CN113185855A - Preparation method and automation equipment of graphene modified powder - Google Patents
Preparation method and automation equipment of graphene modified powder Download PDFInfo
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- CN113185855A CN113185855A CN202110421093.5A CN202110421093A CN113185855A CN 113185855 A CN113185855 A CN 113185855A CN 202110421093 A CN202110421093 A CN 202110421093A CN 113185855 A CN113185855 A CN 113185855A
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Abstract
The invention discloses a preparation method of graphene modified powder and automatic equipment, belonging to the technical field of graphene powder.
Description
Technical Field
The invention relates to the technical field of graphene powder, in particular to a preparation method and automation equipment of graphene modified powder.
Background
The problem exists in the application process of graphene, that is, in the dispersion process of graphene, since graphene with a complete structure consists of benzene six-membered rings containing stable bonds, the chemical stability is high, the surface is in an inert state, the interaction with other media is weak, and strong intermolecular force exists among the sheets of graphene, the sheets are very easy to stack together and are difficult to disperse, and the sheets are difficult to dissolve in a solvent and difficult to uniformly compound with other organic or inorganic materials. This causes great difficulty in further research and application of graphene, and thus improving the dispersibility of graphene and its compatibility with various solvents and materials becomes a problem to be solved urgently in expanding the application field of graphene. One effective way to solve the above problem is to functionalize the surface. The graphene surface functionalization is that a specific functional group is introduced at a defect position of an imperfect graphene surface through covalent bond and non-covalent bond connection, so that certain properties of the graphene surface are changed. The method can achieve the following effects: improving the dispersibility of graphene; the surface activity of the material is improved; endows the material with new physical and chemical properties; improving the compatibility of the graphene with other materials.
At present, the research on graphene surface functionalization is in a development stage, and from the viewpoint of a functionalization method, the method is mainly divided into two types: (1) covalent bond functionalization; (2) non-covalent bond functionalization. Functionalization is an important means for realizing dispersion, dissolution and molding processing of graphene, and electronic property modification such as doping, ion bombardment and the like is added, and in addition, the graphene polymer composite material is prepared directly by high-energy ball milling. However, the ion bombardment methods have unique advantages, and by endowing bombardment ions with appropriate energy and bombarding specific positions of graphene, substitution defects (i.e., carbon atoms in graphene are substituted) and vacancy defects can be formed in graphene, so that the intrinsic two-dimensional structure of graphene is kept unchanged, and new electrical properties are endowed. However, the current method has more theoretical researches, and the problem of bombarding graphene at fixed ions, fixed energy and fixed positions in a laboratory is still a big problem. In recent years, the modification of graphene has been greatly advanced, but in order to fully exert the physical properties of graphene and further expand the application field of graphene, a new modification method and an existing method which is improved and improved are required to be researched.
CN201710249590.5 discloses a preparation method of a titanium nano polymer coated by a static-assisted graphene intercalation, belonging to the field of polymer preparation. The method comprises the following steps: 1. mixing graphite powder and titanium powder in a certain mass proportion; 2. and (3) putting the mixed powder material in the step (1), epoxy resin E44, low-molecular polysiloxane, DPM-30, epoxy siloxane and a solvent into a stainless steel reaction kettle to react to complete the preparation of the graphene intercalation coated titanium nano polymer slurry.
Or the existing Graphene modification method is mainly to perform acidification treatment on Graphene to obtain Graphene Oxide (GO) by a chemical oxidation method in the preparation process, wherein the Graphene Oxide contains a large amount of active groups such as carboxyl, hydroxyl, epoxy and the like, so that covalent bond functionalization can be performed on the Graphene surface by utilizing chemical reactions between the groups and other molecules.
