CN115197472A - Preparation method and application of functional cross-linked network modified nano talcum powder - Google Patents
Preparation method and application of functional cross-linked network modified nano talcum powder Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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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
- 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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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Abstract
The invention relates to a preparation method and application of talcum powder, in particular to a preparation method and application of functional cross-linked network modified nano talcum powder, which comprises the following steps: obtaining modified talcum powder A; obtaining modified talcum powder particle dispersion liquid B; the obtained polymer/inorganic talcum powder composite hydrogel is soaked in deionized water for swelling, unreacted monomers and other small molecular impurities are removed, and the functional cross-linked network modified talcum powder nano-particles are formed through freeze drying, crushing and granulation, so that the hydrophilic performance and the dispersion stability of the talcum powder particles are improved, the shell layer of the nano talcum powder in water can absorb water for swelling, and the surface of the shell layer is provided with carboxylic acid groups, carboxylate groups, catechol groups and amino groups, so that the nano talcum powder composite hydrogel can easily interact with other materials through static electricity, hydrogen bonds, van der Waals force and the like, and the hydrophilic performance and the dispersion stability of the talcum powder particles and the affinity of the talcum powder with a matrix resin material are improved.
Description
Technical Field
The invention relates to a preparation method and application of talcum powder, in particular to a preparation method and application of functional cross-linked network modified nano talcum powder.
Background
The talcum is a layered hydrous magnesium silicate, has good electrical insulation property, heat resistance and mechanical property, can improve the thermal expansion property and mechanical property of the composite material when being added into an organic material as a filling material, generally does not act with strong acid and strong base, and has good chemical stability; china has abundant talc reserves and low price, and various characteristics of the talc determine that the talc is widely applied to the fields of electronic packaging materials, military packaging materials, automobile instruments and the like as a filler. With the increasing demand of the above fields for fine miniaturization of products, the compatibility between the filler and the organic resin is in high demand.
Therefore, how to realize the cross-linked network structure on the surface of the talcum powder and further enhance the interface bonding capability of the talcum powder and other materials is a technical problem to be solved.
Disclosure of Invention
The invention aims to provide a preparation method and application of functional cross-linked network modified nano talcum powder, and aims to solve the technical problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of functional cross-linked network modified nano talcum powder comprises the following steps:
step a, dispersing 2g of talc powder in 120mL of ethanol, and ultrasonically dispersing the mixture for 30 minutes, and then mechanically stirring at 500rpm at room temperature; dissolving 5mL of gamma-methacryloxypropyltrimethoxysilane in 20mL of absolute ethanol, adding 2mL of deionized water, adjusting the pH to 4 by using dilute HCl, and carrying out prehydrolysis; slowly dripping gamma-methacryloxypropyl trimethoxy silane into an ethanol solution of the talcum powder, and refluxing for 6 hours at the temperature of 80 ℃; centrifuging at high speed, repeatedly washing with ethanol for 3 times, vacuum drying at 60 deg.C for 24 hr, and grinding to obtain modified pulvis Talci A;
step b, dissolving 2g of chitosan in 100mL of acetic acid aqueous solution to obtain a transparent uniform aqueous solution; dispersing 1.5g of silane modified talcum powder particles A in the 100mL of chitosan solution, performing ultrasonic dispersion, and adsorbing chitosan molecular chains to the surfaces of the silane modified talcum powder particles through electrostatic interaction to form core-shell talcum powder particles, so as to obtain modified talcum powder particle dispersion liquid B;
step C, dissolving 1.8g of acrylic acid in 10mL of sodium hydroxide aqueous solution, and reacting for 5-10 hours to obtain an aqueous solution C of acrylic acid and sodium acrylate; adding 10mL of modified talcum powder particle dispersion liquid B,0.2g of dopamine hydrochloride and 50mg of initiator ammonium persulfate into the solution C in sequence, then introducing nitrogen to remove oxygen, and magnetically stirring for 2 minutes to obtain a uniform dispersion solution; the temperature of the mixed dispersion was raised and,
after the reaction is finished, the obtained polymer/inorganic talcum powder composite hydrogel is soaked in deionized water for swelling, unreacted monomers and other small molecular impurities are removed, and the functional cross-linked network modified talcum powder nano-particles are formed through freeze drying, crushing and granulation and stored in a cool and dry place for later use.
Preferably, the nano-scale talcum powder has a particle size of 40-80nm.
Preferably, the mass fraction of the functionalized crosslinked network shell layer in the whole modified inorganic particle is 15-30%.
Preferably, the shell layer includes poly (acrylic acid-co-sodium acrylate), polydopamine and chitosan, and has a carboxylic acid group, a carboxylate group, a catechol group and an amino group on the surface.
