CN109179386B - Low-degree graphene oxide nanosheet layer powder and preparation method and application thereof - Google Patents
Low-degree graphene oxide nanosheet layer powder and preparation method and application thereof Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract
Graphite powder, an oxidant and a dispersing aid are mixed and ground to prepare the few-lamella large-size low-oxidation-degree graphene oxide nanosheet powder, the thickness of the obtained dry-powder-shaped nano low-oxidation-degree graphene nanosheet is 2.35-2.75 nm, the lamella plane size is 1.3-2.5 mu m, the oxygen content is 8.5-12.8%, and the specific surface area is 261-287 m2The concrete has the advantages that the mixing amount is 1.5-3.5% of the mass of the cement powder, the compressive strength, the flexural strength and the heat conductivity coefficient of the cement-based material at the age of 28 days are respectively improved by not less than 39%, 54% and 300% compared with a reference sample, and the anti-penetration, anti-freezing and anti-carbonization capabilities of the concrete reach the best level. The preparation method has the advantages of cheap and easily obtained materials, reasonable process route, convenient operation, no pollution in the preparation process, remarkable social and economic benefits and the like.
Description
Technical Field
The invention relates to a graphene oxide nano material, in particular to a preparation method and application of low-degree graphene oxide nano lamellar powder prepared from graphite powder by adopting a ball milling method.
Technical Field
The graphene oxide is a nanoscale lamellar material, has a structure and performance similar to those of graphene, has a large specific surface area, an ultrastrong mechanical property, a good heat-conducting property and a nanometer effect, and is widely applied to the aspects of adsorption, catalysis, biological analysis and detection, medical carriers, photoelectric materials, composite materials and the like. The preparation method of the graphene oxide comprises three methods, namely Brodie, Staudenmaier and Hummers, and the preparation principle is that graphite is treated by inorganic strong protonic acid such as concentrated sulfuric acid, fuming nitric acid and the like, small molecules of strong acid are inserted between graphite layers, and then the graphite layers are oxidized by strong oxidants such as potassium permanganate and potassium chlorate. The Hummers method which is most commonly used at present has the advantages that the graphene oxide with high oxidation degree can be obtained, and the oxidation degree and the lamella size can be regulated and controlled. However, these methods have disadvantages of low efficiency, high pollution, and high amount of waste acid water, resulting in high price of graphene oxide. Meanwhile, different application fields have different requirements on the structure of the graphene oxide, so that the research and development of the graphene oxide which is high in efficiency, low in cost and low in pollution and is suitable for the requirements of the application fields is a research hotspot and an urgent need technology at present.
At present, the application of graphene oxide in cement-based composite materials is valued by people, the main effect of the graphene oxide in the use of the cement-based materials is to regulate and control the structure and aggregation state structure of cement hydration products through the template effect of graphene oxide nanosheets, promote the formation of a regular, uniform and compact structure of the cement-based materials, improve the strength and toughness of the cement-based materials, and reduce or eliminate the problems of cracks, leakage and the like caused by nonuniform shrinkage and expansion of the structure, the graphene oxide with high oxidation degree (oxygen content is more than 30%) is required in this respect, and the graphene oxide is generally prepared by a Hummers method. The main problems of the cement-based materials are cracks and brittleness, the main reason of the cracks is the cracks caused by the difficulty in dissipating the hydration heat of the cement, the heat conductivity coefficient of the concrete is about 1.6W/(m.K), the heat conductivity coefficient of the metal copper is 401W/(m.K), and the heat conductivity coefficient of the water at 27 ℃ is 0.6084W/(m.K). The graphene is the heat conduction material with the best heat conduction performance at present, the heat conduction coefficient reaches 5300W/(m.K), and the graphene is doped to improve the heat conduction coefficient of concrete and improve the dispersion of cement hydration heat so as to eliminate cracks caused by hydration heat. However, graphene is a hydrophobic nano material and cannot be doped and uniformly dispersed in a cement matrix to form good uniform dispersion, and the graphene oxide nanosheet layer has hydrophilicity and can be doped in the cement matrix in the mixing preparation process of concrete. The thermal conductivity of the graphene oxide is reduced compared with that of the graphene due to partial damage of the hexagonal honeycomb crystal structure of the graphene oxide in the oxidation process, and the thermal conductivity of graphene oxide films with 35.21% and 16.21% of oxygen content is 36W/(m.K) and 373W/(m.K) respectively, because the oxidant generates larger damage to the two-dimensional perfect crystal structure of the graphene in the preparation process of the Hummers method, and the thermal resistance of the graphene oxide films is large due to more oxygen-containing groups and small sizes on the sheet layer. The graphene oxide is used for regulating and controlling the oxidation degree of a hydration product structure in a cement-based material, the doping amount is about 0.03% generally, the doping amount is small, a continuous heat conduction path cannot be formed, and the influence on the heat conduction coefficient of the cement-based material is small. In order to improve the heat conductivity of the cement-based material, the doping amount of the graphene oxide needs to be increased, and the problem of environmental pollution and price caused by the preparation of the graphene oxide by the Hummers method cannot be realized. Therefore, a new preparation method of graphene oxide with low oxidation degree must be sought.
