CN115322611A - Lamellar kaolin material and preparation method and application thereof - Google Patents
Lamellar kaolin material and preparation method and application thereof Download PDFInfo
- Publication number
- CN115322611A CN115322611A CN202211029759.3A CN202211029759A CN115322611A CN 115322611 A CN115322611 A CN 115322611A CN 202211029759 A CN202211029759 A CN 202211029759A CN 115322611 A CN115322611 A CN 115322611A
- Authority
- CN
- China
- Prior art keywords
- kaolin
- lamellar
- temperature
- time
- drying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 239000005995 Aluminium silicate Substances 0.000 title claims abstract description 103
- 235000012211 aluminium silicate Nutrition 0.000 title claims abstract description 103
- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000004913 activation Effects 0.000 claims abstract description 29
- 238000000576 coating method Methods 0.000 claims abstract description 27
- 238000000227 grinding Methods 0.000 claims abstract description 26
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 238000009830 intercalation Methods 0.000 claims abstract description 18
- 230000002687 intercalation Effects 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 230000010355 oscillation Effects 0.000 claims abstract description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000138 intercalating agent Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 3
- 241000276425 Xiphophorus maculatus Species 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 2
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 description 48
- 239000003960 organic solvent Substances 0.000 description 25
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 19
- 239000006185 dispersion Substances 0.000 description 19
- 239000002904 solvent Substances 0.000 description 18
- 239000010410 layer Substances 0.000 description 17
- 239000002245 particle Substances 0.000 description 17
- 229910052622 kaolinite Inorganic materials 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000011324 bead Substances 0.000 description 12
- 239000012153 distilled water Substances 0.000 description 12
- 238000001878 scanning electron micrograph Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 8
- 238000005119 centrifugation Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 6
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229920006334 epoxy coating Polymers 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- CVXBEEMKQHEXEN-UHFFFAOYSA-N carbaryl Chemical compound C1=CC=C2C(OC(=O)NC)=CC=CC2=C1 CVXBEEMKQHEXEN-UHFFFAOYSA-N 0.000 description 1
- 229960005286 carbaryl Drugs 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- 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
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
-
- 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
- C08K7/00—Use of ingredients characterised by shape
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention belongs to the technical field of inorganic materials, and particularly relates to a lamellar kaolin material as well as a preparation method and application thereof. The preparation method of the lamellar kaolin material comprises the following steps: s1, performing high-temperature activation on kaolin to obtain activated kaolin; s2, mixing and grinding the intercalation agent and the activated kaolin to obtain slurry; and S3, oscillating and ultrasonically treating the slurry to obtain the lamellar kaolin material. According to the invention, the kaolin is subjected to high-temperature activation treatment, so that the activity of the kaolin is improved, impurities in the raw materials are removed, the influence of the impurities in the raw materials on the subsequent preparation process is avoided, the intercalation of the intercalation agent is more facilitated after the high-temperature activation, the intercalation rate is improved, and the agglomeration of lamellar kaolin materials is reduced; and the grinding period can be shortened by the oscillation and ultrasonic treatment, and the production efficiency is improved. The lamellar kaolin prepared by the method disclosed by the invention is uniform in distribution, free of stacking phenomenon, good in dispersity in the coating and capable of effectively enhancing the air tightness of the coating.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a lamellar kaolin material as well as a preparation method and application thereof.
Background
Kaolin has a wide range of applications in industry, is an important raw material in many fields such as the production of ceramics, cement, rubber, polymers, etc., and its main mineral is kaolinite, which belongs to the group of 1: a layer 1 of a layered silicate, the crystal mainly consisting of silicon-oxygen tetrahedra and aluminum-oxygen tetrahedra, wherein the silicon-oxygen tetrahedra are linked in a two-dimensional direction in a manner of sharing a vertex angle to form a grid layer in a hexagonal arrangement, and the unshared vertex oxygen of each silicon-oxygen tetrahedra faces one side; the oxygen peaks of the common silicon oxygen tetrahedral layer consisting of a silicon oxygen tetrahedral layer and an aluminum oxygen octahedral layer constitute 1: type 1 unit layer. The kaolinite layer is neutral and is linked every two consecutive layers by hydrogen bonds, three of the four hydroxyl groups linked to the octahedral sheets are located on the inner surface of the layer, one on the layer, these inner surface hydroxyl groups are almost perpendicular to the tetrahedral sheets of the next layer, resulting in the formation of strong hydrogen bonds.
