CN111558362A - Preparation process of graphene activated carbon composite material - Google Patents
Preparation process of graphene activated carbon composite material Download PDFInfo
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- CN111558362A CN111558362A CN202010433307.6A CN202010433307A CN111558362A CN 111558362 A CN111558362 A CN 111558362A CN 202010433307 A CN202010433307 A CN 202010433307A CN 111558362 A CN111558362 A CN 111558362A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28066—Surface area, e.g. B.E.T specific surface area being more than 1000 m2/g
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/182—Graphene
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention discloses a preparation process of a graphene activated carbon composite material, and relates to the field of purification materials. The technical key points are as follows: the method comprises the following steps: step one, taking graphite, and preparing graphene oxide by adopting an improved Hummers method, wherein in the preparation process, the mass ratio of the graphite to concentrated sulfuric acid is (10-30): 100, obtaining graphene oxide/concentrated sulfuric acid dispersion liquid after complete reaction; step two, uniformly mixing 10-40 parts by weight of saccharide powder, 5-20 parts by weight of water and 10-20 parts by weight of sodium peroxide, adding the mixture into the graphene oxide/concentrated sulfuric acid dispersion liquid obtained in the step one, and continuously stirring to obtain a viscous paste; step three, dehydrating the viscous paste obtained in the step two, and calcining the product at 900-950 ℃ for 4-10 hours; the product is washed to be neutral after being cooled, and the graphene/active carbon composite adsorbent can be obtained.
Description
Technical Field
The invention relates to the field of purification materials, in particular to a preparation process of a graphene activated carbon composite material.
Background
Since the preparation of graphene materials in 2004 by anderley K haim (andrek. geim) of manchester university, uk, and the like, graphene materials have received wide attention due to their unique structures and optoelectronic properties. Single layer graphene has many attractive properties, for example: (1) high strength, young's modulus, breaking strength; (2) high thermal conductivity; (3) high conductivity, high carrier transport rate; (4) high specific surface area.
Among them, the ultra-high specific surface area makes it receive a great deal of attention in the field of adsorption materials. The graphene aerogel prepared by the assembly method has an intercommunicated pore structure and a large specific surface area, and is a research hotspot of the existing graphene adsorption material. But it is difficult to use it alone as an adsorbent material because of its poor mechanical properties and difficult structure retention.
The activated carbon is the most commonly used adsorbing material at present, and has a developed microporous structure, a huge specific surface area, excellent adsorption performance and good acid and alkali resistance. Many researchers have attempted to complex activated carbon with graphene in recent years.
For example, chinese patent publication No. CN103723723B discloses a method for preparing graphene modified activated carbon, which comprises using traditional wood or straw activated carbon as a raw material, matching with graphene with specific parameters, activating in a deionized water solution at high temperature, filtering, and drying to obtain graphene modified activated carbon. The graphene modified activated carbon has a mass specific capacitance of more than 290F/g and a volume specific capacitance of 185F/cm2The method is suitable for manufacturing the super capacitor.
Also, for example, chinese patent publication No. CN104118874B discloses an activated carbon/graphene composite and a method for preparing the same. Uniformly mixing 45-90% of biomass, 5-50% of carbon nitrogen compound and 5-10% of transition metal-containing compound by mass; heating the mixed raw materials at 300-500 ℃ for 2-5 h to obtain a gray block material with a fluffy structure; and heating the block material in a protective gas atmosphere at 600-900 ℃ for 5-60 min to obtain the activated carbon/graphene compound. The specific capacitance composite electrode material of the active carbon/graphene composite material meets the requirements, and is suitable for application in the field of electrochemistry.
Similar to the above-mentioned activated carbon/graphene composite in the prior art, the following defects exist: the highest specific surface area which can be reached after the active carbon and the graphene are compounded can only reach 2000m2(ii)/g, the specific surface area cannot be further increased.
