CN110803699A - Composite carbon material for seawater desalination and preparation method thereof - Google Patents
Composite carbon material for seawater desalination and preparation method thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
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- C—CHEMISTRY; METALLURGY
- 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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention discloses a composite carbon material for seawater desalination and a preparation method thereof, wherein the composite carbon material is composed of graphene and activated carbon, wherein the graphene is filled on the surface of the activated carbon; the preparation method comprises the steps of respectively preparing activated carbon and graphene oxide, carrying out ultrasonic reaction on the graphene oxide and the activated carbon, and then carrying out reduction reaction on the graphene oxide and glutathione. The composite carbon material has the advantages of large specific surface area, clear pore structure, simple preparation process, high product yield, low cost and high resource utilization rate, can provide a good ion transmission channel, and can be produced on a large scale; meanwhile, the composite carbon material has high capacitance, is applied to the deionization capacitor electrode material for seawater desalination, can improve the performance of deionization capacitance, and improves the seawater desalination efficiency.
Description
Technical Field
The invention belongs to the field of seawater desalination, and particularly relates to a composite carbon material for seawater desalination and a preparation method thereof.
Background
Data statistics show that the water resource on the earth is 1.4 x 1018m371% of the surface of the earth is covered with water. However, 98% of this water is salt water present in the ocean, inland sea and underground basins and cannot be drunk, and drinkable fresh water accounts for only about 2% of the total global water. With the development of economy and the progress of society, the demand of people for water is getting larger and larger, and fresh water resources become a worldwide problem due to the shortage of water resources, uneven space-time distribution, over-limit exploitation, and unregulated waste and pollution, and many countries begin to find new water sources. The active carbon has higher specific surface area, good conductivity and higher electric adsorption capacity, and has potential as an electrode of a deionization capacitor. Unfortunately, the capacitance performance of activated carbon on the market is not satisfactory, limiting the application to capacitors. Therefore, improving the synthesis process of the activated carbon becomes an effective means for popularizing the activated carbon for the capacitive deionization technology.
Disclosure of Invention
The purpose of the invention is as follows: the first purpose of the invention is to provide a composite carbon material for seawater desalination, which has large specific surface area, obvious gap structure and high specific capacitance;
the second purpose of the invention is to provide a preparation method of the composite carbon material.
The technical scheme is as follows: the composite carbon material for seawater desalination is composed of graphene and activated carbon, wherein the graphene is filled on the surface of the activated carbon.
According to the invention, the graphene and the activated carbon are compounded to prepare the composite carbon material, the activated carbon supports the three-dimensional structure of the graphene, the conductivity of the activated carbon is improved, and the N, S and O functional groups on the surface of the material improve the ion selective adsorption capacity.
The method for preparing the composite carbon material comprises the following steps:
(1) washing and drying a biomass carbon source, grinding into powder, and putting into a KOH solution to prepare a mixed solution; heating the mixed solution for 2-3 hours under the conditions of 1-3 Mpa and 100-120 ℃ to prepare a solid, washing and drying the solid, heating to 800-1000 ℃ in an argon atmosphere, preserving the heat for 2-3 hours, washing and drying to prepare activated carbon;
(2) mixing and heating graphite, potassium persulfate and phosphorus pentoxide according to the mass ratio of 1: 0.5-1.5 to 85-95 ℃, carrying out heat preservation reaction for 5-8 h for pre-oxidation, mixing and heating the pre-oxidized graphite, concentrated sulfuric acid and potassium permanganate to 30-40 ℃, carrying out heat preservation reaction for 3-5 h to obtain graphene oxide, carrying out ultrasonic reaction on the graphene oxide and active carbon according to the mass ratio of 1: 0.4-0.8 under the condition of 150-250W for 2-4 h to obtain a semi-finished product, and finally carrying out reduction reaction on the semi-finished product and glutathione according to the mass ratio of 1: 0.4-0.8 to obtain the active carbon.
Furthermore, in the step (1), the biomass carbon source can be lotus seedpod, lotus seed pod or lotus seed stem. The drying is carried out at the temperature of 70-80 ℃. The temperature rise rate is 4-8 ℃/min when the temperature rises to 800-1000 ℃.