Kaolinite is an inexpensive additive that forms stable dispersions and improves the properties of the material, and the thickness of the kaolin particles significantly affects its dispersion properties in the material, and in the industry, separation of the kaolinite particles into platelets, also known as "delamination", is achieved by conventional mechanical milling or stirring. It requires cutting along a vertical plane between layers of kaolinite to degrade the kaolinite crystal structure, thereby increasing the specific surface area, and grinding the kaolinite chips for a short time can cause cracking along the basal plane and simultaneously increase the specific surface area. However, prolonged grinding can result in the formation of agglomerates with an amorphous surface layer and a reduction in specific surface area.
There have been many methods for inserting and peeling kaolinite, in which organic compounds having strong polarity such as formamide, potassium acetate, and dimethyl sulfoxide are inserted into the layered kaolinite particles sandwiched between the layered kaolinite particles, and at the same time, ultrasonic methods, mechanical pulverization methods, and high-speed stirring methods are combined to weaken hydrogen bonds between layers of kaolinite, so that the kaolinite layer is easily displaced, thereby peeling kaolinite. At present, the kaolin stripping method generally consumes a long time, needs complex pretreatment, and the pretreatment condition is often harsh, so that the stripping type lamellar kaolin material is difficult to effectively prepare.
Disclosure of Invention
The present invention has been made to solve at least one of the above-mentioned problems occurring in the prior art. Therefore, the invention provides a preparation method of lamellar kaolin, and the obtained kaolin is distributed in a lamellar manner, and has small layer thickness and large specific surface area.
The invention also provides a lamellar kaolin material obtained by the preparation method and application thereof.
In a first aspect of the present invention, a method for preparing a lamellar kaolin material, comprises the steps of:
s1, performing high-temperature activation on kaolin to obtain activated kaolin;
s2, mixing and grinding the intercalation agent and the activated kaolin to obtain slurry;
and S3, oscillating and ultrasonically treating the slurry to obtain the lamellar kaolin material.
According to the first aspect of the present invention, at least the following advantages are obtained:
according to the invention, the kaolin is subjected to high-temperature activation treatment, so that the activity of the kaolin is improved, impurities in the raw materials are removed, the influence of the impurities in the raw materials on the subsequent preparation process is avoided, the intercalation of the intercalation agent is more facilitated after the kaolin is activated, the intercalation rate is improved, and the agglomeration of lamellar kaolin materials is reduced; and the grinding period can be shortened by oscillating and ultrasonic processing, the integrity of the kaolin material crystal is ensured, and the production efficiency is improved.
Preferably, in step S1, the temperature of the high-temperature activation is 300 to 700 ℃, more preferably 400 to 550 ℃; the time for high-temperature activation is 4 to 15 hours, and more preferably 6 to 12 hours.
Preferably, step S1 further comprises a pretreatment of washing, centrifuging, and drying the kaolin.
Preferably, the solvent used for washing is water, and the mass volume ratio of the kaolin to the solvent is 0.05-0.5 g:1mL, more preferably 0.1 to 0.3g:1mL.
Preferably, the rotating speed of the centrifugal treatment is 1000-7000 r/min, more preferably 2000-5000 r/min; the time for the centrifugation treatment is 2 to 30min, more preferably 5 to 10min.
Preferably, the drying temperature is 40-90 ℃, and more preferably 65-70 ℃; the drying time is 15 to 50 hours, and more preferably 24 to 36 hours.
Preferably, in step S2, the grinding is ball milling, and the rotation speed of the grinding is 500 to 7000r/min, more preferably 1000 to 6000r/min, and further preferably 2000 to 5000r/min; the polishing time is 2 to 12 hours, more preferably 4 to 8 hours.
