CN108359272B - Preparation method and application of conductive pearl powder with graphene as base material - Google Patents
Preparation method and application of conductive pearl powder with graphene as base material Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/10—Interference pigments characterized by the core material
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/50—Interference pigments comprising a layer or a core consisting of or comprising discrete particles, e.g. nanometric or submicrometer-sized particles
- C09C2200/505—Inorganic particles, e.g. oxides, nitrides or carbides
Abstract
The invention provides a conductive coating with a pearlescent effect and a preparation method thereof. The conductive pearl powder is formed by using graphene as a base material and coating a layer of bismuth oxychloride crystal on the surface of the graphene. The conductive coating with the pearlescent effect prepared by the method has strong conductivity and stable color, and can be well compatible with an organic solvent.
Description
Technical Field
The invention belongs to the field of paint preparation, and particularly relates to a preparation method of conductive pearl powder with graphene as a base material and application of the conductive pearl powder in a conductive paint.
Background
The conductive coating is one of coatings, and is a special functional coating which is rapidly developed along with modern science and technology. The conductive coating can be used for eliminating static electricity, electromagnetic shielding, electric heating and corrosion prevention due to the special functions of the conductive coating, and is widely applied to various fields of modern electronics, buildings, transportation, military and the like.
In recent years, people have pursued good conductivity and have pursued more beautiful application of the coating, such as preparing conductive coating with different colors, etc. So that the conductive paint can have a pearl effect.
Disclosure of Invention
The invention provides a preparation method of conductive pearl powder by taking graphene as a base material, and the conductive pearl powder is used for preparing a novel conductive coating with a pearl effect.
The conductive pearlescent powder provided by the invention is prepared by taking graphene as a substrate, coating a layer of conductive material of bismuth oxychloride pearlescent crystal on the surface of the graphene, hydrolyzing bismuth salt to generate bismuth oxychloride in the preparation process, then coating the bismuth oxychloride on graphene oxide, and finally adding a reducing agent to convert the graphene oxide into graphene, thereby preparing the conductive pearlescent pigment taking the graphene as the substrate.
The preparation method of the conductive pearl powder with the graphene as the base material comprises the following specific steps:
(1) weighing 6-10g of anhydrous bismuth nitrate, putting the anhydrous bismuth nitrate into a beaker, and then dropwise adding 5.4-9mL of concentrated hydrochloric acid to fully dissolve the anhydrous bismuth nitrate to obtain a bismuth salt solution.
(2) Dispersing a certain amount of graphene oxide in 200mL of deionized water, starting stirring and heating to 50-80 ℃, and adjusting the pH value of the solution to 1 by using a 6mol/L hydrochloric acid solution to obtain a graphene oxide solution; wherein the amount of the graphene oxide is 0.1-0.5% of the mass of the deionized water.
(3) And (3) slowly dropwise adding the bismuth salt solution prepared in the step (1) into the graphene oxide solution prepared in the step (2), and reacting for 1-3 hours to obtain the graphene oxide-based pearlescent pigment dispersion liquid.
(4) Keeping the temperature unchanged, adding a reducing agent sodium sulfide into the pearlescent pigment dispersion liquid obtained in the step (4), continuously stirring and heating for 0.5-2 hours, reducing graphene oxide into graphene, cooling to room temperature, starting washing and suction filtration, and finally drying to obtain the bismuth oxychloride conductive pearlescent powder with the graphene as the base material. Wherein the mass ratio of the reducing agent to the graphene oxide is 1: (0.5 to 10).
The bismuth oxychloride is prepared by the bismuth salt hydrolysis method, the preparation method is direct and simple, and the bismuth oxychloride is uniformly coated on the graphene oxide by utilizing the electrostatic adsorption effect. The bismuth oxychloride is adopted as the pearlescent pigment, so that the cost can be saved, meanwhile, the bismuth oxychloride is a semiconductor material and almost non-conductive, and the bismuth oxychloride and the graphene are compounded to bring good conductive performance.