Therefore, a new solution is needed to solve the above problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation process of a graphene activated carbon composite material, which has the advantages that the produced graphene/activated carbon composite adsorbent has extremely high porosity and extremely high specific surface area.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation process of a graphene activated carbon composite material comprises the following steps:
taking 10-30 parts by weight of graphite, and preparing graphene oxide by adopting an improved Hummers method, wherein in the preparation process, the mass ratio of the graphite to concentrated sulfuric acid is (10-30): 100, obtaining graphene oxide/concentrated sulfuric acid dispersion liquid after complete reaction;
step two, uniformly mixing 10-40 parts by weight of saccharide powder, 5-20 parts by weight of water and 10-20 parts by weight of sodium peroxide, adding the mixture into the graphene oxide/concentrated sulfuric acid dispersion liquid obtained in the step one, and continuously stirring to obtain a viscous paste;
step three, dehydrating the viscous paste obtained in the step two at the temperature of 200-450 ℃, then putting the product into a tube furnace, and heating to 900-950 ℃ in a nitrogen atmosphere to calcine for 4-10 hours; and (4) washing the product to be neutral after cooling to obtain the graphene/activated carbon composite adsorbent.
By adopting the technical scheme, the concentrated sulfuric acid which needs to be removed after the preparation of the graphene oxide is finished is directly utilized. Firstly, in the second step, the reaction of concentrated sulfuric acid and saccharide powder not only can consume redundant concentrated sulfuric acid, but also can form a porous carbon skeleton wrapped by oxidized graphene, and a composite structure is formed in situ, so that a porous skeleton with high porosity is generated preliminarily.
Secondly, in step two, water is mixed with Na2O2NaOH and hydrogen peroxide (H) are generated in the first-stage reaction2O2) In which H is2O2The graphene/activated carbon composite adsorbent is a good activating agent, has a good activating effect on activated carbon, and can greatly improve the molding porosity of the graphene/activated carbon composite adsorbent.
Furthermore, water and Na2O2Will generate oxygen (i.e. H) in the second reaction2O2Is decomposed into water and oxygen), and the oxygen in the product can impact the porous framework to form pores, so that the porosity of the porous framework is further improved. Meanwhile, water in the secondary reaction product can be mixed with the original water and reacts with concentrated sulfuric acid to generate a large amount of heat, so that the system temperature is increased, and H is accelerated2O2The decomposition generates oxygen, the impact pore-forming of the oxygen is accelerated, and the molding porosity of the porous framework is further improved.
Then, in the second step, water and Na2O2The reaction of (2) can generate NaOH, and the NaOH can be neutralized with redundant concentrated sulfuric acid, so that the subsequent operation of cleaning the concentrated sulfuric acid can be omitted.
Finally, as NaOH is also a good activating agent, after the neutralization reaction in the second step, redundant NaOH can further activate the porous framework in the third step, and the reaction mechanism is as follows: the carbon consumed in the activation process mainly generates sodium carbonate, and at about 900 ℃, the metallic sodium (boiling point 883 ℃) reduced by the carbon can be separated out, the vapor of the metallic sodium continuously enters between layers formed by carbon atoms for activation, and the two reactions enable the product to further obtain a large specific surface area.
Therefore, under the synergistic effect of the multiple reaction mechanisms, the produced graphene/activated carbon composite adsorbent has extremely high porosity and extremely high specific surface area, and experiments show that the specific surface area can reach 2600m2More than g.
More preferably, in the first step, the saccharide powder is one of xylose, sucrose, glucose, fructose, lactose, starch and cellulose.
By adopting the technical scheme, xylose, sucrose, glucose, fructose, lactose, starch and cellulose are all organic matters and can be used as a carbon skeleton to form a porous carbon skeleton coated by graphene oxide.
More preferably, the pH of the viscous paste obtained in the second step is controlled to be 8-9.
By adopting the technical scheme, at the moment, the NaOH is excessive, and the NaOH can obtain more sodium vapor after being subjected to high temperature in the third step, so that the product can obtain larger specific surface area.
More preferably, in the second step, 1-3 parts by weight of 50% sodium chloride solution is further added to the graphene oxide/concentrated sulfuric acid dispersion liquid.
By adopting the technical scheme, the sodium chloride is neutral, and the porous framework activated by NaOH cannot be influenced; meanwhile, sodium chloride can provide sodium ions, so that the amount of sodium vapor generated after sodium is reduced is increased, and the activation efficiency is improved; and the sodium chloride solution contains water, so that the water quantity in the activation process can be provided, and the complete activation of the porous framework is ensured.