Preferably, in step S2, the mass-to-volume ratio of the activated kaolin to the intercalating agent is 0.05 to 0.4g:1mL, more preferably 0.1 to 0.25g:1mL.
Preferably, in step S2, the intercalating agent is a strongly polar organic solvent including at least one of formamide, dimethyl sulfoxide, and dimethylformamide.
Preferably, the grinding media comprises zirconia particles; the particle size of the grinding media is 0.1 to 2mm, more preferably 0.2 to 1.4mm, and still more preferably 0.2 to 0.8mm.
Preferably, the mass volume ratio of the grinding medium to the intercalating agent is 0.05-0.5 g:1mL, more preferably 0.1 to 0.25g:1mL.
Preferably, in step S3, the frequency of the oscillation treatment is 20 to 400r/min, more preferably 50 to 200r/min; the temperature of the oscillation treatment is 20 to 80 ℃, and the temperature is preferably 40 to 60 ℃; the time for the shaking treatment is 2 to 12 hours, more preferably 4 to 10 hours.
Preferably, in the step S3, the power of the ultrasonic treatment is 100 to 1000w, more preferably 200 to 800w; the time of the ultrasonic treatment is 10 to 30min, more preferably 10 to 20min.
Preferably, in step S3, a solvent is further added after the ultrasonic treatment is finished, and the treatment of centrifuging, drying and removing the intercalation agent and the solvent at high temperature is performed; the rotating speed of the centrifugal treatment is 2000-7000 r/min, and more preferably 3000-5000 r/min; the time of the centrifugal treatment is 5 to 50min, and more preferably 10 to 30min; the drying temperature is 30-90 ℃, and more preferably 60-80 ℃; the drying time is 20 to 40 hours, and more preferably 24 to 30 hours.
Preferably, the temperature of the high-temperature intercalation agent removing and solvent treatment is 150-500 ℃, and more preferably 200-300 ℃; the time is 1 to 8 hours, more preferably 2 to 5 hours.
Preferably, the solvent is at least one of ethanol, propanol and water.
In a second aspect of the present invention, a lamellar kaolin material prepared by the above preparation method is provided.
Preferably, the thickness of the lamellar kaolin material is from 20 to 60nm, more preferably from 30 to 50nm, even more preferably from 39.7 to 46.2nm.
Preferably, the platelet-like kaolin material has a particle size of from 500 to 1600nm, more preferably from 800 to 1500nm, even more preferably from 902 to 1402nm.
Preferably, the specific surface area of the lamellar kaolin material is 60 to 150m 2 Per g, more preferably 80 to 100m 2 Per g, more preferably 89.18 to 93.86m 2 /g。
In a third aspect of the invention, the use of the platelet-shaped kaolin material in a coating.
Preferably, the coating comprises at least one of an epoxy coating, an acrylic coating, a polyurethane coating, and a latex coating.
Preferably, the coating is a low viscosity epoxy resin manufactured by carbaryl paints limited.
Preferably, the mass percentage of the lamellar kaolin in the coating is 0.1-5%, and more preferably 0.5-3%.
Preferably, the thickness of the coating is 1 to 10mm, more preferably 2 to 5mm.
Compared with the prior art, the invention at least has the following beneficial effects:
1. according to the invention, the kaolin is activated at high temperature, so that the activity of the kaolin is improved, impurities in the raw materials are removed, the influence of the impurities on the subsequent preparation process is avoided, the intercalation of the intercalating agent is more facilitated after the kaolin is activated, the intercalation rate is improved, and the agglomeration phenomenon is reduced; the oscillation and ultrasonic treatment can effectively shorten the grinding period, avoid the damage of the crystal structure of the kaolin material due to long-time grinding, keep the integrity of the crystal and improve the production effect.
2. The lamellar kaolin prepared by the method is uniform in distribution, free of stacking phenomenon, small in thick layer and granularity and large in specific surface area.