The invention also provides the application of the conductive pearl powder with the graphene as the substrate, the conductive pearl powder is used for preparing the conductive film with the pearl effect, the preparation method comprises the steps of firstly preparing the conductive material (the conductive pearl pigment) with the pearl effect by using the graphene as the substrate and coating a layer of the pearl pigment of bismuth oxychloride on the surface of the substrate, then adding the conductive pearl pigment and the curing agent into the resin substrate together, uniformly mixing the conductive pearl pigment and the curing agent to prepare the conductive coating with the pearl effect, then coating the conductive coating with the pearl effect, drying and finally preparing the conductive film. Wherein the addition amount of the curing agent is 1 to 4 weight percent of the mass of the resin matrix, and the addition amount of the conductive pearlescent pigment is 1 to 45 weight percent of the mass of the resin matrix.
The specific method comprises the following steps:
the prepared conductive pearl powder taking the graphene as the base material and the curing agent are added into the epoxy resin together, and the mixture is uniformly mixed by a mechanical stirring method to prepare the conductive coating with the pearl effect. And then coating the film, and drying the film at the temperature of 30-70 ℃ to finally prepare the conductive film.
Wherein, the addition amount of the conductive pearlescent pigment is 1 to 45 weight percent of the resin matrix, the adopted curing agent is m-phenylenediamine in aromatic amines, and the addition amount is 1 to 4 weight percent of the resin matrix.
Has the advantages that: according to the preparation method of the conductive coating with the pearlescent effect, provided by the invention, when the conductive pearlescent pigment is prepared, bismuth oxychloride is used as the pearlescent powder, and the bismuth oxychloride is used for preparing the conductive pearlescent pigment, so that the preparation method has the advantages of simplicity and convenience in operation, high efficiency, environmental friendliness, low cost and the like. After the conductive pearlescent pigment is mixed with the resin and the curing agent, the prepared conductive coating with the pearlescent effect has good antistatic performance and high-brightness pearlescent effect compared with conductive coatings prepared from other conductive powder, so that the coating has excellent conductive performance and aesthetic property, which are performances that other coatings do not have at present.
The bismuth oxychloride pearlescent pigment is used as the luminescent substrate, the bismuth oxychloride is low in cost and easy to dissolve in an organic solvent relative to mica, and the pearlescent effect of the bismuth oxychloride pearlescent pigment is remarkably enhanced after the bismuth oxychloride pearlescent pigment is dissolved in the organic solvent to prepare the coating.
Detailed Description
For the purpose of illustrating the technical content of the present invention and achieving the object, the present invention will be further described in detail with reference to several embodiments.
Example 1
Step 1, preparing the bismuth oxychloride conductive pearlescent pigment with the graphene as the base material:
(1) 10g of anhydrous bismuth nitrate was weighed into a beaker, and then 9mL of concentrated hydrochloric acid was added dropwise to dissolve it sufficiently.
(2) 0.3g of graphene oxide was dispersed in 200mL of deionized water, heated to 70 ℃ with stirring, and the solution was adjusted to pH 1 with 6mol/L hydrochloric acid solution.
(3) And slowly dripping the prepared bismuth salt solution into the graphene oxide solution, and reacting for 2 hours to obtain the graphene oxide-based pearlescent pigment dispersion liquid.
(4) Keeping the temperature unchanged, adding a reducing agent sodium sulfide into the pearlescent pigment dispersion liquid, continuously stirring and heating for 1 hour, and reducing the graphene oxide into graphene, wherein the mass ratio of the reducing agent to the graphene oxide is 1: 5. then cooling to room temperature, starting washing and suction filtration, and finally drying to obtain the bismuth oxychloride conductive pearlescent pigment powder with the graphene substrate, wherein the resistivity of the bismuth oxychloride conductive pearlescent pigment powder is 1.2 multiplied by 104Omega cm, good conductivity. Meanwhile, the refractive index of the conductive pearlescent pigment is changed from 2.15 of bismuth oxychloride to 2.21, and the refractive index is increased after the graphene is compounded.