The present company also previously filed for patent (patent No.: CN 201911097413.5): a process for preparing graphene and the slurry containing graphene includes such steps as putting flaky graphite powder, modifier such as silane coupling agent or compound containing Si-OH, distilled water and boric acid solution in stainless steel high-pressure bottle, pumping air from stainless steel high-pressure bottle, filling liquid gas in stainless steel high-pressure bottle, shaking and laying aside to make liquid gas, modifier and water infiltrate and permeate into gaps between graphite powder layers. And connecting the stainless steel high-pressure bottle with a solid gas preparation machine to prepare the solid gas. Placing solid gas in an ultraviolet light cleaning machine with 185 and 254nm wavelength for high-energy ultraviolet irradiation, directly and quickly sublimating the solid gas by receiving high-energy radiation to generate a microscopic bursting effect, stripping off few-layer or even single-layer graphene, simultaneously inducing the surface of the graphene to generate C ═ O groups and C-OH groups by the high energy generated by irradiation, continuously grafting and modifying with a modifier, continuing the ultraviolet irradiation for a period of time after the solid gas completely disappears to prepare modified graphene powder, continuously exposing the modified graphene powder under an ultraviolet lamp to obtain graphene, storing the graphene in vacuum, further preparing the prepared modified graphene intermediate into a dispersed modified titanium-silicon graphene slurry by a one-step method, wherein the method for preparing the modified graphene and the dispersed slurry thereof is efficient and environment-friendly, and meanwhile, the graphene slurry has excellent dispersibility and surface functionalization characteristics, and meanwhile, the titanium-silicon-graphene ternary composite material is subjected to bonding, grafting and modification with nano titanium and silicon to form a titanium-silicon-graphene ternary composite novel material, can be conveniently dispersed and grafted in various polymer media, and can be effectively coated with other nano material composite grafts, so that the conductivity of graphene is reduced, convenience is provided for later-stage preparation of a shielding anticorrosive coating, and a carbon cathode is unlikely to form. The method still has the defects of low single-machine yield, complex flow and the like, and has higher cost for large-scale downstream application.
Disclosure of Invention
The embodiment of the invention provides a preparation method and automatic equipment of graphene modified powder, which can be used for rapidly preparing various grafted or interface modified graphene powder and slurry in batches by directly purchasing graphene powder in an outsourcing manner for automatic batch modification, and provides a brand new technical route for downstream large-scale use of various modified graphene.
The embodiment of the invention adopts the following technical scheme: the embodiment of the invention provides a preparation method of graphene modified powder and automation equipment, and the preparation method comprises a material conveying disc, an irradiation chamber, an ozone nozzle and an atomizing nozzle, wherein the material conveying disc penetrates through the irradiation chamber, the atomizing nozzle and the ozone nozzle are both arranged in the irradiation chamber, and the atomizing nozzle is arranged at an outlet close to the irradiation chamber.
Further, the number of layers of the graphene powder is 3-10, the thickness is 1-10 nanometers, the sheet diameter is 0.1-5 micrometers, the graphene powder is evenly paved in a stainless steel conveying material tray of equipment, and the paving density of each square meter of the material is controlled to be 0.3-0.5 kg.
Further, the formula of the graphene is as follows:
diaryliodonium salt I-250: 0.01-0.1;
benzoin ethyl ether: 1-5;
KH-560 silane coupling agent: 1-5;
epoxy polysiloxane Acrylate (AEPS): 80-90.
Furthermore, the wavelength of ultraviolet light of the high-density ultraviolet lamp in the irradiation chamber is 250-2. The radiation receiving conveying stroke is 5-10 m, the width is 0.5, and the walking speed is 0.2-0.5 m/min.
Furthermore, baffles are arranged at the inlet and the outlet of the irradiation chamber.
Further, the material conveying disc is provided with a high-frequency vibrator.
Furthermore, six atomizing spray heads are arranged on the two sides of the material conveying disc and are respectively arranged at a position close to one meter of the outlet of the irradiation chamber, and the total amount of the modifier sprayed is 50-100ml per minute.
The embodiment of the invention adopts at least one technical scheme which can achieve the following beneficial effects:
firstly, under the condition that the feeding of the material conveying disc is not influenced, the inlet and the outlet of the irradiation chamber are respectively provided with the baffle plate, so that the overflow of ozone can be reduced, and the working cost is reduced.