Disclosure of Invention
The invention aims to provide low-degree graphene oxide nanosheet layer powder which is low in price, high in production efficiency and free of pollution and can be produced in a large scale, and a preparation method and application thereof.
In order to achieve the purpose, the invention provides a preparation method of low-degree graphene oxide nanosheet powder, which comprises the steps of putting 90-120 parts by mass of graphite powder, 6-9 parts by mass of grinding aid and 8-12 parts by mass of dispersing aid into a ball milling tank, mixing and grinding for 1 hour, adding 14-16 parts by mass of oxidant and 2-3 parts by mass of oxidation aid, and continuously grinding for 20 hours to obtain the low-degree graphene oxide nanosheet powder.
The particle size of the graphite powder is 13-15 mu m, and the carbon content is not less than 99.5%.
The oxidant is prepared by mixing potassium chlorate, potassium persulfate and potassium dichromate according to the mass ratio of 5:5: 6.
The oxidation assistant is lead dioxide or cobalt trifluoride.
The dispersing auxiliary agent is a powdery polycarboxylic acid water reducing agent, the content of the solid polycarboxylic acid water reducing agent is not less than 99.5%, the water content is not more than 2%, the fineness is that the average particle size is 35 mu m, and the water reducing rate is not less than 30%.
The grinding aid is prepared by mixing silicon powder and steel slag powder according to the mass ratio of 1:2, wherein the particle size of the silicon powder is 2-10 mu m, and the specific surface area is not less than 3000m2/kg, the content of silicon dioxide is more than 90 percent; the steel slag powder is obtained by grinding slag produced by a steel plant, the particle size is 2-10 mu m, and the specific surface area is not less than 3000m2Per kg, the sulfur trioxide content is not more than 4.0 percent.
The grinding equipment is a high-energy planetary ball mill, the ball milling tank is a stainless steel tank, grinding balls are GCr15 super-hardness alloy grinding balls, the ball material ratio is 8:1, and the ball milling rotating speed is 300 r/min.
The thickness of the low-degree graphene oxide nanosheet powder sheet layer prepared by the preparation method is 2.35-2.75 nm, the plane size of the sheet layer is 1.3-2.5 mu m, the oxygen content is 8.5-12.8%, and the specific surface area is 261-287 m2The thermal conductivity coefficient is 1326-1852W/(m.K).
According to the application of the low-degree graphene oxide nanosheet layer powder prepared by the preparation method, according to the cement-based material preparation method, the doping amount of the low-degree graphene oxide nanosheet layer powder is 1.5-3.5% of the mass of the cement powder, the low-degree graphene oxide nanosheet layer powder is doped in the mixing process and uniformly stirred, and the compressive strength, the flexural strength and the heat conductivity coefficient of the cement-based material in the age of 28 days are respectively improved by not less than 39%, 54% and 300% compared with those of a control sample.
