CN110562966A - Preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder - Google Patents
Preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder Download PDFInfo
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- CN110562966A CN110562966A CN201910928570.XA CN201910928570A CN110562966A CN 110562966 A CN110562966 A CN 110562966A CN 201910928570 A CN201910928570 A CN 201910928570A CN 110562966 A CN110562966 A CN 110562966A
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- tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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Abstract
The invention belongs to the field of inorganic chemistry, and particularly relates to a preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder. The method specifically comprises the following steps: a preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder comprises the following steps: the preparation method comprises the following steps of preparing a graphene dispersion liquid, preparing the graphene dispersion liquid by grinding and stripping, and preparing the graphene dispersion liquid by drying and solidifying into powder, wherein the graphene dispersion heat formula comprises the following components in percentage by mass: 71.8% deionized water, 0.3% polyether siloxane copolymer wetting agent, 0.3% silicone defoamer, 0.3% kathon preservative, 1% PVP, 2% CTAB, 0.3% fluorosurfactant, 12% tetrafluoroethylene-hexafluoropropylene polymer dispersion, and 12% vermicular graphite. Charged tetrafluoroethylene-hexafluoropropylene polymer dispersion liquid and a fluorine surfactant are added in the graphene powder manufacturing process, so that the material composition is optimized, the graphene is efficiently stripped, and finally the graphene with high purity, large size and few-layer structure is formed. The process has the advantages of simple production process, high production efficiency, short reaction time and the like, optimizes the material composition and reduces the production cost.
Description
Technical Field
The invention belongs to the field of inorganic chemistry, and particularly relates to a preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder.
Background
Graphene possesses unique physicochemical properties, however, fine graphene cannot really exert its superior properties, and therefore, research on preparation of large-sized, high-efficiency graphene is necessary. Since 2004, how to efficiently prepare graphene has attracted the attention of researchers, and the theory and method for preparing graphene are also endless. However, the conventional few-layer graphene is prepared by using chemical chloride as an intercalating agent or a penetrating agent, which has low stripping efficiency and long reaction time, and the materials are not easy to remove, so that the corrosion resistance is influenced in the future.
therefore, it is necessary to provide a technical means to solve the above-mentioned drawbacks.
Disclosure of Invention
In view of the above problems, the main task of the present invention is to provide a process for preparing a graphene powder containing charged tetrafluoroethylene-hexafluoropropylene polymer, so as to solve the problems that the exfoliation efficiency of the intercalation agent is low, the reaction time is long, the materials of the intercalation agent are not easy to remove, and the corrosion resistance is influenced in the future, in which the chemical chloride is used as the intercalation agent or penetrating agent for the few-layer graphene.
the technical scheme provided by the invention for solving the technical problem is as follows:
A manufacturing process of charged tetrafluoroethylene-hexafluoropropylene-containing polymer graphene powder comprises the following processing steps:
S1001: weighing deionized water, a polyether siloxane copolymer wetting agent, an organic silicon defoaming agent, a kaempon preservative, PVP, CTAB, a fluorine surfactant, tetrafluoroethylene-hexafluoropropylene polymer dispersion liquid and vermicular graphite, sequentially adding the weighed materials into a material pulling cylinder of a dispersion machine according to a proportion, slowly stirring for 1 hour, and then stirring for 1 hour at a high speed to fully dissolve the materials to obtain dispersion liquid for later use;
S1002: conveying the dispersion liquid into an ultrasonic dispersion machine, vibrating for 1.5 hours under the environment of 20000Hz ultrasonic waves, and crushing agglomerated particles in the dispersion liquid to uniformly disperse the particles;
S1003: inputting the dispersion liquid processed in the step S1002 into a nano sand mill for circular grinding for 4.5 hours to obtain graphene liquid slurry;
s1004: and conveying the graphene liquid slurry to a spray dryer for rotary atomization and drying granulation to obtain finished graphene powder, and collecting the finished graphene powder through a powder collector.
preferably, the stirring speed of the disperser in step S1001 is 100-1600 rpm.
preferably, the rotation speed of the spray dryer is 100-300rpm, the inlet temperature of the spray dryer is 200 ℃ and the outlet temperature of the spray dryer is 95 ℃.
Preferably, the temperature of the dispersion liquid in step S1003 and the dispersion liquid in step S1004 is controlled by a constant temperature freezer, and the pressure in the constant temperature freezer is 0.8 Mpa.
Preferably, the temperature of the dispersion liquid in step S1003 and step S1004 is 45 ℃.
Preferably, the grinding media in the nano sand mill are zirconia beads with a diameter of 0.8mm to 1.2 mm.
preferably, the pressure in the spray dryer in the step S1004 is 0.8 MPa.