And secondly, the conveying material tray is used for conveying the graphene powder to an irradiation chamber, the conveying material tray is continuously vibrated by the high-frequency vibrator, the graphene powder is continuously stirred, the contact area between the graphene powder and ultraviolet light and ozone is increased, and the probability of surface oxidation caused by ultraviolet light excitation and ozone is greatly improved.
Thirdly, this patent is through respectively distributing three automatic atomizer in one meter within range both sides of irradiation chamber rear end, can guarantee that graphite alkene powder and graphite alkene modification auxiliary agent mix the contact completely, increases the goodness rate of product.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic perspective view of the present invention;
FIG. 2 is a schematic cross-sectional view of the present invention;
FIG. 3 is a schematic view of the reaction of KH560 with GO;
FIG. 4 is FT-IR chart of GO, KH-560, f-GO.
Reference numerals
The device comprises a material conveying disc 1, a high-frequency vibrator 11, an irradiation chamber 2, a baffle 21, an ozone nozzle 3 and an atomizing nozzle 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the specific embodiments of the present invention and the accompanying drawings. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical solutions provided by the embodiments of the present invention are described in detail below with reference to the accompanying drawings.
The embodiment of the invention provides a preparation method of graphene modified powder and automatic equipment, wherein the preparation method comprises a conveying material tray 1, an irradiation chamber 2, an ozone nozzle 3 and an atomizing nozzle 4, the conveying material tray 1 penetrates through the irradiation chamber 2, the atomizing nozzle 4 and the ozone nozzle 3 are both arranged in the irradiation chamber 2, the atomizing nozzle 4 is arranged close to an outlet of the irradiation chamber 2, when the graphene modified powder is used, the graphene modified powder is automatically conveyed into the irradiation chamber 2 through the conveying material tray 1, ozone is discharged through the ozone nozzle 3 to mix the graphene modified powder with the ozone, a graphene modification auxiliary agent is sprayed out through the atomizing nozzle 4 to promote primary surface modification of the graphene modified powder, and the irradiation chamber 2 emits high-density ultraviolet rays to react with the graphene modified powder.
Preferably, the number of layers of the graphene powder is 3-10, the thickness is 1-10 nanometers, the sheet diameter is 0.1-5 micrometers, the graphene powder is uniformly paved in a stainless steel conveying material tray 1 of equipment, and the paving density of each square meter of the material is controlled to be 0.3-0.5 kg.
Preferably, the graphene is prepared from the following formula
Diaryliodonium salt I-250: 0.01-0.1
Benzoin ethyl ether: 1-5
KH-560 silane coupling agent: 1-5
Epoxy polysiloxane Acrylate (AEPS): 80-90, the key points and points to be protected of the patent: the formulation materials used, the ultraviolet modification involved, the delivery rate, the spraying device and the spraying amount.
Preferably, the high-density ultraviolet lamp in the irradiation chamber 2 has an ultraviolet wavelength of 250-285nm and an irradiation intensity of 2000-5000W/M2. The radiation receiving conveying stroke is 5-10 m, the width is 0.5, and the walking speed is 0.2-0.5 m/min.
Preferably, the inlet and outlet of the irradiation chamber 2 are provided with the baffles 21, so that the baffles 21 are arranged at the inlet and outlet of the irradiation chamber 2 under the condition that the feeding of the material conveying plate 1 is not influenced, the overflow of ozone can be reduced, and the working cost is reduced.
Preferably, transportation material dish 1 is provided with high frequency vibrator 11, and its effect lies in, uses transportation material dish 1 to transport graphite alkene powder to shine in the room 2, makes transportation material dish 1 constantly be in vibrations through high frequency vibrator 11, and the state that graphite alkene powder constantly stirs increases graphite alkene powder and ultraviolet light and ozone's area of contact, improves the probability that receives ultraviolet excitation and take place surface oxidation with ozone of powder by a wide margin.
Preferably, the atomizing spray heads 4 are six, the six atomizing spray heads 4 are respectively arranged at two sides of the material conveying disc 1 and close to one meter of an outlet of the irradiation chamber 2, the total amount of the modifier sprayed is 50-100 ml/min, and the effect is that the three automatic atomizing spray heads 4 are respectively distributed at two sides of the rear end of the irradiation chamber 2 within one meter, so that the graphene powder and the graphene modification aid can be ensured to be completely mixed and contacted, and the yield of the product is increased.
