CN110845874A - Preparation method of aqueous micro-nano flaky graphite material - Google Patents
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses a preparation method of an aqueous micro-nano flaky graphite material, which is characterized by comprising the following steps of: heating expandable graphite powder to 450 ℃ and calcining to obtain expanded graphite powder; taking the raw materials according to the mass percentage of 2-11% of expanded graphite powder, 0.5-3% of film-forming additive, 0.5-3% of coupling agent, 0.5-3% of dispersing agent, 0.1-0.5% of defoaming agent, 15-20% of hydroxyethyl cellulose aqueous solution and 60-82% of water; adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, and adding a hydroxyethyl cellulose aqueous solution and a defoaming agent under stirring; adding expanded graphite powder, stirring and uniformly mixing, and putting into a pulping machine to grind into uniform slurry to obtain slurry; and drying and dehydrating the slurry to obtain the aqueous micro-nano flaky graphite powder. The method has simple process and low cost, and the prepared aqueous micro-nano flaky graphite material can be widely applied to the industries of aqueous industry, such as corrosion resistance, water resistance, electric conduction, heat conduction, electromagnetic shielding and the like.
Description
Technical Field
The invention belongs to preparation of graphite materials, and relates to a preparation method of an aqueous micro-nano flaky graphite material. The aqueous micro-nano flaky graphite material prepared by the method has a flaky structure with micro-nano size, is low in cost, aqueous and environment-friendly, is simple in process, and can be widely applied to aqueous industrial industries such as corrosion prevention, water prevention, electric conduction, heat conduction, electromagnetic shielding and the like.
Background
Graphene is a novel nano graphite material, has become the leading edge and the hot spot which are attracted attention at home and abroad since the emergence of the world, is a two-dimensional crystal formed by closely packing carbon atoms, is bonded into a honeycomb crystal lattice by sp2 hybrid orbitals, and is the thinnest nano material with the strongest hardness in the world at present. The special structure of graphene enables the graphene to have a plurality of excellent physicochemical properties, such as: mechanical properties, electrical properties, thermal properties, corrosion resistance, excellent light transmittance and the like, and the excellent properties of graphene provide a wide imagination space for the application of graphene in many aspects. With the progress of research, the application of graphene in the aspects of materials, energy, environment, coatings and the like has excellent development and results, particularly in the field of coatings, graphene has the advantages of small size, high electron transfer speed, good conductivity, high hardness and the like, the flaky structure of the graphene brings a good shielding effect, the water resistance, corrosion resistance, flexibility and impact resistance of the coating can be improved, and the coating can be endowed with some new functions, such as static electricity conduction, wave absorption stealth, photocatalysis and the like, so that the application prospect is very good.
At present, the preparation methods of graphene are various, such as a mechanical stripping method, a redox method, an epitaxial growth method, a vapor deposition method and the like are common, and ultrathin materials with the thickness of several nanometers are generally prepared, in the prior art, the reports of the preparation methods of the water-based graphite materials are few, and the defects of complex preparation process, high production cost, poor practicability and the like exist:
(1) the cost is very high, the market price is 7000 yuan to 20000 yuan per kilogram, which severely limits the popularization and application;
(2) graphene materials prepared by the prior art are nano-scale materials, the average thickness of the graphene materials is generally several nanometers, the graphene materials are difficult to disperse, the manufacturing difficulty is increased in the industries of paint, plastics and the like, and the graphene materials are not beneficial to popularization and use;
(3) the existing graphene materials generally have strong hydrophobicity and are not beneficial to being used in a water-based system, and oily coatings, plastics and the like have good dryness and water resistance, but can generate a large amount of volatile organic solvents to cause serious environmental pollution, and are forcibly prohibited to be used in a plurality of fields.
Therefore, the micro-nano graphite material with lower cost has wide application prospect, is easier to prepare, has relatively lower cost, is easier to disperse and is better applied to the industries of coating plastics and the like, and meanwhile, the development and application of the water-based graphite material are imperative.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of an aqueous micro-nano flaky graphite material. The invention provides a novel method for preparing a micro-nano thin-layer graphite material by aqueous expansion-dispersion-grinding.
