CN111484011A - Preparation method and application of porous carbon based on cotton - Google Patents
Preparation method and application of porous carbon based on cotton Download PDFInfo
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- CN111484011A CN111484011A CN202010506101.1A CN202010506101A CN111484011A CN 111484011 A CN111484011 A CN 111484011A CN 202010506101 A CN202010506101 A CN 202010506101A CN 111484011 A CN111484011 A CN 111484011A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
Abstract
The invention discloses a preparation method and application of porous carbon based on cotton, and relates to preparation of porous carbon. The invention aims to solve the problems of low specific surface area and low pollutant adsorption capacity of the porous carbon prepared by the existing method and based on cotton. The method comprises the following steps: firstly, soaking and drying cotton; secondly, firing the cotton; thirdly, grinding; fourthly, mixing with an activating agent; fifthly, activation; sixthly, washing; the application comprises the following steps: porous carbon based on cotton is used for adsorption of pollutants in water. The invention relates to a preparation method of porous carbon for cotton.
Description
Technical Field
The invention relates to the preparation of porous carbon.
Background
In recent years, antibiotics have been used in human medicine, agriculture, and animal husbandry, and the threat caused by antibiotics has attracted attention. Studies have shown that 70% of these applied antibiotics enter the water or environment in the form of urine and feces, and are often detected in surface water, ground water, soil, sediment and sewage treatment plants, which also demonstrates the persistence and the difficulty of the antibiotics in the environment. The use of antibiotics leads to the development of resistance by pathogenic microorganisms, and the effective dose of antibiotics to kill bacteria is increasing. Moreover, the drug-resistant gene can expand and evolve in the environment, and potential threats are caused to the ecological environment and human health. There have been a lot of studies on the removal of antibiotics from water by using techniques such as adsorption, membrane filtration, ion exchange, advanced oxidation, coagulation, etc., in which the adsorption technique is considered as a green technique that does not cause secondary pollution. The porous carbon material has the advantages of rich pore channel structure, larger specific surface area, good thermal stability, good chemical stability and the like, and is widely applied to the aspects of adsorption separation, catalyst carriers, capacitor capacitance and the like. However, due to the shortage of fossil energy, the development and application of carbon materials have been limited in recent years. The biological resource can be used as a renewable resource and a substitute of fossil resources to relieve the dilemma caused by the exhaustion of the fossil resources.
The porous carbon prepared by the existing method based on cotton has low specific surface area (0.37 cm)2/g～115cm2/g), low adsorption capacity for contaminants (unmodified porous carbon has almost no adsorption capacity for sulfamethoxazole).
Disclosure of Invention
The invention provides a preparation method and application of porous carbon based on cotton, aiming at solving the problems of low specific surface area and low pollutant adsorption capacity of porous carbon based on cotton prepared by the existing method.
A preparation method of porous carbon based on cotton is characterized by comprising the following steps:
firstly, soaking waste cotton in acetone at a ventilated place to obtain soaked cotton;
secondly, washing the soaked cotton with deionized water, and then drying in an oven to obtain dried cotton;
thirdly, placing the dried cotton in an alumina crucible, then firing in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the firing process, wherein the nitrogen flow is 50m L/min-150 m L/min, then heating the firing temperature to 500-800 ℃ under the condition that the heating rate is 2 ℃/min-5 ℃/min, and firing for 0.5-5 h under the condition that the firing temperature is 500-800 ℃ to obtain a fired sample;
naturally cooling the fired sample to room temperature, and finally grinding the sample into powder to obtain porous carbon powder;
fifthly, mixing an activating agent with the porous carbon powder, and grinding the mixture in a mortar until the mixture is fully mixed to obtain a mixed sample;
the mass ratio of the activating agent to the porous carbon powder is (1-5) to 1;
placing the mixed sample in a covered alumina crucible, heating and activating in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the activation process, wherein the nitrogen flow is 50m L/min-150 m L/min, then heating the activation temperature to 700-1000 ℃ under the condition that the heating rate is 2 ℃/min-5 ℃/min, and activating for 1-5 h under the condition that the activation temperature is 700-1000 ℃ to obtain activated porous carbon;
seventhly, naturally cooling the porous carbon to be activated to room temperature, and washing the porous carbon to be activated by using deionized water as a washing liquid until the washing liquid is neutral to obtain neutral porous carbon powder;
and eighthly, placing the neutral porous carbon powder in an oven for drying to obtain the porous carbon based on cotton.