According to the invention, the graphene oxide nano lamellar powder with few lamellar layers, large size, relatively complete two-dimensional crystal structure, high heat conduction and electric conduction coefficient is prepared by grinding the mixture of the graphite powder, the oxidant, the oxidation assistant and the dispersing assistant, and the graphene oxide nano lamellar powder has the advantages of low price, high production efficiency and no pollution, can be produced in large quantities, can be doped into a large amount of cement-based materials, improves the heat conduction performance of the cement-based materials, and eliminates cracks caused by uneven dispersion of cement hydration heat.
The method comprises the steps of mixing graphite powder with an oxidant and a dispersing auxiliary agent, and promoting the graphite to generate physical and chemical changes under the action of mechanical force in the grinding process to obtain few-lamella large-size low-degree graphene oxide nano-lamella powder, wherein the lamella thickness of the powder is 2.35-2.75 nm, the plane size of the powder is 1.3-2.5 mu m, and meanwhile, a small amount of chemical groups such as carboxyl, hydroxyl and epoxy groups are generated on the lamella and can be compatible with a water phase and uniformly dispersed in the powder. The preparation method has the advantages of low environmental pollution, low price, large production, capability of increasing the mixing amount in the cement matrix, realization of the functions of strengthening and toughening and improving the cement hydration heat dispersion of the cement matrix, easy obtainment of materials, reasonable process route, convenient operation, no pollution in the preparation process, low price and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method has the advantages that few-sheet large-size low-degree graphene oxide nano-sheet powder is efficiently prepared, the pollution in the preparation process is small, the prepared low-degree graphene oxide nano-sheet powder is low in price compared with a Hummers method, and the method is suitable for large-scale preparation and production and can be applied to cement-based materials with large mixing amount.
(2) The heat conductivity of the cement-based material is obviously improved, the hydration heat of the cement can be conducted and eliminated in time, and cracks generated due to uneven aggregation and dispersion of the hydration heat are eliminated. The graphene oxide lamellar powder obtained by the method has good heat conductivity, the heat conductivity coefficient is 1326-1852W/(m.K), the heat conductivity coefficient of concrete can be improved after the graphene oxide lamellar powder is doped into a cement matrix, heat generated by cement hydration can be dispersed in time, and cracks caused by untimely and uneven diffusion of hydration heat are eliminated.
(3) The low-degree graphene oxide nanosheet powder has the obvious effects of enhancing and toughening, has the filling effect and the nanometer size effect in a cement matrix, has a strong acting force with the cement matrix, and has the capability of promoting the cement-based material to form a uniform and compact structure. Meanwhile, active oxygen-containing groups on the graphene oxide lamella can participate in cement hydration reaction, and the graphene oxide lamella itself becomes a part of a cement matrix and a structure, so that the effects of strengthening and toughening are exerted.
(4) The method has no pollution in the production process, the graphene oxide lamellar powder is prepared from the graphite powder by adopting a dry ball milling method, the added graphite powder, the oxidant, the oxidation auxiliary agent, the dispersing auxiliary agent and the like are all converted into products, and no waste gas, waste water or waste residue is generated.
(5) The graphene oxide prepared by the method is low in price and suitable for large-scale use in the production of cement-based materials. The cost of the graphene oxide prepared by the Hummers method is about 30 ten thousand yuan/ton, the cost of the graphene oxide prepared by the method is about 1.5 ten thousand yuan/ton, if the graphene oxide is doped according to 1.5-3.5% of the amount of cement powder, the cost of the graphene oxide prepared by the Hummers method is about 2025-4725 yuan calculated according to 450 kg of cement in each cubic meter of concrete, and the cost of the graphene oxide lamellar powder prepared by the ball milling method is about 101.25-236.25 yuan, so the price advantage of the method is obvious.
Detailed Description
The present invention is described in detail below with reference to specific embodiments so that the advantages of the present invention can be more easily understood by those skilled in the art, but is not intended to limit the scope of the present invention.
Example 1:
putting 90 parts of graphite powder, 6 parts of grinding aid and 8 parts of dispersing aid into a ball milling tank for mixing and grinding according to the mass parts, adding 14 parts of oxidant and 2 parts of oxidation aid after grinding for 1 hour, and then continuously grinding for 20 hours to obtain a lamella with the thickness of 2.35nm, the plane size of the lamella of 1.3 mu m, the oxygen content of 8.5 percent and the specific surface area of 261m2The thermal conductivity coefficient is 1326W/(m.K). The results applied to cement-based composites are shown in table 1.
