃, putting the alkali-treated activated carbon into the impregnation solution, impregnating for 48 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying at 140 ℃ for 3 hours to obtain the impregnated activated carbon;
the mass ratio of the alkali-treated activated carbon to the impregnation liquid is 35: 100;
in the impregnation liquid, the mass ratio of hydrazine sulfate, sodium thiosulfate, thiourea dioxide and deionized water is 10: 9:11: 95.
4. Activation of
Putting the impregnated activated carbon into a vacuum tube furnace, introducing mixed gas of ammonia and nitrogen, heating to 800 ℃ at the heating rate of 8 ℃/min, preserving the temperature for 2.5 hours, continuing introducing the mixed gas, cooling to room temperature, and taking out to obtain nitrogen-containing activated carbon;
the volume ratio of ammonia gas to nitrogen gas in the mixed gas is 1: 2;
the introduction speed of the mixed gas is 3.5 mL/min.
Comparative example 1: in example 1, the activated carbon was directly activated without pretreatment, alkali treatment, or impregnation, and the activation temperature was 700 ℃
The operations of the steps 1, 2 and 3 are not carried out;
step 4 was performed as in example 1.
Comparative example 2: in example 1, the activated carbon was directly activated without pretreatment, alkali treatment, or impregnation, and the activation temperature was 900 deg.C
The operations of the steps 1, 2 and 3 are not carried out;
in step 4, the temperature was raised to 900 ℃ for activation, and the rest of the procedure was the same as in example 1.
Analyzing nitrogen-containing activated carbon elements and calculating yield:
1. measuring the contents of C, H, N and O in the nitrogen-containing activated carbon sample by adopting a Vario EL cube type element analyzer of Elementar company of Germany;
2. calculating the yield of the activated carbon containing nitrogen after the activation of ammonia gas according to the mass ratio of the obtained activated carbon containing nitrogen to the raw material activated carbon;
the test results are given in the following table:
Claims (3)
1. a method for preparing nitrogen-containing activated carbon by activating ammonia gas is characterized by comprising the following steps: comprises four steps of pretreatment, alkali treatment, impregnation and activation;
dissolving water-soluble amide, a surfactant and an auxiliary permeation agent in deionized water to prepare a pretreatment solution, controlling the temperature to be 60-90 ℃, putting activated carbon into the solution, carrying out ultrasonic oscillation for 2-8 hours, filtering out the activated carbon, leaching the activated carbon with the deionized water until the pH value is neutral, putting the activated carbon into an oven, and drying the activated carbon for 2-4 hours at the temperature of 90-130 ℃ to obtain the pretreated activated carbon;
the particle size of the activated carbon is 5-30 meshes, the internal pore diameter is 50-150 nanometers, and the specific surface area is 700-950 m/g;
the mass ratio of the activated carbon to the pretreatment solution is 20-40: 100;
in the pretreatment solution, the mass ratio of water-soluble amide, a surfactant, a penetration enhancer and deionized water is 5-10: 1-2: 0.5-1.5: 50-80;
the water-soluble amide is one of cyanoacetamide, sulfonamide and methyl sulfonamide;
the surfactant is one of N, N, 4-trimethylaniline amine oxide, N-dimethyl decyl-N-amine oxide and tri (2-hydroxyethyl) methyl amine hydroxide;
the penetration enhancer is fatty alcohol-polyoxyethylene ether;
dissolving quaternary ammonium salt and amine-containing phosphonic acid in a sodium hydroxide aqueous solution to obtain an alkali treatment solution, controlling the temperature to be 40-70 ℃, putting the pretreated activated carbon into the alkali treatment solution, soaking for 40-50 hours, taking out, leaching with deionized water until the pH of an eluate is neutral, and drying for 1-4 hours at 90-130 ℃ to obtain the alkali-treated activated carbon;
the mass ratio of the pretreated activated carbon to the alkali treatment solution is 15-30: 100;
in the alkali treatment liquid, the mass ratio of the quaternary ammonium salt to the amine-containing phosphonic acid to the sodium hydroxide aqueous solution is 2-9: 0.8-2: 60-75;
the mass concentration of the sodium hydroxide aqueous solution is 10-16 wt%;
the quaternary ammonium salt is one of tetraethylammonium chloride, tetrapropylammonium chloride and tetrapropylammonium bromide;
the amine-containing phosphonic acid is one of hexamethylenediamine tetramethylene phosphonic acid, polyamino polyether methylene phosphonic acid and bis (1, 6-hexamethylene triamine pentamethylene phosphonic acid);
dissolving hydrazine sulfate, sodium thiosulfate and thiourea dioxide in deionized water to obtain an impregnation solution, controlling the temperature to be 50-70 ℃, putting the alkali-treated activated carbon into the impregnation solution, taking out after impregnating for 24-48 hours, leaching with deionized water until the pH of an eluate is neutral, and drying at 100-140 ℃ for 1.5-3 hours to obtain the impregnated activated carbon;
the mass ratio of the alkali-treated activated carbon to the impregnation liquid is 15-35: 100;
in the dipping solution, the mass ratio of hydrazine sulfate, sodium thiosulfate, thiourea dioxide and deionized water is 3-10: 2-9: 1-11: 70-95;
putting the impregnated activated carbon into a vacuum tube furnace, introducing mixed gas of ammonia gas and nitrogen gas, heating to 700-800 ℃, keeping the temperature for 1-2.5 hours, continuing introducing the mixed gas, cooling to room temperature, and taking out to obtain nitrogen-containing activated carbon;
the volume ratio of ammonia gas to nitrogen gas in the mixed gas is 1: 0.5-2.
2. The method for preparing nitrogen-containing activated carbon by activating ammonia gas as claimed in claim 1, wherein the method comprises the following steps:
in the activation step, the introduction speed of the mixed gas is 0.5-3.5 mL/min.
3. The method for preparing nitrogen-containing activated carbon by activating ammonia gas as claimed in claim 1, wherein the method comprises the following steps:
in the activation step, the temperature rise rate is 2-8 ℃/min.
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| CN114956079A (en) * | 2022-06-27 | 2022-08-30 | 浙江农林大学 | Method for preparing activated carbon by wood biomass ammonia baking pretreatment |
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| CN114956079B (en) * | 2022-06-27 | 2024-03-08 | 浙江农林大学 | Method for preparing activated carbon by baking pretreatment of woody biomass ammonia |
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Denomination of invention: A method for preparing nitrogen-containing activated carbon by ammonia activation Effective date of registration: 20230104 Granted publication date: 20220607 Pledgee: Linqu Chengguan sub branch of Weifang Bank Co.,Ltd. Pledgor: SHANDONG HENGCHANG SHENGCHENG CHEMICAL Co.,Ltd. Registration number: Y2023980030162 |
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