Step 2, preparing a novel conductive film with a pearl effect:
adding the conductive pearlescent pigment prepared in the step 1 and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 20 wt% of the resin matrix, and in addition, the adopted conductive pearlescent pigmentThe curing agent is m-phenylenediamine, and the addition amount of the curing agent is 2 wt% of the resin matrix. Mixing them uniformly by mechanical stirring method, coating film, drying at 50 deg.C to obtain conductive film with good conductivity and resistivity of 0.8 × 104Ω·cm。
Example 2
Step 1, preparing the bismuth oxychloride conductive pearlescent pigment with the graphene as the base material:
(1) 8g of anhydrous bismuth nitrate was weighed into a beaker, and then 7.2mL of concentrated hydrochloric acid was added dropwise to dissolve it sufficiently.
(2) 0.6g of graphene oxide was dispersed in 200mL of deionized water, heated to 70 ℃ with stirring, and the solution was adjusted to pH 1 with 6mol/L hydrochloric acid solution.
(3) And slowly dripping the prepared bismuth salt solution into the graphene oxide solution, and reacting for 3 hours to obtain the graphene oxide-based pearlescent pigment dispersion liquid.
(4) Keeping the temperature unchanged, adding a reducing agent sodium sulfide into the pearlescent pigment dispersion liquid, continuously stirring and heating for 0.5 hour, and reducing the graphene oxide into graphene, wherein the mass ratio of the reducing agent to the graphene oxide is 1: 10. then cooling to room temperature, starting washing and suction filtration, and finally drying to obtain the bismuth oxychloride conductive pearlescent pigment powder with the graphene as the base material, wherein the resistivity of the bismuth oxychloride conductive pearlescent pigment powder is 3.7 multiplied by 104Ω · cm, the conductivity decreases. At this time, the refractive index of the conductive pearlescent pigment was changed from 2.15 to 1.97 of bismuth oxychloride itself, indicating that the brightness of the pearlescent pigment was decreased.
Step 2, preparing a novel conductive coating with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 20 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine in aromatic amines, and the addition amount of the m-phenylenediamine is 2 wt% of the resin matrix. Then, they were mixed uniformly by a mechanical stirring method, then they were coated with a film and dried at 50 ℃ to finally prepare a conductive film having a resistivity of 3.3X 104Ω·cm。
Example 3
Step 1, preparing the bismuth oxychloride conductive pearlescent pigment with the graphene as the base material:
(1) 6g of anhydrous bismuth nitrate was weighed into a beaker, and then 5.4mL of concentrated hydrochloric acid was added dropwise to dissolve it sufficiently.
(2) 0.1g of graphene oxide was dispersed in 200mL of deionized water, heated to 50 ℃ with stirring, and the solution was adjusted to pH 1 with 6mol/L hydrochloric acid solution.
(3) And slowly dripping the prepared bismuth salt solution into the graphene oxide solution, and reacting for 3 hours to obtain the graphene oxide-based pearlescent pigment dispersion liquid.
(4) Keeping the temperature unchanged, adding a reducing agent sodium sulfide into the pearlescent pigment dispersion liquid, continuously stirring and heating for 3 hours, and reducing the graphene oxide into graphene, wherein the mass ratio of the reducing agent to the graphene oxide is 1: 2. then cooling to room temperature, starting washing and suction filtration, and finally drying to obtain the bismuth oxychloride conductive pearlescent pigment powder with the graphene substrate, wherein the resistivity of the bismuth oxychloride conductive pearlescent pigment powder is 2.8 multiplied by 104Omega cm. At this time, the refractive index of the conductive pearlescent pigment is changed from 2.15 to 2.08 of bismuth oxychloride itself, indicating that the brightness of the pearlescent pigment is reduced.
Step 2, preparing a novel conductive coating with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 20 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine in aromatic amines, and the addition amount of the m-phenylenediamine is 2 wt% of the resin matrix. Then, they were mixed uniformly by a mechanical stirring method, then they were coated with a film and dried at 50 ℃ to finally prepare a conductive film having a resistivity of 2.4X 104Ω·cm。
Example 4
The preparation method of the conductive pearlescent pigment of step 1 in this example is the same as that of example 1.