Use of cotton-based porous carbon for the adsorption of pollutants in water.
The invention has the beneficial effects that: 1. the waste cotton in life and production can be recycled to prepare the porous carbon adsorption material, so that resources are saved.
2. The porous carbon prepared from cotton is activated, the activating agent is easy to obtain, the activation method is simple and easy to implement, the porous carbon can be formed in one step, the preparation speed of the porous carbon is greatly improved, and the specific surface area (which can reach 1808.89 m) is increased2More than g).
3. The adsorption capacity of the activated porous carbon to pollutants is greatly improved, the activated porous carbon can adsorb the pollutants in water in a short time with a small dosage, for example, the activated porous carbon is added into water containing sulfamethoxazole in a solid-liquid mass ratio of 1:10, 97% of sulfamethoxazole can be adsorbed when the solid-liquid mass ratio is 2min, and the adsorption rate is close to 100% when the solid-liquid mass ratio is 6 min.
The invention relates to a preparation method and application of porous carbon based on cotton.
Drawings
FIG. 1 is an XRD pattern of unactivated porous carbon prepared by a comparative experiment;
fig. 2 is an XRD pattern of the cotton-based porous carbon prepared in example one;
FIG. 3 is the BET test results, 1 for cotton-based porous carbon prepared in example one, 2 for unactivated porous carbon prepared in comparative experiment;
fig. 4 is a graph showing adsorption results on sulfamethoxazole, 1 is porous carbon based on cotton prepared in example one, and 2 is non-activated porous carbon prepared in comparative experiment.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: the preparation method of the porous carbon based on cotton according to the embodiment is carried out according to the following steps:
firstly, soaking waste cotton in acetone at a ventilated place to obtain soaked cotton;
secondly, washing the soaked cotton with deionized water, and then drying in an oven to obtain dried cotton;
thirdly, placing the dried cotton in an alumina crucible, then firing in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the firing process, wherein the nitrogen flow is 50m L/min-150 m L/min, then heating the firing temperature to 500-800 ℃ under the condition that the heating rate is 2 ℃/min-5 ℃/min, and firing for 0.5-5 h under the condition that the firing temperature is 500-800 ℃ to obtain a fired sample;
naturally cooling the fired sample to room temperature, and finally grinding the sample into powder to obtain porous carbon powder;
fifthly, mixing an activating agent with the porous carbon powder, and grinding the mixture in a mortar until the mixture is fully mixed to obtain a mixed sample;
the mass ratio of the activating agent to the porous carbon powder is (1-5) to 1;
placing the mixed sample in a covered alumina crucible, heating and activating in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the activation process, wherein the nitrogen flow is 50m L/min-150 m L/min, then heating the activation temperature to 700-1000 ℃ under the condition that the heating rate is 2 ℃/min-5 ℃/min, and activating for 1-5 h under the condition that the activation temperature is 700-1000 ℃ to obtain activated porous carbon;
seventhly, naturally cooling the porous carbon to be activated to room temperature, and washing the porous carbon to be activated by using deionized water as a washing liquid until the washing liquid is neutral to obtain neutral porous carbon powder;
and eighthly, placing the neutral porous carbon powder in an oven for drying to obtain the porous carbon based on cotton.
According to the embodiment, waste cotton in life, such as alcohol cotton, can be used as a raw material, the porous carbon adsorption material is prepared by a high-temperature calcination method, and is activated to increase the specific surface area, so that the adsorption capacity of the porous carbon adsorption material on pollutants in water is enhanced.
Waste cotton generated in life and production is used as a precursor to prepare the porous carbon material with high-efficiency adsorption performance, so that the rapid and high-efficiency purification of sewage is ensured, the resource recovery is realized, and the environmental pollution is reduced.
The beneficial effects of the embodiment are as follows: 1. the waste cotton in life and production can be recycled to prepare the porous carbon adsorption material, so that resources are saved.
2. The porous carbon prepared from cotton is activated, the activating agent is easy to obtain, the activation method is simple and easy to implement, the porous carbon can be formed in one step, the preparation speed of the porous carbon is greatly improved, and the specific surface area (which can reach 1808.89 m) is increased2More than g).