Furthermore, in the step (2), the mass-to-volume ratio of the pre-oxidized graphite to the concentrated sulfuric acid is 1: 50-75, and the pre-oxidized graphite to the KMnO4The mass ratio of (A) to (B) is 1: 3-4.5.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the composite carbon material has the advantages of large specific surface area, clear pore structure, simple preparation process, high product yield, low cost and high resource utilization rate, can provide a good ion transmission channel, and can be produced on a large scale; meanwhile, the composite carbon material has high capacitance, is applied to the deionization capacitor electrode material for seawater desalination, can improve the performance of deionization capacitance, and improves the seawater desalination efficiency.
Drawings
FIG. 1 is a schematic structural diagram of a composite carbon material of the present invention;
FIG. 2 is a transmission electron micrograph of the composite carbon material of the present invention;
FIG. 3 is a graph showing the cyclic discharge efficiency of the composite carbon material prepared in example 1;
FIG. 4 is a graph of the cyclic discharge efficiency of the activated carbon prepared in example 1;
fig. 5 is a graph of the cyclic discharge efficiency of the reduced graphene oxide prepared in example 1;
FIG. 6 is a graph of the cyclic discharge efficiency of the composite carbon material prepared in example 2;
FIG. 7 is a graph of the cyclic discharge efficiency of the activated carbon prepared in example 2;
fig. 8 is a graph of the cyclic discharge efficiency of the reduced graphene oxide prepared in example 2;
FIG. 9 is a graph of the cyclic discharge efficiency of the composite carbon material prepared in example 3;
FIG. 10 is a graph of the cyclic discharge efficiency of the activated carbon prepared in example 3;
fig. 11 is a graph of the cyclic discharge efficiency of reduced graphene oxide prepared in example 3;
FIG. 12 is a graph comparing the desalination efficiencies of examples 1 to 3.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following examples.
The raw materials adopted by the invention can be purchased from the market.
Example 1 seedpod as a Biomass carbon Source
The method for preparing the composite carbon material comprises the following steps:
(1) removing lotus seeds from fresh lotus seedpod, washing with tap water, soaking in 3000ml beaker with deionized water, ultrasonically treating for 30min, drying in blast drying oven at 70 deg.C for 16h, and grinding into fine powder;
(2) weighing 4g of lotus powder, adding the lotus powder into a 250ml beaker, weighing 6mol of KOH, pouring the KOH into the 250ml beaker filled with 100ml of deionized water, and stirring and dissolving under ultrasonic to obtain a mixed solution;
(3) pouring the mixed solution into a 100ml high-pressure reaction kettle, screwing the mixed solution, putting the screwed mixed solution into an air-blast drying oven, heating the mixed solution for 2 hours under the conditions of 1.5Mpa and 120 ℃, cooling the mixed solution, pouring the cooled mixed solution into two 50ml centrifuge tubes, centrifuging the centrifuge tubes for three minutes at the revolution of 8000r/min, taking out the solid, and putting the solid into a vacuum drying oven to dry the solid for 12 hours at the temperature of 70 ℃;
(4) putting the dried material into a tubular furnace, introducing nitrogen, raising the temperature to 800 ℃ at the speed of 4 ℃/min, reacting for 2 hours at constant temperature, and taking out after cooling;
(5) putting the fired material into two 50ml centrifuge tubes, adding 20ml dilute hydrochloric acid solution, stirring with a glass rod, completely dispersing, and centrifuging at 9000r/min for 3 min; washing with deionized water by the same method, centrifuging for 4-5 times, finally checking to be neutral by pH test paper, and drying in an oven at 70 ℃ for 12h to obtain activated carbon;
(6) 2g of graphite, 1g of potassium persulfate and 1g of phosphorus pentoxide are mixed and placed in a three-neck flask, the mixture is heated to 80 ℃ in an oil bath and reacts at a constant temperature for 6 hours for pre-oxidation, and the pre-oxidation product is washed to be neutral by water;
(7) 1g of preoxidation product, 50ml of concentrated sulfuric acid and 3g of KMnO4Mixing, putting into a three-neck flask, heating to 35 ℃, keeping the temperature, reacting for 3 hours to obtain graphene oxide, and washing the graphene oxide to be neutral;
(8) mixing 0.5g of graphene oxide with 0.2 g of activated carbon, and carrying out ultrasonic treatment for 4 hours under the condition of 150W to obtain a semi-finished product;
(9) and (3) mixing 0.5g of the semi-product with 2g of glutathione, and heating in a water bath for 3 hours to obtain the composite material.