Step 2, preparing a novel conductive coating with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 40 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine in aromatic amines, and the addition amount of the m-phenylenediamine is 4 wt% of the resin matrix. Then, the mixture was mixed uniformly by a mechanical stirring method, then, the mixture was coated with a film and dried at 70 ℃ to obtain a conductive film having a reduced conductivity and a resistivity of 0.9X 104Ω·cm。
Example 5
The preparation method of the conductive pearlescent pigment of step 1 in this example was the preparation method of example 1.
Step 2, preparing a novel conductive coating with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 10 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine in aromatic amines, and the addition amount of the m-phenylenediamine is 1 wt% of the resin matrix. Then, the mixture was mixed uniformly by a mechanical stirring method, then, the mixture was coated with a film and dried at 40 ℃ to finally obtain a conductive film having a weak conductivity and a specific resistance of 2.2X 104Ω·cm。
Comparative example 1
Step 1, preparing the bismuth oxychloride conductive pearlescent pigment with the graphene as the base material:
(1) 10g of anhydrous bismuth nitrate was weighed into a beaker, and then 9mL of concentrated hydrochloric acid was added dropwise to dissolve it sufficiently.
(2) 0.3g of graphene oxide was dispersed in 200mL of deionized water, heated to 70 ℃ with stirring, and the solution was adjusted to pH 1 with 6mol/L hydrochloric acid solution.
(3) And slowly dripping the prepared bismuth salt solution into the graphene oxide solution, and reacting for 2 hours to obtain the graphene oxide-based pearlescent pigment dispersion liquid.
(4) Adding no reducing agent, cooling to room temperature, washing, and vacuum filteringAnd drying to obtain the bismuth oxychloride conductive pearlescent pigment powder with the graphene substrate, wherein the resistivity of the bismuth oxychloride conductive pearlescent pigment powder is 5.7 multiplied by 105Omega cm, the conductivity is poor, at this time, the refractive index of the conductive pearlescent pigment is changed from 2.15 of bismuth oxychloride per se to 1.87, and compared with the case of adding the reducing agent, the brightness of the conductive material is reduced by not adding the reducing agent.
Step 2, preparing a novel conductive coating with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 20 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine in aromatic amines, and the addition amount of the m-phenylenediamine is 2 wt% of the resin matrix. Then, the mixture was mixed uniformly by a mechanical stirring method, then, the mixture was coated with a film and dried at 50 ℃ to obtain a conductive film having a resistivity of 5.2X 10 without much change in conductivity5Ω·cm。
Comparative example 2
Step 1, preparing a mica titanium conductive pearlescent pigment with graphene as a base material:
(1) 10g of mica titanium pearl powder was weighed out and dispersed in 200mL of deionized water, sufficiently dissolved, heated to 70 ℃ with stirring, and the solution was adjusted to pH 1 with 6mol/L hydrochloric acid solution.
(2) 0.3g of graphene oxide was added to the dispersion liquid, and reacted for 2 hours to obtain a graphene oxide-based pearlescent pigment dispersion liquid.
(3) Keeping the temperature unchanged, adding a reducing agent sodium sulfide into the pearlescent pigment dispersion liquid, continuously stirring and heating for 1 hour, and reducing the graphene oxide into graphene, wherein the mass ratio of the reducing agent to the graphene oxide is 1: 5. then cooling to room temperature, starting washing and suction filtration, and finally drying to obtain the bismuth oxychloride conductive pearlescent pigment powder with the graphene substrate, wherein the resistivity of the bismuth oxychloride conductive pearlescent pigment powder is 4.7 multiplied by 104Omega cm, poor conductivity. At this time, the refractive index of the conductive pearlescent pigment is changed from 2.52 to 2.61 of the mica titanium itself, which indicates that the brightness of the pearlescent pigment is increased.