3. The lamellar kaolin disclosed by the invention has good dispersibility in the coating, and can effectively enhance the air tightness of the coating.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a scanning electron micrograph of a kaolin material prepared in comparative example 1;
FIG. 2 is a scanning electron micrograph of a lamellar kaolin material prepared in example 1 according to the invention;
FIG. 3 is a scanning electron micrograph of a lamellar kaolin material prepared in example 2 according to the invention;
FIG. 4 is a scanning electron micrograph of a lamellar kaolin material prepared in example 3 according to the invention;
FIG. 5 is a scanning electron micrograph of a lamellar kaolin material prepared in example 4 according to the invention;
FIG. 6 is a scanning electron micrograph of a coating made from the kaolin material of comparative example 1 of the present invention;
FIG. 7 is a scanning electron micrograph of a coating made from the kaolin material of example 2 of the present invention.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Unless otherwise indicated, the raw materials used in the present invention are all those commonly used in the art, and the test methods are all those commonly used in the art.
Example 1
Washing untreated kaolin with distilled water, and carrying out centrifugal drying treatment on the slurry, wherein the dispersion concentration of the kaolin in the distilled water is 0.1g/mL, the centrifugal rotation speed is 2000r/min, the centrifugal time is 5min, the drying temperature is 60 ℃, and the drying time is 24h. After centrifugal drying, high-temperature activation treatment is carried out, the temperature of high-temperature activation is 400 ℃, and the time of high-temperature activation is 6 hours.
Adding an organic solvent and activated kaolin into a ball mill, simultaneously adding a grinding medium of zirconia beads, wherein the concentration of the kaolin in the organic solvent is 0.1g/mL, the particle size of the zirconia beads is 0.2mm, the concentration of the grinding medium in the organic solvent is 0.1g/mL, and then stirring for 4 hours at a rotating speed of 3000r/min, wherein the organic solvent is formamide. And then filtering the ball-milled slurry, oscillating at a certain temperature, and performing secondary crushing and dispersion by using ultrasound, wherein the oscillation frequency of the filtered solution is 200r/min, the oscillation temperature is 60 ℃, the time is 10h, the power of ultrasonic crushing and dispersion is 200w, and the ultrasonic time is 10min.
And adding ethanol into the solution after ultrasonic treatment, centrifuging and drying, and removing the solvent at high temperature to obtain the peeled lamellar kaolin material. The centrifugation speed is 3000r/min, the centrifugation time is 10min, the drying temperature is 70 ℃, the drying time is 24h, the temperature for removing the solvent at high temperature is 200 ℃, and the time is 2h. The microstructure of the prepared exfoliated lamellar kaolin material is shown in figure 2.
Example 2
Washing untreated kaolin with distilled water, and carrying out centrifugal drying treatment on the slurry, wherein the dispersion concentration of the kaolin in the distilled water is 0.2g/mL, the centrifugal rotation speed is 4000r/min, the centrifugal time is 10min, the drying temperature is 70 ℃, and the drying time is 36h. After centrifugal drying, high-temperature activation treatment is carried out, the temperature of high-temperature activation is 500 ℃, and the time of high-temperature activation is 8 hours.
Adding an organic solvent and activated kaolin into a ball mill, simultaneously adding a grinding medium of zirconia beads, wherein the concentration of the kaolin in the organic solvent is 0.2g/mL, the particle size of the zirconia beads is 0.6mm, and the concentration of the grinding medium in the organic solvent is 0.12g/mL, and then stirring for 6h at the rotating speed of 2000r/min, wherein the organic solvent is dimethyl sulfoxide. And then filtering the ball-milled slurry, oscillating at a certain temperature, and performing secondary crushing and dispersion by using ultrasound, wherein the oscillation frequency of the filtered solution is 100r/min, the oscillation temperature is 40 ℃, the time is 8h, the power of ultrasonic crushing and dispersion is 400w, and the ultrasonic time is 20min.