The content of the invention is as follows: a preparation method of an aqueous micro-nano flaky graphite material is characterized by comprising the following steps:
a. preparing expanded graphite powder:
heating expandable graphite powder (product production or sale enterprises: Shanghai Xili carbon Co., Ltd., model: 40 mesh; Shanghai Xili carbon Co., Ltd., model: 100 mesh; Shijiazhuang Ruizi Ming mineral Co., Ltd., model: 200 mesh; etc.) to 450 deg.C, calcining until no water gas emerges, and completing expansion to obtain expanded graphite powder;
b. preparing water-based expanded graphite powder slurry:
preparing materials: taking raw materials of each component according to the mass percentage of 2-11% of expanded graphite powder, 0.5-3% of film-forming auxiliary agent alcohol ester-12, 0.5-3% of coupling agent, 0.5-3% of dispersing agent, 0.1-0.5% of defoaming agent, 15-20% of hydroxyethyl cellulose aqueous solution and 60-82% of water, wherein the sum of the components is 100% for later use;
the hydroxyethyl cellulose aqueous solution is a hydroxyethyl cellulose aqueous solution with the mass percentage content of hydroxyethyl cellulose of 2 percent; the preparation method comprises the following steps: adding 1 part by weight of hydroxyethyl cellulose into 49 parts by weight of water (slowly), and stirring the mixture to be colloidal while adding the hydroxyethyl cellulose to obtain a 2% hydroxyethyl cellulose aqueous solution;
the preparation method comprises the following steps: adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, adding the hydroxyethyl cellulose aqueous solution and the defoaming agent under stirring, and stirring and dispersing until the materials are uniformly mixed; then adding expanded graphite powder, stirring (dispersing at a high speed till full mixing) and uniformly mixing to obtain aqueous expanded graphite powder slurry;
c. grinding aqueous micro-nano flaky graphite powder slurry:
putting the aqueous expanded graphite powder slurry into a pulping machine, and grinding into uniform slurry to obtain aqueous micro-nano flaky graphite powder slurry;
d. drying to prepare aqueous micro-nano flaky graphite material powder:
and drying and dehydrating the aqueous micro-nano flaky graphite powder slurry to obtain the aqueous micro-nano flaky graphite material.
The invention comprises the following steps: in the step c, the aqueous expanded graphite powder slurry is put into a pulping machine to be ground into uniform slurry, preferably: and (3) putting the aqueous expanded graphite powder slurry into a pulping machine for (repeated) grinding, observing the slurry, and obtaining uniform slurry when the slurry presents (weak) silvery luster and (naked eyes) the uniform slurry of coarse particles is not seen.
The invention comprises the following steps: in the step b, the film forming additive alcohol ester-12 can be produced by a production or sale enterprise: guangzhou City Liqiao trade company, model: SD-505, Shanghai Motian chemical Co., Ltd, model number: ncp-2, or Guangzhou Shuangpu trade company Limited, model: a coalescent of TEXANOL; and the like.
The invention comprises the following steps: in step b, the coupling agent, manufacturing or selling enterprise may be: hangzhou Jessica chemical Co., Ltd, type: KH-550, model number of bisilication chemical ltd, tokyo: KH-560, or Kyoho chemical coating technology Limited, model: a coupling agent of KH-570; and the like.
The invention comprises the following steps: in the step b, the dispersant is a dispersant for water-based paint, and the production or sale enterprises can be: chengdu Chenbang chemical industry, type: CB-1108, Shanghaineda chemical Co., Ltd, type: SN-5040, or Shandong constant chemical Co., Ltd, model number: a dispersant of HL-5040; and the like.
The invention comprises the following steps: in the step b, the defoaming agent is a defoaming agent for the water-based paint, and the production or sale enterprises can be: hangzhou Longmao chemical Co., Ltd, model number: LM-100, New technology Co, build Bao Beijing, model: build Bao/150, or Chengdu auspicious coatings GmbH, model: a defoamer of W-W103; and the like.