The structure of the composite carbon material prepared in this embodiment is shown in fig. 1 and fig. 2, and as can be seen from fig. 1 and fig. 2, graphene is filled on the surface of activated carbon, and has a clear structure and a uniform size, and can better provide an ion transmission channel and enhance the conductivity of the material.
Comparative examples 1 to 1
The method for preparing activated carbon of this comparative example includes the steps of:
(1) removing lotus seeds from fresh lotus seedpod, washing with tap water, soaking in 3000ml beaker with deionized water, ultrasonically treating for 30min, drying in blast drying oven at 70 deg.C for 16h, and grinding into fine powder;
(2) weighing 4g of lotus powder, adding the lotus powder into a 250ml beaker, weighing 6mol of KOH, pouring the KOH into the 250ml beaker filled with 100ml of deionized water, and stirring and dissolving under ultrasonic to obtain a mixed solution;
(3) pouring the mixed solution into a 100ml high-pressure reaction kettle, screwing the mixed solution, putting the screwed mixed solution into an air-blast drying oven, heating the mixed solution for 2 hours under the conditions of 1-3 Mpa and 120 ℃, cooling the mixed solution, pouring the cooled mixed solution into two 50ml centrifugal tubes, centrifuging the mixed solution for three minutes at the revolution speed of 8000r/min, taking the solid, and putting the solid into a vacuum drying oven to dry the solid for 12 hours at the temperature of 70 ℃;
(4) putting the dried material into a tubular furnace, introducing nitrogen, raising the temperature to 800 ℃ at the speed of 4 ℃/min, reacting for 2 hours at constant temperature, and taking out after cooling;
(5) putting the fired material into two 50ml centrifuge tubes, adding 20ml dilute hydrochloric acid solution, stirring with a glass rod, completely dispersing, and centrifuging at 9000r/min for 3 min; and then washing and centrifuging for 4-5 times by using deionized water by the same method, finally testing the neutral pH value by using pH test paper, and drying in an oven at 70 ℃ for 12h to obtain the activated carbon.
Comparative examples 1 to 2
The method for preparing graphene according to the comparative example includes the following steps:
(1) 2g of graphite, 1g of potassium persulfate and 1g of phosphorus pentoxide are mixed and placed in a three-neck flask, the mixture is heated to 80 ℃ in an oil bath and reacts at a constant temperature for 6 hours for pre-oxidation, and the pre-oxidation product is washed to be neutral by water;
(2) 1g of preoxidation product, 50ml of concentrated sulfuric acid and 3g of KMnO4Mixing, putting into a three-neck flask, heating to 35 ℃, keeping the temperature, reacting for 3 hours to obtain graphene oxide, and washing the graphene oxide to be neutral;
(3) and (3) mixing 0.5g of the semi-product with 2g of glutathione, and heating in a water bath for 3 hours to obtain the reduced graphene.
The results of the performance tests of the products prepared in example 1, comparative examples 1-1 and comparative examples 1-2 are shown in fig. 3 to 5, and it can be seen from fig. 3 to 5 that the capacitance of activated carbon is 220F/g, the capacitance of reduced graphene oxide is 210F/g, and the capacitance of the composite is 320F/g. The synergistic effect of the activated carbon and the redox graphene in the composite material is shown, and the specific capacity of the material is higher than that of the activated carbon and the redox graphene.
Example 2 shower nozzle stems as a Biomass carbon Source
The basic procedure is the same as in example 1, except that: the biomass carbon source is a lotus seed stem, the activation temperature is 200 ℃, and the heat preservation temperature of the tubular furnace is 500 ℃.
Comparative example 2-1
The basic procedure was the same as in comparative example 1-1, except that a shower stem was used as the biomass carbon source.
Comparative examples 2 to 2
The procedure was the same as in comparative examples 1-2.
The results of the performance tests of the products prepared in example 2, comparative example 2-1 and comparative example 2-2 are shown in fig. 6 to 8, and it can be seen from fig. 6 to 8 that the capacitance of the activated carbon is 210F/g, the capacitance of the reduced graphene oxide is 260F/g, and the capacitance of the composite is 330F/g. The synergistic effect of the activated carbon and the redox graphene in the composite material is shown, and the specific capacity of the material is higher than that of the activated carbon and the redox graphene.