The particle size of the graphite powder in the embodiment is 13-15 μm, and the carbon content is not less than 99.5%; the oxidant is prepared by mixing potassium chlorate, potassium persulfate and potassium dichromate according to the mass ratio of 5:5: 6; the oxidation assistant is lead dioxide or cobalt trifluoride; the dispersing auxiliary agent is a powdery polycarboxylic acid water reducing agent, the content of the solid polycarboxylic acid water reducing agent is not less than 99.5 percent, the water content is not more than 2 percent, the fineness is that the average particle size is 35 mu m, and the water reducing rate is not less than 30 percent; the grinding aid is prepared by mixing silicon powder and steel slag powder according to the mass ratio of 1:2, wherein the particle size of the silicon powder is 2-10 mu m, and the specific surface area is not less than 3000m2Kg, silica content greater than 90%; the slag powder being produced by steel worksThe slag is obtained by grinding, the particle size is 2-10 mu m, and the specific surface area is not less than 3000m2Per kg, the sulfur trioxide content is not more than 4.0 percent; the ball milling is a high-energy planetary ball mill, the ball milling tank is a stainless steel tank, the grinding balls are GCr15 super-hardness alloy grinding balls, the ball material ratio is 8:1, and the ball milling rotating speed is 300 r/min.
Example 2:
100 parts of graphite powder, 8 parts of grinding aid and 10 parts of dispersing aid are put into a ball milling tank for mixing and grinding according to the mass parts, 15 parts of oxidant and 2.5 parts of oxidizing aid are added after grinding for 1 hour, and then the mixture is continuously ground for 20 hours to obtain a lamella with the thickness of 2.53nm, the size of the plane of the lamella of 1.9 mu m, the oxygen content of 9.6 percent and the specific surface area of 275m2The thermal conductivity coefficient is 1685W/(m.K) low-degree graphene oxide nano-sheet layer powder. The rest is the same as example 1.
The results applied to cement-based composites are shown in table 1.
Example 3:
putting 120 parts of graphite powder, 9 parts of grinding aid and 12 parts of dispersing aid into a ball milling tank for mixing and grinding according to the mass parts, adding 16 parts of oxidant and 3 parts of oxidation aid after grinding for 1 hour, and then continuously grinding for 20 hours to obtain a lamella with the thickness of 2.75nm, the plane size of the lamella of 2.5 mu m, the oxygen content of 12.8 percent and the specific surface area of 287m2The thermal conductivity coefficient is 1852W/(m.K) low degree graphene oxide nano-sheet layer powder. The rest is the same as example 1.
The results applied to cement-based composites are shown in table 1.
TABLE 1 sample application results of the examples
The results in the table show that the cement-based material sample prepared by the method has good heat-conducting property, compressive strength and flexural strength in 28-day-old cement-based material, and is remarkably improved compared with a control sample, so that the nano graphene oxide sheet layer powder prepared by the method has good effects of enhancing and toughening the cement matrix and improving the heat-conducting property, the water permeability resistance, freeze-thaw resistance, carbonization resistance and the like of the nano graphene oxide sheet layer powder reach the best level, and the prepared cement-based sample has no crack and leakage defects.
Preparing a cement-based composite material: P.O42.5 ordinary portland cement, low-degree graphene oxide nanosheet powder, water and a solid polycarboxylic acid water reducing agent in a mass ratio of 100:1.5:30:0.3 are cured according to a standard method.
The detection method comprises the following steps: the thermal conductivity was measured according to GB10294-1988, test on the Steady-State thermal resistance of Heat-insulating Material and the measurement of the properties of the Heat-protective plate. The compressive strength and the flexural strength are carried out according to the method of GB50107-2010 concrete strength test and evaluation Standard. The water permeability resistance is carried out according to the method of GB/T50082-2009, and the sample size
The osmotic pressure is 3.5MPa, and the pressurizing time is 48 h. The freeze-thaw resistance is carried out according to JTG E30-2005 test specification of road engineering cement and cement concrete, a rapid freezing tester is adopted to measure the frost resistance of the concrete, one freeze-thaw cycle lasts for 2-5 h, the freeze-thaw temperature is-18 ℃, and the sample size is 100mm multiplied by 500 mm. The carbonized sample is tested according to GB/T50082-2009 Standard test method for the long-term performance and durability of ordinary concrete, and the size of the sample is 100mm multiplied by 100 mm.