The invention comprises the following steps: the hydroxyethyl cellulose production or sale enterprise in the step b can be: three liter trade company, model number, in the area of Changshan, Changde: HS10000YP2, Guangzhou City Convolvulus chemical Co., Ltd., type: HS30000YP2, or Shanghai Jixian New Material Co., Ltd., model number: hydroxyethyl cellulose of HS60000YP 2; etc. of
The invention comprises the following steps: in the step c, the aqueous expanded graphite powder slurry is put into a pulping machine to be ground into uniform slurry, preferably: and (3) putting the aqueous expanded graphite powder slurry into a pulping machine for (repeated) grinding, observing the slurry, and obtaining uniform slurry when the slurry presents (weak) silvery luster and (naked eyes) the uniform slurry of coarse particles is not seen.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) by adopting the method, the thickness of the prepared aqueous micro-nano flaky graphite material is several nanometers to hundreds of nanometers, the cost is about 50-100 yuan/kg, and is far lower than the price of 7000-20000 yuan/kg of graphene powder materials on the market, the cost advantage is excellent, the key problem that the price of the graphene material is extremely high is solved, and the application prospect is good;
(2) by adopting the preparation method, the prepared water-based micro-nano thin-layer graphite material is technically modified to be water-based, can be widely applied to industries such as water-based paint, environment-friendly plastics and the like, is water-based and environment-friendly, provides an excellent material for the environmental protection technology improvement of the industry, and makes a prominent contribution to the industry technology improvement;
(3) the invention adopts a method of expansion-dispersion-grinding to prepare the water-based micro-nano thin graphite material, the surface area of the water-based micro-nano thin graphite material is more than 100 times larger than that of common powder particles, and the water-based micro-nano thin graphite material can be well compatible with a high-molecular film forming material due to the organic property of graphite, is superposed in a coating film and is tightly connected to form a multi-layer shielding structure, is an excellent blocking and shielding material, is particularly suitable for the preparation of materials such as waterproof, anticorrosion, electromagnetic shielding and the like, and has the effects of four or two jacks, and the inventor adds the water-based anticorrosion coating prepared by the material with 0.8 percent of solid content, and the water-based anticorrosion coating can still be intact after a water resistance test for 3 months and can far exceed the standard requirement for;
(4) the method has simple process, does not use high temperature and high pressure, does not need expensive equipment and implementation investment, does not use corrosive acid-base materials, does not generate waste water and waste gas, is a physical clean production process, and has the advantages of environmental protection, safety, good application prospect and strong practicability; the prepared aqueous micro-nano flaky graphite material has a micro-nano flaky structure, is low in cost, aqueous and environment-friendly, is simple in process, and can be widely applied to aqueous industrial corrosion prevention, waterproof, electric conduction, heat conduction, electromagnetic shielding and other industries.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
Example 1:
a preparation method of an aqueous micro-nano flaky graphite material comprises the following steps:
a. preparing expanded graphite powder: heating expandable graphite powder to 450 ℃, calcining until no water gas emerges, and completing expansion to obtain expanded graphite powder;
b. preparing water-based expanded graphite powder slurry:
preparing materials: taking raw materials of each component according to the mass percentage of 7 percent of expanded graphite powder, 1 percent of film forming additive, 2 percent of coupling agent, 2 percent of dispersing agent, 0.2 percent of defoaming agent, 15 percent of hydroxyethyl cellulose aqueous solution and 72.8 percent of water for standby;
the hydroxyethyl cellulose aqueous solution is a hydroxyethyl cellulose aqueous solution with the mass percentage content of hydroxyethyl cellulose of 2 percent; the preparation method comprises the following steps: adding 1 part by weight of hydroxyethyl cellulose into 49 parts by weight of water, and stirring the mixture to be colloidal while adding the hydroxyethyl cellulose to obtain a 2% hydroxyethyl cellulose aqueous solution; (ii) a
The preparation method comprises the following steps: adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, adding a hydroxyethyl cellulose aqueous solution and a defoaming agent into the dispersion machine under stirring, and stirring and dispersing the materials until the materials are uniformly mixed; then adding expanded graphite powder, stirring (dispersing at a high speed till full mixing) and uniformly mixing to obtain aqueous expanded graphite powder slurry;
c. grinding aqueous micro-nano flaky graphite powder slurry:
putting the water-based expanded graphite powder slurry into a pulping machine for (repeated) grinding, observing the slurry, and when the slurry presents (weak) silvery luster and (naked eyes) does not see the uniform slurry of coarse particles, obtaining uniform slurry, namely the water-based micro-nano flaky graphite powder slurry is prepared;
d. drying to prepare aqueous micro-nano flaky graphite material powder: and drying and dehydrating the aqueous micro-nano flaky graphite powder slurry to obtain the aqueous micro-nano flaky graphite material.