And adding ethanol into the solution after ultrasonic treatment, centrifugally drying, and removing the solvent at high temperature to obtain the peeled lamellar kaolin material. The centrifugal speed is 4000r/min, the centrifugal time is 15min, the drying temperature is 60 ℃, the drying time is 30h, the temperature for removing the solvent at high temperature is 300 ℃, and the time is 4h. The microstructure of the prepared exfoliated lamellar kaolin material is shown in figure 3.
Example 3
Washing untreated kaolin with distilled water, and carrying out centrifugal drying treatment on the slurry, wherein the dispersion concentration of the kaolin in the distilled water is 0.15g/mL, the centrifugal rotation speed is 3000r/min, the centrifugal time is 5min, the drying temperature is 65 ℃, and the drying time is 24h. After centrifugal drying, high-temperature activation treatment is carried out, wherein the high-temperature activation temperature is 450 ℃, and the high-temperature activation time is 10 hours.
Adding an organic solvent and activated kaolin into a ball mill, simultaneously adding a grinding medium of zirconia beads, wherein the concentration of the kaolin in the organic solvent is 0.15g/mL, the particle size of the zirconia beads is 0.4mm, the concentration of the grinding medium in the organic solvent is 0.15g/mL, and then stirring for 4 hours at the rotating speed of 5000r/min, wherein the organic solvent is formamide. And then filtering the ball-milled slurry, oscillating at a certain temperature, and performing secondary crushing and dispersion by using ultrasound, wherein the oscillation frequency of the filtered solution is 150r/min, the oscillation temperature is 40 ℃, the time is 6h, the power of ultrasonic crushing and dispersion is 600w, and the ultrasonic time is 20min.
And adding ethanol into the solution after ultrasonic treatment, centrifugally drying, and removing the solvent at high temperature to obtain the peeled lamellar kaolin material. The centrifugal speed is 4000r/min, the centrifugal time is 30min, the drying temperature is 70 ℃, the drying time is 30h, the temperature for removing the solvent at high temperature is 260 ℃, and the time is 5h. The microstructure of the prepared exfoliated lamellar kaolin material is shown in figure 4.
Example 4
Washing untreated kaolin with distilled water, and carrying out centrifugal drying treatment on the slurry, wherein the dispersion concentration of the kaolin in the distilled water is 0.3g/mL, the centrifugal rotation speed is 5000r/min, the centrifugal time is 10min, the drying temperature is 70 ℃, and the drying time is 24h. After centrifugal drying, high-temperature activation treatment is carried out, wherein the high-temperature activation temperature is 550 ℃, and the high-temperature activation time is 12 hours.
Adding an organic solvent and activated kaolin into a ball mill, simultaneously adding a grinding medium of zirconium oxide beads, wherein the concentration of the kaolin in the organic solvent is 0.25g/mL, the particle size of the zirconium oxide beads is 0.8mm, and the concentration of the grinding medium in the organic solvent is 0.25g/mL, and then stirring for 8 hours at the rotating speed of 2500r/min, wherein the organic solvent is dimethyl sulfoxide. And then filtering the ball-milled slurry, oscillating at a certain temperature, and performing secondary crushing and dispersion by using ultrasound, wherein the oscillation frequency of the filtered solution is 50r/min, the oscillation temperature is 50 ℃, the time is 4h, the power of ultrasonic crushing and dispersion is 800w, and the ultrasonic time is 20min.
And adding ethanol into the solution after ultrasonic treatment, centrifugally drying, and removing the solvent at high temperature to obtain the peeled sheet-shaped layered kaolin material. The centrifugal speed is 5000r/min, the centrifugal time is 20min, the drying temperature is 80 ℃, the drying time is 30h, the temperature for removing the solvent at high temperature is 280 ℃, and the time is 5h. The microstructure of the prepared exfoliated lamellar kaolin material is shown in figure 5.
Comparative example 1
The difference between the comparative example and the example 1 is that the high-temperature activation treatment is omitted, and the specific process is as follows:
washing untreated kaolin with distilled water, and carrying out centrifugal drying treatment on the slurry, wherein the dispersion concentration of the kaolin in the distilled water is 0.1g/mL, the centrifugal rotation speed is 2000r/min, the centrifugal time is 5min, the drying temperature is 60 ℃, and the drying time is 24h.