Compared with the prior art, the invention has the beneficial technical effects that:
1. according to the invention, charged tetrafluoroethylene-hexafluoropropylene polymer is added, fluorine-containing particles are used as a stripping impact agent of graphite, and a fluorine-containing surfactant with high permeability is combined, so that the charged tetrafluoroethylene-hexafluoropropylene polymer and the fluorine-containing surfactant have a synergistic effect mutually in the manufacturing process, and the graphite can be rapidly, orderly and efficiently stripped to form complete large-size few-layer structure graphene. The surface of the stripped graphene is loaded with charged tetrafluoroethylene-hexafluoropropylene copolymer and fluorine surfactant, namely, the graphite can be efficiently and completely stripped to prepare stable dispersion liquid containing large-size few-layer graphene in a fluorinated state, so that the liquid graphene has high stability and good dispersibility in a graphene system; through the boiling, moist and hot granulation treatment of the dispersion liquid, the multilayer graphene in the drying process can be rolled and folded into the fluorine-containing flower-shaped graphene sphere which can be folded, so that the flower-shaped graphene sphere has a very high surface area and can be used as a carrier of a high-efficiency catalyst. According to the invention, charged tetrafluoroethylene-hexafluoropropylene copolymer and fluorine surfactant are added in the graphene powder manufacturing process, so that the material composition is optimized, graphene is efficiently stripped, and finally, the graphene powder with a specific surface area of more than 20m2/g, a C content of more than 90 wt%, a high purity, a large size and a few-layer structure is formed, has the functions of reinforcement, toughening, wear resistance, electric conduction, heat conduction, corrosion resistance and the like, and is a preferred high-quality composition agent for preparing advanced functional materials.
2. The process has the advantages of simple production process, high production efficiency, short reaction time and the like.
drawings
Fig. 1 is a flow chart of a manufacturing process of a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to the present invention.
Fig. 2 is a picture of a scanning electron microscope after stripping graphene from a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to the present invention.
Fig. 3 is a scanning electron microscope image of a fluorine-containing flower-like graphene sphere in a charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder according to the present invention.
Fig. 4 is a raman spectrum of graphene containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder, wherein: the preparation process of the charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder comprises the following processing steps:
S1001: weighing deionized water, a polyether siloxane copolymer wetting agent, an organic silicon defoaming agent, a kaempon preservative, PVP, CTAB, a fluorine surfactant, tetrafluoroethylene-hexafluoropropylene polymer dispersion liquid and vermicular graphite, sequentially adding the weighed materials into a material pulling cylinder of a dispersion machine according to a proportion, slowly stirring for 1 hour, and then stirring for 1 hour at a high speed to fully dissolve the materials to obtain dispersion liquid for later use;
S1002: conveying the dispersion liquid into an ultrasonic dispersion machine, vibrating for 1.5 hours under the environment of 20000Hz ultrasonic waves, and crushing agglomerated particles in the dispersion liquid to uniformly disperse the particles;
S1003: inputting the dispersion liquid processed in the step S1002 into a nano sand mill for circular grinding for 4.5 hours to obtain graphene liquid slurry;
S1004: conveying the graphene liquid slurry to a spray dryer for rotary atomization and drying to obtain finished graphene powder, and collecting the finished graphene powder through a powder collector.
Further, the stirring speed of the disperser in step S1001 is 100-1600 rpm.
Further, the rotation speed of the spray dryer is 100-300rpm, the inlet temperature of the spray dryer is 200 ℃, and the outlet temperature of the spray dryer is 95 ℃.
Further, the dispersion liquid in the step S1003 and the step S1004 is temperature-controlled by a constant temperature freezer in which a pressure is 0.8 Mpa.
Further, the temperature of the dispersion liquid in step S1003 and step S1004 is 45 ℃.
Further, the grinding medium in the nanometer sand mill is zirconia beads with the diameter of 0.8mm-1.2 mm.
Further, the pressure in the nano sand mill in the step S1003 is 0.8 Mpa.
further, the pressure in the spray dryer in the step S1004 is 0.8 MPa.