The thickness of the prepared aqueous micro-nano flaky graphite material is 1-500 nanometers, and the width is 1-60 micrometers.
Examples 2 to 17:
a preparation method of an aqueous micro-nano flaky graphite material mainly changes the percentage contents of expanded graphite powder, a film-forming aid, a coupling agent, a dispersing agent and a defoaming agent in ingredients, changes the percentage content of water at the same time, and has the same other raw materials and percentages as those in example 1, and the related parameter changes are as follows:
the preparation method and procedure of examples 2-17 are otherwise the same as in example 1 and are omitted.
The thickness of the prepared aqueous micro-nano flaky graphite material is 1-500 nanometers, and the width is 1-60 micrometers.
Examples 18 to 22:
a preparation method of an aqueous micro-nano flaky graphite material mainly changes the percentage content of 2% hydroxyethyl cellulose aqueous solution in ingredients and changes the percentage content of water, other raw materials and percentages are the same as those in example 1, and relevant parameter changes are as follows:
the preparation method and procedure of examples 18 to 22 were otherwise the same as in example 1, and were omitted.
The thickness of the prepared aqueous micro-nano flaky graphite material is 1-500 nanometers, and the width is 1-60 micrometers.
Example 23:
a preparation method of an aqueous micro-nano flaky graphite material comprises the following steps:
a. preparing expanded graphite powder:
heating expandable graphite powder to 450 ℃, calcining until no water gas emerges, and completing expansion to obtain expanded graphite powder;
b. preparing water-based expanded graphite powder slurry:
preparing materials: taking raw materials of each component according to the mass percentage of 2 percent of expanded graphite powder, 0.5 percent of film forming additive, 0.5 percent of coupling agent, 0.5 percent of dispersant, 0.1 percent of defoaming agent, 15 percent of hydroxyethyl cellulose aqueous solution and 81.4 percent of water for standby;
the hydroxyethyl cellulose aqueous solution is a hydroxyethyl cellulose aqueous solution with the mass percentage content of hydroxyethyl cellulose of 2 percent; the preparation method comprises the following steps: adding 1 part by weight of hydroxyethyl cellulose into 49 parts by weight of water, and stirring the mixture to be colloidal while adding the hydroxyethyl cellulose to obtain a 2% hydroxyethyl cellulose aqueous solution;
the preparation method comprises the following steps: adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, adding a hydroxyethyl cellulose aqueous solution and a defoaming agent into the dispersion machine under stirring, and stirring and dispersing the materials until the materials are uniformly mixed; then adding expanded graphite powder, stirring (dispersing at a high speed till full mixing) and uniformly mixing to obtain aqueous expanded graphite powder slurry;
c. grinding aqueous micro-nano flaky graphite powder slurry:
putting the aqueous expanded graphite powder slurry into a pulping machine, and grinding into uniform slurry to obtain aqueous micro-nano flaky graphite powder slurry;
d. drying to prepare aqueous micro-nano flaky graphite material powder:
and drying and dehydrating the aqueous micro-nano flaky graphite powder slurry to obtain the aqueous micro-nano flaky graphite material.