Adding an organic solvent and dried kaolin into a ball mill, simultaneously adding a grinding medium zirconia beads, wherein the concentration of the kaolin in the organic solvent is 0.1g/mL, the particle size of the zirconia beads is 0.2mm, the concentration of the grinding medium in the organic solvent is 0.1g/mL, and then stirring for 4h at the rotating speed of 3000r/min, wherein the organic solvent is formamide. And then filtering the ball-milled slurry, oscillating at a certain temperature, and performing secondary crushing and dispersion by using ultrasound, wherein the oscillation frequency of the filtered solution is 200r/min, the oscillation temperature is 60 ℃, the time is 10h, the power of ultrasonic crushing and dispersion is 200w, and the ultrasonic time is 10min.
And adding ethanol into the ultrasonic solution, centrifuging, drying, and removing the solvent at high temperature to obtain the kaolin material. The centrifugation speed is 3000r/min, the centrifugation time is 10min, the drying temperature is 70 ℃, the drying time is 24h, the temperature for removing the solvent at high temperature is 200 ℃, and the time is 2h. The microstructure of the prepared kaolin material is shown in figure 1.
Comparative example 2
The difference between the comparative example and the example 1 is that the oscillation and ultrasonic treatment are omitted, and the specific process is as follows:
washing untreated kaolin with distilled water, and carrying out centrifugal drying treatment on the slurry, wherein the dispersion concentration of the kaolin in the distilled water is 0.1g/mL, the centrifugal rotation speed is 2000r/min, the centrifugal time is 5min, the drying temperature is 60 ℃, and the drying time is 24h. After centrifugal drying, high-temperature activation treatment is carried out, the temperature of high-temperature activation is 400 ℃, and the time of high-temperature activation is 6 hours.
Adding an organic solvent and activated kaolin into a ball mill, simultaneously adding a grinding medium zirconia beads, wherein the concentration of the kaolin in the organic solvent is 0.1g/mL, the particle size of the zirconia beads is 0.2mm, and the concentration of the grinding medium in the organic solvent is 0.1g/mL, and then stirring for 4h at the rotating speed of 3000r/min, wherein the organic solvent is formamide. And adding ethanol into the ball-milled solution, centrifuging, drying, and removing the solvent at high temperature to obtain the kaolin material. The centrifugation speed is 3000r/min, the centrifugation time is 10min, the drying temperature is 70 ℃, the drying time is 24h, the temperature for removing the solvent at high temperature is 200 ℃, and the time is 2h.
Test examples
This test example tests the lamellar kaolin prepared in the examples and comparative examples and its performance in coatings. Wherein:
1. surface topography of lamellar Kaolin Material
TABLE 1 Properties of Kaolin Material prepared according to examples 1-4 of the present invention and comparative examples 1-2
Item | Rate of intercalation | Specific surface area (m) 2 /g) | Particle size (nm) | Thickness (nm) |
Comparative example 1 | 0% | 27.93 | 3527 | 589.4 |
Comparative example 2 | 55.7% | 54.37 | 765.8 | 157.7 |
Example 1 | 100% | 89.18 | 902.6 | 46.2 |
Example 2 | 100% | 90.16 | 985.3 | 43.8 |
Example 3 | 100% | 93.86 | 1117 | 39.7 |
Example 4 | 100% | 88.57 | 1402 | 45.1 |
The method for testing the intercalation rate comprises the following steps: the X-ray diffraction test is carried out on the obtained material to obtain an X-ray diffraction pattern, and the intercalation ratio is calculated according to the intensity of the newly added characteristic diffraction peak and the main peak, wherein the formula is as follows:
E i is the intercalation rate of organic molecules, I kc Is a new peak intensity of low-angle diffraction of an organic matter-kaolinite complex, I koc The intensity of the original main characteristic diffraction peak of the kaolinite after intercalation.