More preferably, in the first step, the mass ratio of the graphite to the concentrated sulfuric acid is (20-25): 100.
by adopting the technical scheme, the graphene/activated carbon composite adsorbent has higher specific surface area in the proportion.
More preferably, in the second step, the sugar powder: water: the ratio of sodium peroxide to sodium peroxide is 2:1: 1.
By adopting the technical scheme, the graphene/activated carbon composite adsorbent has higher specific surface area in the proportion.
More preferably, in step three, the dehydration temperature of the viscous paste is 300 ℃.
By adopting the technical scheme, the dehydration can be rapidly carried out at the temperature, sodium vapor can not be generated, and the stability is high.
More preferably, in step three, the time for calcining the viscous paste in the tube furnace is 7 hours.
By adopting the technical scheme, the graphene/activated carbon composite adsorbent with the maximum yield can be obtained after 7 hours of calcination.
In summary, compared with the prior art, the invention has the following beneficial effects:
graphene oxide was prepared by the Hummers method and graphene oxide/concentrated sulfuric acid dispersion was mixed with saccharide powder, water, and sodium peroxide during the preparation. Firstly, the reaction of concentrated sulfuric acid and saccharide powder can consume redundant concentrated sulfuric acid, and simultaneously, a porous carbon skeleton coated by oxidized graphene can be formed.
Secondly, in step two, water is mixed with Na2O2NaOH and hydrogen peroxide (H) are generated in the first-stage reaction2O2) In which H is2O2The graphene/activated carbon composite adsorbent is a good activating agent, has a good activating effect on activated carbon, and can greatly improve the molding porosity of the graphene/activated carbon composite adsorbent.
Furthermore, water and Na2O2Will generate oxygen (i.e. H) in the second reaction2O2Is decomposed into water and oxygen), and the oxygen in the product can impact the porous framework to form pores, so that the porosity of the porous framework is further improved. Meanwhile, water in the secondary reaction product can be mixed with the original water and reacts with concentrated sulfuric acid to generate a large amount of heat, so that the system temperature is increased, and H is accelerated2O2The decomposition generates oxygen, the impact pore-forming of the oxygen is accelerated, and the molding porosity of the porous framework is further improved.
Then, in the second step, water and Na2O2The reaction of (2) can generate NaOH, and the NaOH can be neutralized with redundant concentrated sulfuric acid, so that the subsequent operation of cleaning the concentrated sulfuric acid can be omitted.
Finally, as NaOH is also a good activating agent, after the neutralization reaction in the second step, redundant NaOH can further activate the porous framework in the third step, and the reaction mechanism is as follows: the carbon consumed in the activation process mainly generates sodium carbonate, and at about 900 ℃, the metallic sodium (boiling point 883 ℃) reduced by the carbon can be separated out, the vapor of the metallic sodium continuously enters between layers formed by carbon atoms for activation, and the two reactions enable the product to further obtain a large specific surface area.
Therefore, under the synergistic effect of the multiple reaction mechanisms, the produced graphene/activated carbon composite adsorbent has extremely high porosity and extremely high specific surface area.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1: a preparation process of a graphene activated carbon composite material is prepared by the following steps:
taking 10 parts by weight of graphite, and preparing graphene oxide by adopting an improved Hummers method, wherein in the preparation process, the mass ratio of the graphite to concentrated sulfuric acid is 10: 100, obtaining graphene oxide/concentrated sulfuric acid dispersion liquid after complete reaction;
step two, uniformly mixing 10 parts by weight of saccharide powder, 5 parts by weight of water and 10 parts by weight of sodium peroxide, adding the mixture into the graphene oxide/concentrated sulfuric acid dispersion liquid obtained in the step one, and continuously stirring to obtain a viscous paste;
step three, dehydrating the viscous paste obtained in the step two at the temperature of 200 ℃, then putting the product into a tube furnace, and heating to 900 ℃ in the nitrogen atmosphere to calcine for 10 hours; and (3) washing the product to be neutral after cooling, and then drying the product in an oven to obtain the graphene/activated carbon composite adsorbent.