The thickness of the prepared aqueous micro-nano flaky graphite material is 1-500 nanometers, and the width is 1-60 micrometers.
Example 24:
a preparation method of an aqueous micro-nano flaky graphite material comprises the following steps:
a. preparing expanded graphite powder:
heating expandable graphite powder to 450 ℃, calcining until no water gas emerges, and completing expansion to obtain expanded graphite powder;
b. preparing water-based expanded graphite powder slurry:
preparing materials: taking raw materials of each component according to the mass percentage of 11 percent of expanded graphite powder, 3 percent of film forming additive, 3 percent of coupling agent, 3 percent of dispersing agent, 0.5 percent of defoaming agent, 19.5 percent of hydroxyethyl cellulose aqueous solution and 60 percent of water for standby;
the hydroxyethyl cellulose aqueous solution is a hydroxyethyl cellulose aqueous solution with the mass percentage content of hydroxyethyl cellulose of 2 percent; the preparation method comprises the following steps: adding 1 part by weight of hydroxyethyl cellulose into 49 parts by weight of water, and stirring the mixture to be colloidal while adding the hydroxyethyl cellulose to obtain a 2% hydroxyethyl cellulose aqueous solution;
the preparation method comprises the following steps: adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, adding a hydroxyethyl cellulose aqueous solution and a defoaming agent into the dispersion machine under stirring, and stirring and dispersing the materials until the materials are uniformly mixed; then adding expanded graphite powder, stirring (dispersing at a high speed till full mixing) and uniformly mixing to obtain aqueous expanded graphite powder slurry;
c. grinding aqueous micro-nano flaky graphite powder slurry:
putting the aqueous expanded graphite powder slurry into a pulping machine, and grinding into uniform slurry to obtain aqueous micro-nano flaky graphite powder slurry;
d. drying to prepare aqueous micro-nano flaky graphite material powder:
and drying and dehydrating the aqueous micro-nano flaky graphite powder slurry to obtain the aqueous micro-nano flaky graphite material.
The thickness of the prepared aqueous micro-nano flaky graphite material is 1-500 nanometers, and the width is 1-60 micrometers.
Example 25:
a preparation method of an aqueous micro-nano flaky graphite material comprises the following steps:
a. preparing expanded graphite powder:
heating expandable graphite powder to 450 ℃, calcining until no water gas emerges, and completing expansion to obtain expanded graphite powder;
b. preparing water-based expanded graphite powder slurry:
preparing materials: taking raw materials of each component according to the mass percentage of 6.5 percent of expanded graphite powder, 1.7 percent of film forming additive, 1.7 percent of coupling agent, 1.7 percent of dispersant, 0.3 percent of defoaming agent, 17 percent of hydroxyethyl cellulose aqueous solution and 71.1 percent of water, wherein the sum of the components is 100 percent for standby;
the hydroxyethyl cellulose aqueous solution is a hydroxyethyl cellulose aqueous solution with the mass percentage content of hydroxyethyl cellulose of 2 percent; the preparation method comprises the following steps: adding 1 part by weight of hydroxyethyl cellulose into 49 parts by weight of water, and stirring the mixture to be colloidal while adding the hydroxyethyl cellulose to obtain a 2% hydroxyethyl cellulose aqueous solution;
the preparation method comprises the following steps: adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, adding a hydroxyethyl cellulose aqueous solution and a defoaming agent into the dispersion machine under stirring, and stirring and dispersing the materials until the materials are uniformly mixed; then adding expanded graphite powder, stirring (dispersing at a high speed till full mixing) and uniformly mixing to obtain aqueous expanded graphite powder slurry;
c. grinding aqueous micro-nano flaky graphite powder slurry:
putting the aqueous expanded graphite powder slurry into a pulping machine, and grinding into uniform slurry to obtain aqueous micro-nano flaky graphite powder slurry;
d. drying to prepare aqueous micro-nano flaky graphite material powder:
and drying and dehydrating the aqueous micro-nano flaky graphite powder slurry to obtain the aqueous micro-nano flaky graphite material.