Example 3 Lotus seed pod as Biomass carbon Source
The basic procedure is the same as in example 1, except that: the carbon source is lotus seed pod.
Comparative example 3-1
The basic procedure was the same as in comparative example 1-1, except that lotus seed pods were used as the biomass carbon source.
Comparative examples 3 to 2
The procedure was the same as in comparative examples 1-2.
The results of the performance tests of the products prepared in example 3, comparative example 3-1 and comparative example 3-2 are shown in fig. 9 to 11, and it can be seen from fig. 9 to 11 that the capacitance of the activated carbon is 240F/g, the capacitance of the reduced graphene oxide is 210F/g, and the capacitance of the composite is 340F/g. The synergistic effect of the activated carbon and the redox graphene in the composite material is shown, and the specific capacity of the material is higher than that of the activated carbon and the redox graphene.
Meanwhile, the composite materials prepared in example 1, example 2 and example 3 were tested for desalination efficiency, and the results are shown in fig. 12, from which it can be seen that: the desalting efficiency of example 1 is 35mg/g, the desalting efficiency of example 2 is 31mg/g, and the desalting efficiency of example 3 is 28mg/g, which are all higher than that of other commercial negative electrode materials of the capacitive deionization equipment.
Example 4 seedpod as a Biomass carbon Source
The method for preparing the composite carbon material comprises the following steps:
(1) removing lotus seeds from fresh lotus seedpod, washing with tap water, soaking in 3000ml beaker with deionized water, ultrasonically treating for 30min, drying in blast drying oven at 70 deg.C for 16h, and grinding into fine powder;
(2) weighing 4g of lotus powder, adding the lotus powder into a 250ml beaker, weighing 6mol of KOH, pouring the KOH into the 250ml beaker filled with 100ml of deionized water, and stirring and dissolving under ultrasonic to obtain a mixed solution;
(3) pouring the mixed solution into a 100ml high-pressure reaction kettle, screwing the mixed solution, putting the screwed mixed solution into a forced air drying oven, heating the mixed solution for 2 hours at the temperature of 2Mpa and 120 ℃, pouring the cooled mixed solution into two 50ml centrifuge tubes, centrifuging the centrifuge tubes for three minutes at the speed of 8000r/min, taking the solid, and putting the solid into a vacuum drying oven to dry the solid for 12 hours at the temperature of 70 ℃;
(4) putting the dried material into a tubular furnace, introducing nitrogen, raising the temperature to 1000 ℃ at the speed of 8 ℃/min, reacting for 2 hours at constant temperature, and taking out after cooling;
(5) putting the fired material into two 50ml centrifuge tubes, adding 20ml dilute hydrochloric acid solution, stirring with a glass rod, completely dispersing, and centrifuging at 9000r/min for 3 min; washing with deionized water by the same method, centrifuging for 4-5 times, finally checking to be neutral by pH test paper, and drying in an oven at 70 ℃ for 12h to obtain activated carbon;
(6) 2g of graphite, 1.5g of potassium persulfate and 1.5g of phosphorus pentoxide are mixed and placed in a three-neck flask, the mixture is heated to 80 ℃ in an oil bath and reacts for 8 hours at constant temperature for preoxidation, and the preoxidation product is washed to be neutral by water;
(7) 1g of preoxidation product, 75ml of concentrated sulfuric acid and 4.5g of KMnO4Mixing, putting into a three-neck flask, heating to 35 ℃, keeping the temperature, reacting for 6 hours to obtain graphene oxide, and washing the graphene oxide to be neutral;
(8) mixing 0.5g of graphene oxide with 0.4g of activated carbon, and carrying out ultrasonic treatment for 4 hours under the condition of 150W to obtain a semi-finished product;
(9) and (3) mixing 0.5g of the semi-product with 0.4g of glutathione, and heating in a water bath for 3 hours to obtain the composite material.