according to the invention, charged tetrafluoroethylene-hexafluoropropylene polymer is added, fluorine-containing particles are used as a stripping impact agent of graphite, and a fluorine-containing surfactant with high permeability is combined, so that the charged tetrafluoroethylene-hexafluoropropylene polymer and the fluorine-containing surfactant have a synergistic effect mutually in the manufacturing process, and the graphite can be rapidly, orderly and efficiently stripped to form complete large-size few-layer structure graphene. The surface of the stripped graphene is loaded with charged tetrafluoroethylene-hexafluoropropylene copolymer and fluorine surfactant, namely, the graphite can be efficiently and completely stripped to prepare stable dispersion liquid containing large-size few-layer graphene in a fluorinated state, so that the liquid graphene has high stability and good dispersibility in a graphene system; by carrying out boiling, moist-heat granulation on the dispersion liquid, folding and folding multiple layers of graphene in the drying process to prepare a foldable fluorine-containing flower-shaped graphene sphere, wherein the structure of the fluorine-containing flower-shaped graphene sphere is shown in fig. 2, so that the flower-shaped graphene sphere has a very high surface area and can be used as a carrier of an efficient catalyst, please refer to fig. 1-4, and fig. 2 is a scanning electron microscope picture of peeled graphene in the process of preparing graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to the formula in the embodiment; fig. 3 is a scanning electron microscope picture of a fluorine-containing flower-like graphene sphere obtained in the process of manufacturing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to the formulation in the example; fig. 4 is a characteristic diagram of the structure and properties of graphene in the charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder prepared according to the formulation in the example, obtained by raman spectroscopy. As can be seen from fig. 1 to fig. 4, charged tetrafluoroethylene-hexafluoropropylene copolymer and fluorine surfactant are added in the graphene powder manufacturing process, so that the material composition is optimized, graphene is efficiently stripped, and finally, the graphene powder with a specific surface area of more than 20m2/g, a C content of more than 90 wt%, a relatively high purity, a large size and a few-layer structure is formed, has the functions of reinforcement, toughening, wear resistance, electric conduction, heat conduction, corrosion resistance and the like, and is a preferred high-quality composite agent for preparing advanced functional materials.
it should be noted that the ultrasonic dispersion machine, the nano sand mill, the spray dryer, the powder collector and the constant temperature refrigerator in the above embodiments are all the prior art, and can be purchased in the relevant shops in the market, and as long as the specifications are matched, the functions required in the above process steps can be realized, and the detailed description is omitted here.
while the preferred embodiments of the present invention have been illustrated in detail in the accompanying drawings, it should be understood that the scope of the invention includes, but is not limited to, the embodiments described above; while the invention has been described with reference to specific embodiments, it will be appreciated by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A preparation process of charged tetrafluoroethylene-hexafluoropropylene polymer-containing graphene powder is characterized by comprising the following processing steps:
S1001: weighing deionized water, a polyether siloxane copolymer wetting agent, an organic silicon defoaming agent, a kaempon preservative, PVP, CTAB, a fluorine surfactant, tetrafluoroethylene-hexafluoropropylene polymer dispersion liquid and vermicular graphite, sequentially adding the weighed materials into a material pulling cylinder of a dispersion machine according to a proportion, slowly stirring for 1 hour, then stirring for 1 hour at a high speed, fully dissolving the materials, and obtaining a dispersion liquid for later use;
S1002: conveying the dispersion liquid into an ultrasonic dispersion machine, vibrating for 1.5 hours under the environment of 20000Hz ultrasonic waves, and crushing agglomerated particles in the dispersion liquid to uniformly disperse the particles;
S1003: inputting the dispersion liquid processed in the step S1002 into a nano sand mill for circular grinding for 4.5 hours to obtain graphene liquid slurry;
S1004: conveying the graphene liquid slurry to a spray dryer for rotary atomization and drying to obtain finished graphene powder, and collecting the finished graphene powder through a powder collector.
2. The process for producing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 1, wherein: the dispersion liquid in the step S1001 has the following components in percentage by mass:
Deionized water, 71.8%; polyether siloxane copolymer wetting agent, 0.3%; 0.3 parts of organic silicon defoaming agent; 0.3 parts of kasong preservative; 1% of PVP; CTAB, 2%; 0.3% of a fluorine surfactant; 12% of tetrafluoroethylene-hexafluoropropylene polymer dispersion; vermicular graphite, 12%.
3. The process for producing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 2, wherein: the stirring speed of the disperser in step S1001 is 100-1600 rpm.
4. The process for producing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 1, wherein: the rotating speed of the spray dryer is 100-300rpm, the temperature of an input port of the spray dryer is 200 ℃, and the temperature of an output port of the spray dryer is 95 ℃.
5. The process for producing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 1, wherein: the temperature of the dispersion liquid in the step S1003 and the step S1004 is controlled by a constant temperature freezer, and the pressure in the constant temperature freezer is 0.8 Mpa.
6. The process according to claim 5, wherein the graphene powder containing charged tetrafluoroethylene-hexafluoropropylene polymer is prepared by: the temperature of the dispersion liquid in step S1003 and step S1004 was 45 ℃.
7. The process for producing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 1, wherein: the grinding medium in the nanometer sand mill is zirconia beads with the diameter of 0.2mm-1.2 mm.
8. The process for producing the graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 1 or 7, wherein: and the pressure intensity in the nanometer sand mill in the step S1003 is 0.8 Mpa.
9. the process for producing a graphene powder containing a charged tetrafluoroethylene-hexafluoropropylene polymer according to claim 1, wherein: the pressure in the spray dryer in the step S1004 is 0.8 Mpa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111548588A (en) * | 2020-06-11 | 2020-08-18 | 北京新世翼节能环保科技股份有限公司 | Composite material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548588A (en) * | 2020-06-11 | 2020-08-18 | 北京新世翼节能环保科技股份有限公司 | Composite material |
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