Claims (5)
1. A preparation method of low-degree graphene oxide nanosheet layer powder is characterized by comprising the following steps: putting 90-120 parts of graphite powder, 6-9 parts of grinding aid and 8-12 parts of dispersing aid into a ball milling tank for mixing and grinding according to the mass parts, adding 14-16 parts of oxidant and 2-3 parts of oxidation aid after grinding for 1 hour, and then continuously grinding for 20 hours to obtain a lamella with the thickness of 2.35-2.75 nm, the plane size of the lamella of 1.3-2.5 mu m, the oxygen content of 8.5-12.8 percent and the specific surface area of 261-287 m2The graphene oxide nano-sheet layer powder with low degree has a thermal conductivity of 1326-1852W/(m.K);
the grinding aid is prepared by mixing silicon powder and steel slag powder according to the mass ratio of 1:2, wherein the particle size of the silicon powder is 2-10 mu m, and the specific surface area is not less than 3000m2Per kg, dioxide oxidationThe silicon content is more than 90 percent; the steel slag powder is obtained by grinding slag produced by a steel plant, the particle size is 2-10 mu m, and the specific surface area is not less than 3000m2Per kg, the sulfur trioxide content is not more than 4.0 percent;
the dispersing auxiliary agent is a powdery polycarboxylic acid water reducing agent, the content of the solid polycarboxylic acid water reducing agent is not less than 99.5 percent, the water content is not more than 2 percent, the fineness is that the average particle size is 35 mu m, and the water reducing rate is not less than 30 percent;
the oxidant is prepared by mixing potassium chlorate, potassium persulfate and potassium dichromate according to the mass ratio of 5:5: 6; the oxidation assistant is lead dioxide or cobalt trifluoride;
the grinding adopts a high-energy planetary ball mill, the ball material ratio is 8:1, and the ball milling rotating speed is 300 r/min.
2. The method for preparing low-degree graphene oxide nanosheet powder of claim 1, wherein the method comprises: the particle size of the graphite powder is 13-15 mu m, and the carbon content is not less than 99.5%.
3. The method for preparing low-degree graphene oxide nanosheet powder of claim 1, wherein the method comprises: the grinding equipment is a high-energy planetary ball mill, the ball milling tank is a stainless steel tank, and the grinding balls are GCr15 super-hardness alloy grinding balls.
4. The low-degree graphene oxide nanosheet powder prepared by the preparation method of claim 1, wherein: the thickness of the low-degree graphene oxide nanosheet powder sheet layer is 2.35-2.75 nm, the plane size of the sheet layer is 1.3-2.5 mu m, the oxygen content is 8.5-12.8%, and the specific surface area is 261-287 m2The thermal conductivity coefficient is 1326-1852W/(m.K).
5. The application of the low-degree graphene oxide nano-sheet powder prepared by the preparation method according to claim 1 is characterized in that according to the preparation method of the cement-based material, the doping amount of the low-degree graphene oxide nano-sheet powder is 1.5-3.5% of the mass of the cement powder, the low-degree graphene oxide nano-sheet powder and the cement powder are uniformly stirred and then doped when concrete is mixed, and the compressive strength, the flexural strength and the heat conductivity coefficient of the cement-based material in the age of 28 days are respectively improved by not less than 39%, 54% and 300% compared with those of a control sample.
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| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN103241983A (en) * | 2013-05-22 | 2013-08-14 | 陕西科技大学 | Preparation method of graphene oxide modified polycarboxylic acid type water-reducer |
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| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN103241983A (en) * | 2013-05-22 | 2013-08-14 | 陕西科技大学 | Preparation method of graphene oxide modified polycarboxylic acid type water-reducer |
| CN108439917A (en) * | 2018-05-21 | 2018-08-24 | 西南交通大学 | A kind of wear-resisting road concrete |
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