In this embodiment, the saccharide powder is glucose.
Example 2: a preparation process of a graphene activated carbon composite material is prepared by the following steps:
step one, taking 20 parts by weight of graphite, and preparing graphene oxide by adopting an improved Hummers method, wherein in the preparation process, the mass ratio of the graphite to concentrated sulfuric acid is 20: 100, obtaining graphene oxide/concentrated sulfuric acid dispersion liquid after complete reaction;
step two, uniformly mixing 20 parts by weight of saccharide powder, 10 parts by weight of water and 15 parts by weight of sodium peroxide, adding the mixture into the graphene oxide/concentrated sulfuric acid dispersion liquid obtained in the step one, and continuously stirring to obtain a viscous paste;
step three, dehydrating the viscous paste obtained in the step two at the temperature of 300 ℃, then putting the product into a tubular furnace, and heating to 950 ℃ to calcine for 7 hours in the nitrogen atmosphere; and (3) washing the product to be neutral after cooling, and then drying the product in an oven to obtain the graphene/activated carbon composite adsorbent.
In this embodiment, the saccharide powder is glucose.
Example 3: a preparation process of a graphene activated carbon composite material is prepared by the following steps:
step one, taking 30 parts by weight of graphite, and preparing graphene oxide by adopting an improved Hummers method, wherein in the preparation process, the mass ratio of the graphite to concentrated sulfuric acid is 30: 100, obtaining graphene oxide/concentrated sulfuric acid dispersion liquid after complete reaction;
step two, uniformly mixing 40 parts by weight of saccharide powder, 20 parts by weight of water and 20 parts by weight of sodium peroxide, adding the mixture into the graphene oxide/concentrated sulfuric acid dispersion liquid obtained in the step one, and continuously stirring to obtain a viscous paste;
step three, dehydrating the viscous paste obtained in the step two at the temperature of 450 ℃, then putting the product into a tubular furnace, and heating to 950 ℃ to calcine for 4 hours in the nitrogen atmosphere; and (3) washing the product to be neutral after cooling, and then drying the product in an oven to obtain the graphene/activated carbon composite adsorbent.
In this embodiment, the saccharide powder is glucose.
Example 4: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3 in that the saccharide powder in the embodiment is xylose.
Example 5: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3 in that the saccharide powder in this embodiment is sucrose.
Example 6: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3 in that the saccharide powder in the embodiment is fructose.
Example 7: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3 in that the saccharide powder in this embodiment is lactose.
Example 8: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3 in that the saccharide powder in this embodiment is starch.
Example 9: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3 in that the saccharide powder in this embodiment is cellulose.
Example 10: the difference between the preparation process of the graphene activated carbon composite material and the embodiment 3 is that the thick paste obtained in the step two is sampled, a centrifugal separator is used for centrifuging, then supernatant is taken, pH test paper is used for testing the pH of the supernatant, and concentrated sulfuric acid and NaOH are used for adjusting the pH of the thick paste, so that the pH of the supernatant in the sampling is 8.
Example 11: the difference between the preparation process of the graphene activated carbon composite material and the embodiment 3 is that the thick paste obtained in the step two is sampled, a centrifugal separator is used for centrifuging, then supernatant is taken, pH of the supernatant is tested by using a pH test paper, and the pH of the thick paste is adjusted by concentrated sulfuric acid and NaOH, so that the pH of the supernatant in the sampling is 9.
Example 12: a preparation process of a graphene activated carbon composite material, which is different from that in the embodiment 3, in the second step, 1 part by weight of 50% sodium chloride solution is added into the graphene oxide/concentrated sulfuric acid dispersion liquid, and the sodium chloride solution is added together with water.
Example 13: a preparation process of a graphene activated carbon composite material, which is different from that in embodiment 3, is different from that in embodiment 3 in that in the second step, 3 parts by weight of 50% sodium chloride solution is further added into the graphene oxide/concentrated sulfuric acid dispersion liquid, and the sodium chloride solution is added together with water.
Comparative example 1: a difference between the graphene activated carbon composite material and example 3 is that sodium peroxide is not added in the second step in this example.
Comparative example 2: the graphene modified activated carbon is prepared according to the first embodiment of the Chinese patent with the granted patent publication number of CN 103723723B.