3. The adsorption capacity of the activated porous carbon to pollutants is greatly improved, the activated porous carbon can adsorb the pollutants in water in a short time with a small dosage, for example, the activated porous carbon is added into water containing sulfamethoxazole in a solid-liquid mass ratio of 1:10, 97% of sulfamethoxazole can be adsorbed when the solid-liquid mass ratio is 2min, and the adsorption rate is close to 100% when the solid-liquid mass ratio is 6 min.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: in the first step, the cotton is soaked in acetone for 24 hours or more than 24 hours in a ventilated place to obtain the soaked cotton. The rest is the same as the first embodiment.
The third concrete implementation mode: this embodiment is different from the first or second embodiment in that: drying in an oven, specifically drying for 12-48 h at 60-90 ℃; and step eight, placing the neutral porous carbon powder in a drying oven for drying, specifically drying for 12-24 h at the drying temperature of 60-100 ℃. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and the activating agent in the fifth step is sodium hydroxide, potassium hydroxide or potassium carbonate. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the cotton in the step one is waste cotton or unused cotton. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the waste cotton is waste alcohol cotton. The rest is the same as the first to fifth embodiments.
The seventh embodiment is different from the first to sixth embodiments in that the mixed sample is placed in a covered alumina crucible in the sixth step, and then heated and activated in a tubular furnace, in the activation process, inert gas nitrogen is continuously introduced into the tubular furnace, the nitrogen flow is 50m L/min-100 m L/min, then the activation temperature is raised to 800 ℃ to 1000 ℃ under the condition that the temperature raising speed is 2 ℃/min-5 ℃/min, and the activation temperature is activated for 2 h-5 h under the condition that the activation temperature is 800 ℃ to 1000 ℃, so that activated porous carbon is obtained, and the rest is the same as the first to sixth embodiments.
The specific implementation mode is eight: the porous carbon based on cotton of this embodiment is used for the adsorption of pollutants in water.
The specific implementation method nine: the eighth embodiment is different from the eighth embodiment in that: the pollutants in the water are one or a mixture of more of sulfamethoxazole, sulfisoxazole, sulfadiazine, ciprofloxacin or tetracycline. The rest is the same as the embodiment eight.
The detailed implementation mode is ten: this embodiment differs from one of the eighth or ninth embodiments in that: the cotton-based porous carbon is used for adsorbing pollutants in water by the following steps:
weighing porous carbon based on cotton, and adding the porous carbon into water containing pollutants according to the mass ratio of solid to liquid of (1-2) to 10 to obtain mixed solution;
the concentration of the pollutants in the water containing the pollutants is 0.2 mg/L-2 mg/L;
placing the mixed solution in a shaking table, and adsorbing for 1-60 min under the conditions that the shaking speed is 120-140 r/min and the temperature of the shaking table is 15-45 ℃. The others are the same as the embodiments eight or nine.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of porous carbon based on cotton is carried out according to the following steps:
firstly, soaking waste alcohol cotton in acetone at a ventilated place to obtain soaked alcohol cotton;
secondly, washing the soaked alcohol cotton with deionized water, and then drying in an oven to obtain dried alcohol cotton;
thirdly, placing the dried alcohol cotton in an alumina crucible, and then firing in a tubular furnace, wherein in the firing process, inert gas nitrogen is continuously introduced into the tubular furnace, the nitrogen flow is 70m L/min, then the firing temperature is increased to 700 ℃ under the condition that the temperature rising speed is 2.5 ℃/min, and the firing is carried out for 2 hours under the condition that the firing temperature is 700 ℃ to obtain a fired sample;
naturally cooling the fired sample to room temperature, and finally grinding the sample into powder to obtain porous carbon powder;
fifthly, mixing an activating agent with the porous carbon powder, and grinding the mixture in a mortar until the mixture is fully mixed to obtain a mixed sample;
the mass ratio of the activating agent to the porous carbon powder is 3: 1;
sixthly, placing the mixed sample in a covered alumina crucible, heating and activating in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the activation process, wherein the nitrogen flow is 50m L/min, heating the activation temperature to 800 ℃ under the condition that the heating rate is 5 ℃/min, and activating for 2 hours under the condition that the activation temperature is 800 ℃ to obtain activated porous carbon;
seventhly, naturally cooling the porous carbon to be activated to room temperature, and washing the porous carbon to be activated by using deionized water as a washing liquid until the washing liquid is neutral to obtain neutral porous carbon powder;
and eighthly, placing the neutral porous carbon powder in an oven for drying to obtain the porous carbon based on cotton.
The waste alcohol cotton is waste alcohol cotton in a chemical laboratory;
in the first step, the waste alcohol cotton is soaked in acetone for 24 hours in a ventilated place to obtain soaked alcohol cotton.