Preferably, the high speed centrifugation in step a is centrifugation at 6000rpm for 5 minutes by a high speed centrifuge.
Preferably, the functional cross-linked network modified nano talcum powder can be applied to water-based paint and ink.
Preferably, the time for ultrasonic dispersion in step b is 60 to 90 minutes.
Preferably, the temperature of the mixed dispersion is raised to 80 ℃ in the step c to react for 12 hours.
Compared with the prior art, the invention has the beneficial effects that: the preparation method and application of the functional cross-linked network modified nano talcum powder improve the hydrophilic performance and dispersion stability of talcum powder particles, the shell layer of the nano talcum powder can absorb water and swell in water, and the surface of the shell layer is provided with carboxylic acid groups, carboxylate radical, catechol radicals and amino radicals, so that the shell layer is easy to interact with other materials through static electricity, hydrogen bonds, van der Waals force and the like, and the hydrophilic performance and dispersion stability of the talcum powder particles are improved, and the affinity of the talcum powder and a matrix resin material is improved.
Drawings
FIG. 1 is a schematic diagram of the present invention;
FIG. 2 is a scanning electron microscope image of a mixture of functional cross-linked network modified nano talc powder (using water as a dispersant) and water-based resin (using water as a solvent) in water-based paint or ink, which is freeze-dried to remove water.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
In specific implementation, the preparation method comprises the following steps:
step a, dispersing 2g of talcum powder in 120mL of ethanol, ultrasonically dispersing the mixture for 30 minutes, and then mechanically stirring at 500rpm at room temperature; dissolving 5mL of gamma-methacryloxypropyltrimethoxysilane in 20mL of absolute ethanol, adding 2mL of deionized water, adjusting the pH to 4 by using dilute HCl, and carrying out prehydrolysis; slowly dropping gamma-methacryloxypropyltrimethoxysilane into an ethanol solution of the talcum powder, and refluxing for 6 hours at 80 ℃; centrifuging at high speed (6000rpm, 5 min), washing with ethanol repeatedly for 3 times, vacuum drying at 60 deg.C for 24 hr, and grinding to obtain modified pulvis Talci A;
step b, dissolving 2g of chitosan in 100mL of acetic acid aqueous solution (the volume fraction of acetic acid is 5 percent) to obtain a transparent uniform aqueous solution; dispersing 1.5g of silane modified talcum powder particles A in the 100mL of chitosan solution, performing ultrasonic dispersion for 60-90 minutes, and adsorbing chitosan molecular chains to the surfaces of the silane modified talcum powder particles through electrostatic interaction to form core-shell talcum powder particles, so that the hydrophilic property and the dispersion stability of the talcum powder particles are improved, and the modified talcum powder particle dispersion liquid B is obtained in the step;
step C, dissolving 1.8g of acrylic acid in 10mL of sodium hydroxide aqueous solution (0.45 g), and reacting for 5-10 hours to obtain acrylic acid and sodium acrylate aqueous solution C; adding 10mL of modified talcum powder particle dispersion liquid B,0.2g of dopamine hydrochloride and 50mg of initiator ammonium persulfate into the solution C in sequence, then introducing nitrogen to remove oxygen, and magnetically stirring for 2 minutes to obtain a uniform dispersion solution; and (3) raising the temperature of the mixed dispersion liquid to 80 ℃ for reaction for 12 hours, after the reaction is finished, soaking the obtained polymer/inorganic talcum powder composite hydrogel into deionized water for swelling, removing unreacted monomers and other small molecular impurities, freeze-drying, crushing and granulating to form functional cross-linked network modified talcum powder nanoparticles, and storing the functional cross-linked network modified talcum powder nanoparticles in a cool and dry place for later use.
Wherein the grain size of the nano-scale talcum powder is 40-80nm; the mass fraction of the functionalized crosslinked network shell layer in the whole modified inorganic particle is 15-30%.
The shell layer comprises poly (acrylic acid-co-sodium acrylate), polydopamine and chitosan, and the surface of the shell layer is provided with carboxylic acid groups, carboxylate groups, catechol groups and amino groups; the high speed centrifugation in step a is performed by a high speed centrifuge at 6000rpm for 5 minutes.
The shell layer of the nano talcum powder in water can absorb water and swell, and the surface of the shell layer is provided with carboxylic acid groups, carboxylate groups, catechol groups and amino groups, so that the shell layer is easy to interact with other materials through static electricity, hydrogen bonds, van der Waals force and the like, and the shell layer is favorable for improving the hydrophilic performance and the dispersion stability of talcum powder particles and the affinity of the talcum powder and a matrix resin material.
The functional crosslinking network modified nano talcum powder can be applied to water-based paint and ink, and the crosslinking network structure on the surface of the talcum powder is beneficial to permeation of water-based micromolecular substances or auxiliary agents and diffusion of water-based resin molecules in a water-based paint or ink formula system, so that the interface bonding capability of the talcum powder and other materials is enhanced.