Fig. 1 is an SEM image of kaolin prepared by omitting the high-temperature activation treatment of a comparative example, and fig. 2 to 5 are SEM images of the lamellar kaolin materials prepared in examples 1 to 4, respectively. As can be seen from Table 1 and FIGS. 2 to 5, the kaolin material prepared by the invention is dispersed in a lamellar shape, the thickness is 39.7 to 46.2nm, the particle size is 902.6 to 1402nm, the specific surface area is 88.57 to 93.86m 2 (ii) in terms of/g. As can be seen from fig. 1, in comparative example 1, the high temperature activation treatment is omitted, and the organic solvent cannot be intercalated into the kaolin material which is not subjected to high temperature activation, so that the finally prepared kaolin material has a layered structure with thicker stacked layers, the thickness of the kaolin material is more than 10 times that of the kaolin material, and the particle size of the kaolin material is also obviously increased. Comparative example 2 omits the kaolin material that vibration, ultrasonic treatment obtained is less in granularity, the thickness is great, and kaolin crystal structure integrality is relatively poor, demonstrates that the subsequent treatment of vibration ultrasound can improve its preparation efficiency, guarantees the integrality of peeling type piece stratiform kaolin material crystal structure, shortens the cycle of ball-milling technology earlier stage simultaneously.
2. Coating Properties
0.5g of kaolin material is added into 100g of epoxy resin coating (Carboguard 890 epoxy coating produced by Karaobao paint Co., ltd.), the mixture is uniformly mixed, the surface of concrete is coated, and after natural drying and curing are carried out for 10 days, a coating with the film thickness of 2 mm-5 mm is obtained.
The dispersion of the kaolin materials prepared in comparative example 1 and example 2 in the epoxy resin coating is shown in fig. 6 to 7. As can be seen from fig. 6, the kaolin material prepared in comparative example 1 has poor dispersibility in the epoxy coating, while the kaolin material prepared in the invention in example 2 has good dispersibility and can be uniformly dispersed in the epoxy resin without particle agglomeration.
Table 2 comparison of coating properties with addition of the kaolin materials of comparative example 1 and example 2
Item | Oxygen transmission rate/cc/m 2 day | Tensile Strength/MPa |
Coating + comparative example 1 | 8.957 | 3.89 |
Coating + example 2 | 4.965 | 5.13 |
As can be seen from Table 2, since the lamellar kaolin prepared according to the present invention is uniformly dispersed in the epoxy resin, the resulting coating has good air impermeability and an oxygen permeability of only 4.965cc/m 2 day, while the kaolin of comparative example 1, due to agglomeration, gave coatings with oxygen permeability significantly higher than that of the present invention, up to 8.957cc/m 2 day. Meanwhile, the specific surface area of the lamellar material is small, the coating has good wrapping performance, and the drawing strength of the coating added in the embodiment 2 is 5.13MPa, so that the drawing strength is obviously improved compared with the coating added in the comparative example 1.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. The preparation method of the lamellar kaolin material is characterized by comprising the following steps:
s1, performing high-temperature activation on kaolin to obtain activated kaolin;
s2, mixing and grinding the activated kaolin and intercalation agent soil to obtain slurry;
and S3, oscillating and ultrasonically treating the slurry to obtain the lamellar kaolin material.
2. The method according to claim 1, wherein the temperature of the high-temperature activation in step S1 is 300 to 700 ℃.
3. The method according to claim 2, wherein the high temperature activation time in step S1 is 4 to 15 hours.
4. The preparation method according to claim 1, wherein in step S2, the mass-to-volume ratio of the activated kaolin to the intercalating agent is 0.05 to 0.4g:1mL.
5. The method of claim 1, wherein in step S2, the intercalant comprises at least one of formamide, dimethyl sulfoxide, and dimethylformamide.