The working principle is as follows: when the device is used, graphene powder is automatically conveyed to the irradiation chamber 2 through the conveying material tray 1, ozone is discharged through the ozone nozzle 3 to mix the graphene powder with the ozone, the graphene modification auxiliary agent is sprayed out through the atomizing nozzle 4 to promote preliminary surface modification of the graphene powder, and the irradiation chamber 2 emits high-density ultraviolet rays to react with the graphene powder;
graphene and ozone are subjected to oxidation reaction under the catalysis of super acid or free radical formed by cracking aryl sulfonium salt under the radiation of high-strength ultraviolet rays to form surface edge oxidation or carbonylation and hydroxylation, then the graphene and the silane coupling agent are grafted, and meanwhile, epoxy polysiloxane Acrylate (AEPS) photosensitive polymer is further polymerized on the surface or the edge under the action of a photoinitiator to form a transparent and flexible epoxy polysiloxane acrylate organic layer with silicon rubber properties, so that convenience is provided for downstream dispersion in various media;
in the infrared spectrum of GO: 3415 cm-1 is a characteristic absorption peak of-OH;
in the infrared spectra of f-GO and KH-560:
the characteristic absorption peaks at 2945 cm-1 and 2843 cm-1 are-CH; 1185 cm-1 is the characteristic absorption peak of C-O-C;
the 1087 cm-1 position is the characteristic absorption peak of Si-O-C.
The above description is only an example of the present invention, and is not intended to limit the present invention. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (6)
1. The preparation method of the graphene modified powder and the automation equipment are characterized by comprising a material conveying disc (1), an irradiation chamber (2), an ozone nozzle (3) and an atomizing nozzle (4), wherein the material conveying disc (1) penetrates through the irradiation chamber (2), the atomizing nozzle (4) and the ozone nozzle (3) are both arranged in the irradiation chamber (2), and the atomizing nozzle (4) is arranged at an outlet close to the irradiation chamber (2).
2. The method and the automatic equipment for preparing the graphene modified powder according to claim 1 are characterized in that the graphene powder is evenly paved in a stainless steel conveying material tray (1) of the equipment in a number of layers of 3-10, the thickness of 1-10 nanometers and the sheet diameter of 0.1-5 micrometers, and the paving density of each square meter of the material is controlled to be 0.3-0.5 kg.
3. The method for preparing graphene modified powder according to claim 1, wherein the graphene is prepared according to a formula:
diaryliodonium salt I-250: 0.01-0.1;
benzoin ethyl ether: 1-5;
KH-560 silane coupling agent: 1-5;
epoxy polysiloxane Acrylate (AEPS): 80-90.
4. The method and the automated equipment for preparing graphene modified powder according to claim 1, wherein the irradiation intensity of the high-density ultraviolet lamp in the irradiation chamber (2) is 2000-5000W/M2 with the ultraviolet wavelength of 250-285 nm. The radiation receiving conveying stroke is 5-10 m, the width is 0.5, and the walking speed is 0.2-0.5 m/min.
5. The preparation method and the automation equipment for the graphene modified powder according to claim 1, wherein baffles (21) are arranged at the inlet and the outlet of the irradiation chamber (2).
6. The preparation method and the automation equipment for the graphene modified powder according to claim 1, wherein the material conveying tray (1) is provided with a high-frequency vibrator (11).
The preparation method and the automation equipment of the graphene modified powder according to claim 1, wherein six atomization nozzles (4) are arranged, the six atomization nozzles (4) are respectively arranged at two sides of a material conveying tray (1) and at a position close to one meter at an outlet of an irradiation chamber (2), and the total amount of modifier sprayed is 50-100 ml/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114053937A (en) * | 2021-11-25 | 2022-02-18 | 重庆石墨烯研究院有限公司 | Preparation method and device of graphene mixed powder |
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