FIG. 2 is a scanning electron microscope picture of a water-based coating or ink obtained by mixing functional cross-linked network modified nano talc powder (using water as a dispersant) and water-based resin (using water as a solvent) in the water-based coating or ink to remove moisture after freeze drying.
As can be seen from FIG. 2, the particle size of the functionalized crosslinked network modified nano talcum powder is about 50nm, and the functionalized crosslinked network modified nano talcum powder and a surrounding aqueous resin film present a good adhesion appearance, which shows that the functionalized crosslinked network modified nano talcum powder and the surrounding aqueous resin film are combined together due to excellent interface interaction, even part of the modified talcum powder is connected through a thin line, and therefore, the diffusion and connection effects of the aqueous resin penetrating through the crosslinked network of the outer layer of the talcum powder are illustrated.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of functional cross-linked network modified nano talcum powder is characterized by comprising the following steps:
step a, dispersing 2g of talcum powder in 120mL of ethanol, ultrasonically dispersing the mixture for 30 minutes, and then mechanically stirring at 500rpm at room temperature; dissolving 5mL of gamma-methacryloxypropyltrimethoxysilane in 20mL of absolute ethanol, adding 2mL of deionized water, adjusting the pH to 4 by using dilute HCl, and carrying out prehydrolysis; slowly dropping gamma-methacryloxypropyltrimethoxysilane into an ethanol solution of the talcum powder, and refluxing for 6 hours at 80 ℃; centrifuging at high speed, repeatedly washing with ethanol for 3 times, vacuum drying at 60 deg.C for 24 hr, and grinding to obtain modified pulvis Talci A;
step b, dissolving 2g of chitosan in 100mL of acetic acid aqueous solution to obtain a transparent uniform aqueous solution; dispersing 1.5g of silane modified talcum powder particles A in the 100mL of chitosan solution, performing ultrasonic dispersion, and adsorbing chitosan molecular chains to the surfaces of the silane modified talcum powder particles through electrostatic interaction to form core-shell structured talcum powder particles, so as to obtain modified talcum powder particle dispersion liquid B;
step C, dissolving 1.8g of acrylic acid in 10mL of sodium hydroxide aqueous solution, and reacting for 5-10 hours to obtain an aqueous solution C of acrylic acid and sodium acrylate; adding 10mL of modified talcum powder particle dispersion liquid B,0.2g of dopamine hydrochloride and 50mg of initiator ammonium persulfate into the solution C in sequence, then introducing nitrogen to remove oxygen, and magnetically stirring for 2 minutes to obtain a uniform dispersion solution; and (3) raising the temperature of the mixed dispersion liquid, immersing the obtained polymer/inorganic talcum powder composite hydrogel into deionized water for swelling after the reaction is finished, removing unreacted monomers and other micromolecular impurities, performing freeze drying, crushing and granulating to form functional cross-linked network modified talcum powder nano-particles, and storing the nano-particles in a cool and dry place for later use.
2. The method for preparing the functional crosslinking network modified nanometer talcum powder of claim 1, wherein the grain size of the nanometer talcum powder is 40-80nm.
3. The method for preparing the functional cross-linked network modified nano talcum powder as claimed in claim 1, wherein the mass fraction of the functional cross-linked network shell layer in the whole modified inorganic particles is 15-30%.
4. The method for preparing the functional cross-linked network modified nano talc powder of claim 3, wherein the shell layer comprises poly (acrylic acid-co-sodium acrylate), polydopamine and chitosan, and has carboxylic acid group, carboxylate group, catechol group and amino group on the surface.
5. The method for preparing the functional crosslinking network modified nano talcum powder according to claim 1, wherein the high-speed centrifugation in the step a is performed for 5 minutes at 6000rpm by a high-speed centrifuge.
6. The use of the functional cross-linked network modified nano-talc according to claim 1, wherein the functional cross-linked network modified nano-talc is applicable to water-based paints and inks.
7. The use of the functional crosslinked network modified nano talc according to claim 1, wherein the time of ultrasonic dispersion in step b is 60-90 minutes.
8. The use of the functional crosslinked network modified nano-talc according to claim 1, wherein the temperature of the mixed dispersion is raised to 80 ℃ for 12 hours in step c.
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| CN115537088A (en) * | 2022-11-07 | 2022-12-30 | 苏州优矿塑新材料股份有限公司 | Coating containing novel cross-linked network modified nano talcum powder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115537088A (en) * | 2022-11-07 | 2022-12-30 | 苏州优矿塑新材料股份有限公司 | Coating containing novel cross-linked network modified nano talcum powder and preparation method thereof |
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