Comparative example 3: the graphene modified activated carbon is prepared according to the first embodiment of the Chinese patent with the granted patent publication number of CN 107051381B.
Test samples: the composite materials obtained in examples 1 to 13 were used as test samples 1 to 13, and the composite materials obtained in comparative examples 1 to 3 were used as control samples 1 to 3.
Testing specific surface area and pore volume test
The test method comprises the following steps: the specific surface areas and pore volumes of the test samples 1 to 13 and the control samples 1 to 3 were measured by the BET method. The maximum 2 values and the minimum 2 values of each group were discarded and the rest were averaged.
And (3) test results: as shown in table 1.
TABLE 1 test results of test samples 1-13 and control samples 1-3
And (3) data analysis: as can be seen from comparison of the test samples 1 to 13 with the control samples 1 to 3, the control sample 1, to which no sodium peroxide was added, had a specific surface area of 1416m2In g, comparable to the control sample 3 of the prior art. The test samples 1 to 13 to which sodium peroxide was added had a minimum specific surface area of 2664m2The ratio of the graphene/activated carbon composite adsorbent to the sodium peroxide is greatly higher than that of a control sample 1 without the sodium peroxide and that of control samples 2-3 in the prior art, and the result shows that the graphene/activated carbon composite adsorbent produced by the method has extremely high porosity and extremely high specific surface area under the synergistic effect of multiple reaction mechanisms in the scheme.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (8)
1. A preparation process of a graphene activated carbon composite material is characterized by comprising the following steps:
taking 10-30 parts by weight of graphite, and preparing graphene oxide by adopting an improved Hummers method, wherein in the preparation process, the mass ratio of the graphite to concentrated sulfuric acid is (10-30): 100, obtaining graphene oxide/concentrated sulfuric acid dispersion liquid after complete reaction;
step two, uniformly mixing 10-40 parts by weight of saccharide powder, 5-20 parts by weight of water and 10-20 parts by weight of sodium peroxide, adding the mixture into the graphene oxide/concentrated sulfuric acid dispersion liquid obtained in the step one, and continuously stirring to obtain a viscous paste;
step three, dehydrating the viscous paste obtained in the step two at the temperature of 200-450 ℃, then putting the product into a tube furnace, and heating to 900-950 ℃ in a nitrogen atmosphere to calcine for 4-10 hours; and (4) washing the product to be neutral after cooling to obtain the graphene/activated carbon composite adsorbent.
2. The preparation process of the graphene-activated carbon composite material according to claim 1, wherein in the first step, the saccharide powder is one of xylose, sucrose, glucose, fructose, lactose, starch and cellulose.
3. The preparation process of the graphene-activated carbon composite material according to claim 1, wherein the pH of the viscous paste obtained in the second step is controlled to be 8-9.
4. The preparation process of the graphene activated carbon composite material according to claim 3, wherein in the second step, 1-3 parts by weight of 50% sodium chloride solution is further added into the graphene oxide/concentrated sulfuric acid dispersion liquid.
5. The preparation process of the graphene activated carbon composite material according to claim 1, wherein in the first step, the mass ratio of graphite to concentrated sulfuric acid is (20-25): 100.
6. the preparation process of the graphene-activated carbon composite material according to claim 1, wherein in the second step, the sugar powder is prepared from the following components in parts by weight: water: the ratio of sodium peroxide to sodium peroxide is 2:1: 1.
7. The preparation process of the graphene-activated carbon composite material according to claim 1, wherein in the third step, the dehydration temperature of the viscous paste is 300 ℃.
8. The preparation process of the graphene-activated carbon composite material according to claim 7, wherein in the third step, the calcination time of the viscous paste in a tube furnace is 7 hours.
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| CN114591779A (en) * | 2022-03-03 | 2022-06-07 | 江苏双江能源科技股份有限公司 | Degradable emulsified natural ester lubricating material and preparation method thereof |
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| CN114591779A (en) * | 2022-03-03 | 2022-06-07 | 江苏双江能源科技股份有限公司 | Degradable emulsified natural ester lubricating material and preparation method thereof |
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Application publication date: 20200821 |