Example 5 Lotus seed pod as Biomass carbon Source
The method for preparing the composite carbon material comprises the following steps:
(1) removing lotus seeds from fresh lotus seedpod, washing with tap water, soaking in 3000ml beaker with deionized water, ultrasonically treating for 30min, drying in blast drying oven at 70 deg.C for 16h, and grinding into fine powder;
(2) weighing 4g of lotus powder, adding the lotus powder into a 250ml beaker, weighing 6mol of KOH, pouring the KOH into the 250ml beaker filled with 100ml of deionized water, and stirring and dissolving under ultrasonic to obtain a mixed solution;
(3) pouring the mixed solution into a 100ml high-pressure reaction kettle, screwing the mixed solution, putting the screwed mixed solution into a forced air drying oven, heating the mixed solution for 3 hours at 3Mpa and 1200 ℃, pouring the cooled mixed solution into two 50ml centrifuge tubes, centrifuging the centrifuge tubes for three minutes at the revolution of 8000r/min, taking the solid, and putting the solid into a vacuum drying oven to dry the solid for 12 hours at the temperature of 80 ℃;
(4) putting the dried material into a tubular furnace, introducing nitrogen, raising the temperature to 900 ℃ at the speed of 6 ℃/min, reacting for 3 hours at constant temperature, and taking out after cooling;
(5) putting the fired material into two 50ml centrifuge tubes, adding 20ml dilute hydrochloric acid solution, stirring with a glass rod, completely dispersing, and centrifuging at 9000r/min for 3 min; washing with deionized water by the same method, centrifuging for 4-5 times, finally checking to be neutral by pH test paper, and drying in a drying oven at 80 ℃ for 12 hours to obtain activated carbon;
(6) 2g of graphite, 3g of potassium persulfate and 3g of phosphorus pentoxide are mixed and placed in a three-neck flask, the mixture is heated to 95 ℃ in an oil bath and reacts for 5 hours at constant temperature for preoxidation, and the preoxidation product is washed to be neutral by water;
(7) 1g of preoxidation product, 60ml of concentrated sulfuric acid and 4g of KMnO4Mixing, putting into a three-neck flask, heating to 40 ℃, preserving heat, reacting for 5 hours to obtain graphene oxide, and washing the graphene oxide to be neutral;
(8) mixing 0.5g of graphene oxide with 0.3g of activated carbon, and carrying out ultrasonic treatment for 2 hours under the condition of 250W to obtain a semi-finished product;
(9) and (3) mixing 0.5g of the semi-product with 0.3g of glutathione, and heating in a water bath for 3 hours to obtain the composite material.
Claims (7)
1. A composite carbon material for seawater desalination is characterized in that: the composite carbon material is composed of graphene and activated carbon, wherein the graphene is filled on the surface of the activated carbon.
2. A method of preparing the composite carbon material of claim 1, comprising the steps of:
(1) washing and drying a biomass carbon source, grinding into powder, and putting into a KOH solution to prepare a mixed solution; heating the mixed solution for 2-3 hours under the conditions of 1-3 Mpa and 100-120 ℃ to prepare a solid, washing and drying the solid, heating to 800-1000 ℃ in an argon atmosphere, preserving the heat for 2-3 hours, washing and drying to prepare activated carbon;
(2) mixing and heating graphite, potassium persulfate and phosphorus pentoxide according to a mass ratio of 1: 0.5-1.5 to 80-95 ℃, carrying out a heat preservation reaction for 5-8 h for pre-oxidation, mixing and heating the pre-oxidized graphite, concentrated sulfuric acid and potassium permanganate to 30-40 ℃, carrying out a heat preservation reaction for 3-6 h to obtain graphene oxide, carrying out an ultrasonic reaction on the graphene oxide and activated carbon according to a mass ratio of 1: 0.4-0.8 under a condition of 150-250W for 2-4 h to obtain a semi-finished product, and finally carrying out a reduction reaction on the semi-finished product and glutathione according to a mass ratio of 1: 0.4-0.8 to obtain the composite material.
3. The method of making a composite carbon material of claim 2, wherein: in the step (1), the biomass carbon source is lotus seedpod, lotus seed pod or lotus seed stem.
4. The method of making a composite carbon material of claim 2, wherein: in the step (1), the drying is carried out at the temperature of 70-80 ℃.
5. The method of making a composite carbon material of claim 2, wherein: in the step (1), the heating rate of the temperature rise to 800-1000 ℃ is 4-8 ℃/min.
6. The method of making a composite carbon material of claim 2, wherein: in the step (2), the mass-to-volume ratio of the pre-oxidized graphite to concentrated sulfuric acid is 1: 50-75.
7. The method of making a composite carbon material of claim 2, wherein: in the step (2), the pre-oxidized graphite is mixed with KMnO4The mass ratio of (A) to (B) is 1: 3-4.5.
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