And drying in an oven in the second step, specifically drying for 24 hours at the temperature of 80 ℃.
And step eight, placing the neutral porous carbon powder in an oven for drying, specifically drying for 24 hours at the drying temperature of 80 ℃.
And the activating agent in the fifth step is potassium hydroxide.
The cotton-based porous carbon is used for adsorbing sulfamethoxazole in water.
The method for adsorbing sulfamethoxazole in water by using the cotton-based porous carbon comprises the following steps:
weighing porous carbon based on cotton, and adding the porous carbon into sulfamethoxazole solution according to the solid-to-liquid ratio of 1:10 to obtain mixed solution;
the concentration of the sulfamethoxazole solution is 0.5 mg/L;
secondly, placing the mixed solution in a shaking table, and adsorbing for 30min under the conditions that the shaking speed is 130r/min and the temperature of the shaking table is 25 ℃.
Sampling at intervals of 2m L during the adsorption process, and measuring the concentration of sulfamethoxazole in the solution to examine the adsorption effect of the porous carbon on the sulfamethoxazole.
Comparative experiment:
a preparation method of porous carbon based on cotton is carried out according to the following steps:
firstly, soaking waste alcohol cotton in acetone at a ventilated place to obtain soaked alcohol cotton;
secondly, washing the soaked alcohol cotton with deionized water, and then drying in an oven to obtain dried alcohol cotton;
thirdly, placing the dried alcohol cotton in an alumina crucible, and then firing in a tubular furnace, wherein in the firing process, inert gas nitrogen is continuously introduced into the tubular furnace, the nitrogen flow is 70m L/min, then the firing temperature is increased to 700 ℃ under the condition that the temperature rising speed is 2.5 ℃/min, and the firing is carried out for 2 hours under the condition that the firing temperature is 700 ℃ to obtain a fired sample;
naturally cooling the sample to be fired to room temperature, and finally grinding the sample into powder to obtain unactivated porous carbon;
the waste alcohol cotton is waste alcohol cotton in a chemical laboratory;
in the first step, the waste alcohol cotton is soaked in acetone for 24 hours in a ventilated place to obtain soaked alcohol cotton.
And drying in an oven in the second step, specifically drying for 24 hours at the temperature of 80 ℃.
The non-activated porous carbon is used for adsorbing pollutants in water by the following steps:
weighing unactivated porous carbon, and adding the unactivated porous carbon into sulfamethoxazole solution in a solid-to-liquid ratio of 1:10 to obtain mixed solution;
the concentration of the sulfamethoxazole solution is 0.5 mg/L;
secondly, placing the mixed solution in a shaking table, and adsorbing for 30min under the conditions that the shaking speed is 130r/min and the temperature of the shaking table is 25 ℃.
Sampling at intervals of 2m L during the adsorption process, and measuring the concentration of sulfamethoxazole in the solution to examine the adsorption effect of the porous carbon on the sulfamethoxazole.
FIG. 1 is an XRD pattern of unactivated porous carbon prepared by a comparative experiment; as can be seen from the figure, the (002) plane and the (100) plane of the graphitic carbon appear at diffraction angles of 27.5 ° and 43 °, respectively.
Fig. 2 is an XRD pattern of the cotton-based porous carbon prepared in example one; as can be seen from the figure, the characteristic diffraction peaks (002) crystal plane and (100) crystal plane of the graphite carbon still exist at the diffraction angles of 27.5 degrees and 43 degrees, and the peak intensity is enhanced, which shows that the degree of graphitization of the porous carbon is enhanced after the activation.
FIG. 3 is the BET test results, 1 for cotton-based porous carbon prepared in example one, 2 for unactivated porous carbon prepared in comparative experiment; as can be seen from the graph, the specific surface area of the activated porous carbon is greatly increased, and the specific surface area is 0.37m from the specific surface area without activation2The/g is increased to 1808.89m after activation2/g。
Fig. 4 is a graph of adsorption results on sulfamethoxazole, where 1 is porous carbon based on cotton prepared in the first embodiment, and 2 is non-activated porous carbon prepared in a comparative experiment, and it can be seen from the graph that compared with the non-activated porous carbon, the adsorption effect of the activated porous carbon on sulfamethoxazole is significantly improved, within 30min of adsorption time, the non-activated porous carbon only adsorbs nearly 5% of sulfamethoxazole, while the activated porous carbon can adsorb 97% of sulfamethoxazole when adsorbing for 2min, and the adsorption rate approaches 100% when adsorbing for 6 min.