6. The method according to claim 1, wherein in step S3, the frequency of the oscillation treatment is 20 to 400r/min.
7. The method according to claim 1, wherein in step S3, the power of the ultrasonic treatment is 100 to 1000w.
8. The method according to claim 7, wherein the time for the ultrasonic treatment in step S3 is 10 to 30min.
9. A platelet-shaped kaolin material, characterized in that it is obtained by a process according to any one of claims 1 to 8.
10. Use of the platy kaolin material of claim 9 in a coating.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211029759.3A CN115322611A (en) | 2022-08-25 | 2022-08-25 | Lamellar kaolin material and preparation method and application thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211029759.3A CN115322611A (en) | 2022-08-25 | 2022-08-25 | Lamellar kaolin material and preparation method and application thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115322611A true CN115322611A (en) | 2022-11-11 |
Family
ID=83928629
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202211029759.3A Pending CN115322611A (en) | 2022-08-25 | 2022-08-25 | Lamellar kaolin material and preparation method and application thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115322611A (en) |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106517224A (en) * | 2016-11-28 | 2017-03-22 | 河南理工大学 | Preparation method of kaolinite nanosheets |
-
2022
- 2022-08-25 CN CN202211029759.3A patent/CN115322611A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106517224A (en) * | 2016-11-28 | 2017-03-22 | 河南理工大学 | Preparation method of kaolinite nanosheets |
Non-Patent Citations (2)
Title |
---|
李晓旭等: "高岭土插层与剥离影响因素的研究", 《应用化工》 * |
王菊华(主编), 中国地质大学出版社有限责任公司 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111233509B (en) | Vermiculite nanosheet and preparation method thereof | |
CN110330012A (en) | The preparation method of high concentration graphene aqueous liquid dispersion and self-dispersing graphene powder | |
CN106010043A (en) | Aqueous electromagnetic wave absorption coating based on graphene and carbonyl iron composite material and preparation method of aqueous electromagnetic wave absorption coating | |
CN103112867A (en) | Activating treatment method for sericite | |
CN109666370A (en) | A kind of conductive anti-corrosion coating and preparation method thereof containing graphene | |
CN115028894B (en) | Preparation method of composite slurry for preparing two-dimensional mica composite film, two-dimensional mica composite film and preparation method thereof | |
CN109111798A (en) | Water-repellent paint and preparation method thereof | |
CN110423379B (en) | Magnesium hydroxide/graphene sheet composite flame retardant and preparation method thereof | |
CN108410017A (en) | A kind of preparation method for the high-dispersion barium sulfate composite material in plastic matrix | |
CN115322611A (en) | Lamellar kaolin material and preparation method and application thereof | |
CN116377756B (en) | Method for improving interfacial bonding performance of mica and reinforced fiber | |
CN110407212B (en) | High-dispersity nano carbonate gel as well as preparation method and application thereof | |
US20230339760A1 (en) | Method for preparing graphene by mechanical exfoliation and application thereof | |
CN110482602B (en) | Preparation method of TiO 2/wollastonite compound | |
CN104194193A (en) | Special filler for antistatic wear-resistant PVC (polyvinyl chloride) tube and preparation method thereof | |
CN107012728B (en) | A kind of preparation method for facing paper production sun-screening agent | |
CN111073351A (en) | Preparation method of high-weather-resistance and high-dispersion plastic color master batch titanium dioxide pigment | |
CN112499622B (en) | Silicon dioxide and graphene composite powder material and preparation method and application thereof | |
CN107266709B (en) | A kind of plastics enhancing graphene ca silicate fibre composite material and preparation method | |
CN105883839B (en) | A kind of method for preparing ultra-thin dickite of being delaminated using potassium acetate intercalation | |
CN104177656A (en) | Light-resistant light calcium carbonate filler and preparation method thereof | |
CN104194400A (en) | High-dispersibility modified calcium carbonate filler and preparation method thereof | |
WO2022233034A1 (en) | Method for preparing composite pigment filler for coatings by using coal gasification slag | |
CN107055585B (en) | A kind of preparation method of flame retardant type major diameter flaky calcium carbonate | |
CN107418432A (en) | A kind of method that leather stability and durability are improved based on nano titanium oxide |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20221111 |