Step 2, preparing a novel conductive film with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 20 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine, and the addition amount of the m-phenylenediamine is 2 wt% of the resin matrix. Mixing them uniformly by mechanical stirring method, coating film, drying at 50 deg.C to obtain conductive film with good conductivity and resistivity of 4.5 × 104Ω·cm。
Comparative example 3
Step 1, preparing the bismuth oxychloride conductive pearlescent pigment with vanadium pentoxide as a base material:
(1) 10g of anhydrous bismuth nitrate was weighed into a beaker, and then 9mL of concentrated hydrochloric acid was added dropwise to dissolve it sufficiently.
(2) 0.3g of vanadium pentoxide is dispersed in 200mL of deionized water, heated to 70 ℃ with stirring and the solution is brought to pH 1 with 6mol/L hydrochloric acid solution.
(3) Slowly dripping the prepared bismuth salt solution into the vanadium pentoxide aqueous solution, reacting for 2 hours to obtain vanadium pentoxide base pearlescent pigment dispersion liquid, cooling to room temperature, washing, filtering, and drying to obtain the graphene substrate bismuth oxychloride conductive pearlescent pigment powder with the resistivity of 8.9 multiplied by 104Omega cm, poor conductivity. At this time, the refractive index of the conductive pearlescent pigment is changed from 2.15 to 2.18 of bismuth oxychloride itself, which indicates that the brightness of the pearlescent pigment is increased but not greatly increased.
Step 2, preparing a novel conductive film with a pearl effect:
and (2) adding the conductive pearlescent pigment prepared in the step (1) and a curing agent into epoxy resin together, wherein the addition amount of the conductive pearlescent pigment is 20 wt% of the resin matrix, and the adopted curing agent is m-phenylenediamine, and the addition amount of the m-phenylenediamine is 2 wt% of the resin matrix. Mixing them uniformly by mechanical stirring method, coating film, drying at 50 deg.C to obtain conductive film with good conductivityThe resistivity thereof is 8.7X 104Ω·cm。
Claims (6)
1. A preparation method of conductive pearl powder with graphene as a base material is characterized by comprising the following steps:
(1) weighing 6-10g of anhydrous bismuth nitrate, putting the anhydrous bismuth nitrate into a beaker, and then dropwise adding 5.4-9mL of concentrated hydrochloric acid to fully dissolve the anhydrous bismuth nitrate to obtain a bismuth salt solution;
(2) dispersing graphene oxide in 200mL of deionized water, starting stirring and heating to 50-80 ℃, and adjusting the pH of the solution to =1 by using 6mol/L hydrochloric acid solution to obtain a graphene oxide solution; the using amount of the graphene oxide is 0.1-0.5% of the mass of the deionized water;
(3) slowly dripping the bismuth salt solution in the step (1) into the graphene oxide solution in the step (2), and reacting for 1-3 hours to obtain graphene oxide-based pearlescent pigment dispersion liquid;
(4) keeping the temperature unchanged, adding a reducing agent into the pearlescent pigment dispersion liquid obtained in the step (3), continuously stirring and heating for 0.5-2 hours, cooling to room temperature, washing, filtering, and finally drying to obtain conductive pearlescent powder taking graphene as a base material;
the conductive pearl powder is used for preparing a conductive film with a pearl effect.
2. The method for preparing conductive pearl powder by using graphene as a base material according to claim 1, wherein the reducing agent in the step (4) is sodium sulfide, and the mass ratio of the reducing agent to the graphene oxide is 1: 0.5-10.
3. The method for preparing conductive pearl powder using graphene as a substrate according to claim 1, wherein the conductive film is prepared by adding a curing agent and conductive pearl powder into resin, uniformly mixing to obtain a conductive coating with a pearl effect, coating the conductive coating, and drying to obtain the conductive film.
4. The method for preparing the conductive pearl powder by using the graphene as the base material according to claim 3, wherein the resin is epoxy resin; the curing agent is m-phenylenediamine.
5. The method for preparing conductive pearl powder by using graphene as a base material according to claim 3, wherein the amount of the curing agent is 1-4% of the mass of the resin, and the amount of the conductive pearl powder is 10-45% of the mass of the resin.
6. The method for preparing conductive pearl powder using graphene as base material according to claim 3, wherein the drying temperature is 30-70 ℃.
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