The thickness of the prepared aqueous micro-nano flaky graphite material is 1-500 nanometers, and the width is 1-60 micrometers.
In the above embodiment: all the raw materials are commercially available products.
In the above embodiment: the percentages used, not specifically indicated, are percentages by weight or known to those skilled in the art; the parts by mass (by weight) may all be grams or kilograms.
In the above embodiment: the process parameters (temperature, time, etc.) and the numerical values of the components in each step are in the range, and any point can be applicable.
The present invention and the technical contents not specifically described in the above embodiments are the same as the prior art.
The present invention is not limited to the above-described embodiments, and the present invention can be implemented with the above-described advantageous effects.
Claims (6)
1. A preparation method of an aqueous micro-nano flaky graphite material is characterized by comprising the following steps:
a. preparing expanded graphite powder:
heating expandable graphite powder to 450 ℃, calcining until no water gas emerges, and completing expansion to obtain expanded graphite powder;
b. preparing water-based expanded graphite powder slurry:
preparing materials: taking raw materials of 2-11% of expanded graphite powder, 0.5-3% of film forming auxiliary agent, 0.5-3% of coupling agent, 0.5-3% of dispersing agent, 0.1-0.5% of defoaming agent, 15-20% of hydroxyethyl cellulose aqueous solution and 60-82% of water in percentage by mass for later use;
the hydroxyethyl cellulose aqueous solution is a hydroxyethyl cellulose aqueous solution with the mass percentage content of 2 percent of hydroxyethyl cellulose; the preparation method comprises the following steps: adding 1 part by weight of hydroxyethyl cellulose into 49 parts by weight of water, and stirring the mixture to be colloidal while adding the hydroxyethyl cellulose to obtain a 2% hydroxyethyl cellulose aqueous solution;
the preparation method comprises the following steps: adding water, a film-forming assistant, a coupling agent and a dispersing agent into a dispersion machine in sequence, adding a hydroxyethyl cellulose aqueous solution and a defoaming agent into the dispersion machine under stirring, and stirring and dispersing the materials until the materials are uniformly mixed; then adding expanded graphite powder, and uniformly stirring to obtain aqueous expanded graphite powder slurry;
c. grinding aqueous micro-nano flaky graphite powder slurry:
putting the aqueous expanded graphite powder slurry into a pulping machine, and grinding into uniform slurry to obtain aqueous micro-nano flaky graphite powder slurry;
d. drying to prepare aqueous micro-nano flaky graphite material powder:
and drying and dehydrating the aqueous micro-nano flaky graphite powder slurry to obtain the aqueous micro-nano flaky graphite material.
2. The preparation method of the aqueous micro-nano flaky graphite material according to claim 1, which is characterized by comprising the following steps: and c, putting the aqueous expanded graphite powder slurry into a pulping machine to be ground into uniform slurry, wherein the slurry is prepared by the following steps: and (3) putting the water-based expanded graphite powder slurry into a pulping machine for grinding, observing the slurry, and obtaining uniform slurry when the slurry is uniform slurry with silvery luster and no coarse particles.
3. The preparation method of the aqueous micro-nano flaky graphite material according to claim 1 or 2, which is characterized by comprising the following steps: in step b, the coalescing agent is alcohol ester-12.
4. The preparation method of the aqueous micro-nano flaky graphite material according to claim 1 or 2, which is characterized by comprising the following steps: in step b, the coupling agent is KH-550, KH-560 or KH-570.
5. The preparation method of the aqueous micro-nano flaky graphite material according to claim 1 or 2, which is characterized by comprising the following steps: the dispersant in step b is a commonly used dispersant for aqueous coating materials.
6. The preparation method of the aqueous micro-nano flaky graphite material according to claim 1 or 2, which is characterized by comprising the following steps: the defoaming agent in the step b is a commonly used defoaming agent for water-based paint.
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