Claims (10)
1. A preparation method of porous carbon based on cotton is characterized by comprising the following steps:
firstly, soaking cotton in acetone at a ventilated place to obtain soaked cotton;
secondly, washing the soaked cotton with deionized water, and then drying in an oven to obtain dried cotton;
thirdly, placing the dried cotton in an alumina crucible, then firing in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the firing process, wherein the nitrogen flow is 50m L/min-150 m L/min, then heating the firing temperature to 500-800 ℃ under the condition that the heating rate is 2 ℃/min-5 ℃/min, and firing for 0.5-5 h under the condition that the firing temperature is 500-800 ℃ to obtain a fired sample;
naturally cooling the fired sample to room temperature, and finally grinding the sample into powder to obtain porous carbon powder;
fifthly, mixing an activating agent with the porous carbon powder, and grinding the mixture in a mortar until the mixture is fully mixed to obtain a mixed sample;
the mass ratio of the activating agent to the porous carbon powder is (1-5) to 1;
placing the mixed sample in a covered alumina crucible, heating and activating in a tubular furnace, continuously introducing inert gas nitrogen into the tubular furnace in the activation process, wherein the nitrogen flow is 50m L/min-150 m L/min, then heating the activation temperature to 700-1000 ℃ under the condition that the heating rate is 2 ℃/min-5 ℃/min, and activating for 1-5 h under the condition that the activation temperature is 700-1000 ℃ to obtain activated porous carbon;
seventhly, naturally cooling the porous carbon to be activated to room temperature, and washing the porous carbon to be activated by using deionized water as a washing liquid until the washing liquid is neutral to obtain neutral porous carbon powder;
and eighthly, placing the neutral porous carbon powder in an oven for drying to obtain the porous carbon based on cotton.
2. The method for preparing porous carbon based on cotton according to claim 1, wherein in the first step, the cotton is soaked in acetone for 24 hours or more than 24 hours at a ventilated place to obtain soaked cotton.
3. The preparation method of porous carbon based on cotton according to claim 1, characterized in that in the second step, drying is carried out in an oven, specifically drying is carried out for 12-48 h at a temperature of 60-90 ℃; and step eight, placing the neutral porous carbon powder in a drying oven for drying, specifically drying for 12-24 h at the drying temperature of 60-100 ℃.
4. The method of claim 1, wherein the activating agent in step five is sodium hydroxide, potassium hydroxide or potassium carbonate.
5. The method for preparing cotton-based porous carbon according to claim 1, wherein the cotton in the first step is waste cotton or unused cotton.
6. The method for preparing porous carbon based on cotton according to claim 5, wherein the waste cotton is waste alcohol cotton.
7. The preparation method of porous carbon based on cotton according to claim 1, characterized in that in the sixth step, the mixed sample is placed in a covered alumina crucible, and then is heated and activated in a tubular furnace, during the activation, inert gas nitrogen is continuously introduced into the tubular furnace, the nitrogen flow is 50m L/min-100 m L/min, then the activation temperature is raised to 800 ℃ to 1000 ℃ under the condition that the temperature raising speed is 2 ℃ to 5 ℃ per min, and the activated porous carbon is activated for 2h to 5h under the condition that the activation temperature is 800 ℃ to 1000 ℃ to obtain the activated porous carbon.
8. Use of cotton-based porous carbon prepared according to claim 1, characterized in that the cotton-based porous carbon is used for adsorption of pollutants in water.
9. Use of porous carbon based on cotton according to claim 8, characterized in that the contaminants in the water are one or a mixture of several of sulfamethoxazole, sulfisoxazole, sulfadiazine, ciprofloxacin or tetracycline.
10. Use of cotton-based porous carbon according to claim 8, characterized in that the use of cotton-based porous carbon for the adsorption of pollutants in water is carried out in particular by the following steps:
weighing porous carbon based on cotton, and adding the porous carbon into water containing pollutants according to the mass ratio of solid to liquid of (1-2) to 10 to obtain mixed solution;
the concentration of the pollutants in the water containing the pollutants is 0.2 mg/L-2 mg/L;
placing the mixed solution in a shaking table, and adsorbing for 1-60 min under the conditions that the shaking speed is 120-140 r/min and the temperature of the shaking table is 15-45 ℃.
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