CN114410130A - Modified wollastonite and preparation method and application thereof - Google Patents
Modified wollastonite and preparation method and application thereof Download PDFInfo
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- CN114410130A CN114410130A CN202111393918.3A CN202111393918A CN114410130A CN 114410130 A CN114410130 A CN 114410130A CN 202111393918 A CN202111393918 A CN 202111393918A CN 114410130 A CN114410130 A CN 114410130A
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- wollastonite
- zirconia
- alkali metal
- metal silicate
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- 229910052882 wollastonite Inorganic materials 0.000 title claims abstract description 164
- 239000010456 wollastonite Substances 0.000 title claims abstract description 164
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 85
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims abstract description 64
- 238000000576 coating method Methods 0.000 claims abstract description 34
- 230000004048 modification Effects 0.000 claims abstract description 28
- 238000012986 modification Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 24
- 239000011268 mixed slurry Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 266
- 238000001035 drying Methods 0.000 claims description 38
- 238000000498 ball milling Methods 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000004321 preservation Methods 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 14
- 239000000945 filler Substances 0.000 abstract description 13
- 239000003973 paint Substances 0.000 abstract description 12
- 238000003860 storage Methods 0.000 abstract description 11
- 238000005406 washing Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 238000005336 cracking Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 230000001680 brushing effect Effects 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 description 18
- 239000000047 product Substances 0.000 description 17
- 239000004111 Potassium silicate Substances 0.000 description 10
- 229910052913 potassium silicate Inorganic materials 0.000 description 10
- 235000019353 potassium silicate Nutrition 0.000 description 10
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 10
- 239000002002 slurry Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000012295 chemical reaction liquid Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 238000007873 sieving Methods 0.000 description 6
- 238000006011 modification reaction Methods 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000005347 demagnetization Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- 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
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3045—Treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic 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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention belongs to the technical field of wollastonite fillers, and particularly relates to modified wollastonite and a preparation method and application thereof. The preparation method provided by the invention comprises the steps of mixing wollastonite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the modulus of the alkali metal silicate is 2.5-3.9, and the mass of the alkali metal silicate accounts for 1-5% of that of the wollastonite raw powder; and carrying out wet modification on the mixed slurry to obtain the modified wollastonite. The surface of the modified wollastonite prepared by the preparation method provided by the invention is passivated due to partial hydroxyl groups, so that the reaction activity is reduced, when the modified wollastonite is used as a filler of a pure inorganic coating, the modified wollastonite and the pure inorganic coating have good compatibility, and the pure inorganic coating has high stability in storage and high adhesive strength of a paint film in use. The results of the examples show that when the modified wollastonite provided by the invention is used as a filler of a pure inorganic coating, the storage performance, the cracking resistance, the water resistance and the washing and brushing times of the inorganic coating are improved.
Description
Technical Field
The invention belongs to the technical field of wollastonite fillers, and particularly relates to modified wollastonite and a preparation method and application thereof.
Background
At present, the content of organic emulsion in a mainstream formula of domestic inorganic paint is about 6 percent basically, the organic matter content in the whole system is lower, and a prepared paint film can easily meet the A2-grade fireproof requirement, but in some fields with high fireproof requirement grade such as petrochemical sites, the fireproof requirement grade is often required to reach A1 grade, in the fields, the fireproof of the current inorganic paint is relatively difficult to reach the A1-grade fireproof, the content of the organic matter in the formula system is required to be further reduced, and even the zero emulsion content in the formula is possible. In this case, since there is no binding effect of the emulsion, when the amount of inert filler such as heavy calcium carbonate is large in the purely inorganic paint formulation, the adhesive strength of the paint film is greatly adversely affected, and the properties of scrub resistance, water resistance and the like are greatly reduced.
Wollastonite is a functional silicate mineral material with a high refractive index and a needle-like structure, and is widely applied to the field of coatings such as building coatings, epoxy anticorrosive coatings and the like at present, and the wollastonite is added into inorganic coatings, and reacts with inorganic adhesives such as potassium silicate, sodium silicate and the like in the inorganic coatings, so that the crosslinking density of a paint film is improved, and further, the bonding strength, the water resistance, the washing resistance and the like of the paint film are improved.
However, the addition of ordinary wollastonite products to pure inorganic coatings tends to affect the storage stability of the inorganic coating system.
Disclosure of Invention
In view of the above, the invention provides modified wollastonite and a preparation method and application thereof, hydroxyl groups on the surface of the modified wollastonite are partially passivated, the reaction activity is reduced, when the modified wollastonite is used as a filler of a pure inorganic coating, the modified wollastonite and the pure inorganic coating have good compatibility, and the pure inorganic coating has high storage stability and high adhesive strength of a paint film in use.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of modified wollastonite, which comprises the following steps:
mixing wollastonite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the modulus of the alkali metal silicate is 2.5-3.9, and the mass of the alkali metal silicate accounts for 1-5% of that of the wollastonite raw powder;
and carrying out wet modification on the mixed slurry to obtain the modified wollastonite.
Preferably, the alkali metal silicate comprises a first alkali metal silicate and a second alkali metal silicate, the modulus of the first alkali metal silicate is 2.5-3, the modulus of the second alkali metal silicate is 3.2-3.9, the mass of the first alkali metal silicate accounts for 1-2% of the mass of the wollastonite raw powder, and the mass of the second alkali metal silicate accounts for 1-2% of the mass of the wollastonite raw powder.
Preferably, in the mixed slurry, the mass of the wollastonite raw powder accounts for 50-60% of the total mass of the wollastonite raw powder and water.
Preferably, the heat preservation temperature of the wet modification is 50-60 ℃, the wet modification is carried out under the condition of stirring, the stirring time is 60-90 min, and the stirring rotating speed is 500-800 r/min.
Preferably, the mass percent of silicon dioxide in the wollastonite raw powder is more than or equal to 51%, and the D50 of the wollastonite raw powder is 6-6.5 μm.
Preferably, the preparation method of the wollastonite raw powder comprises the following steps:
ball milling wollastonite to obtain wollastonite raw powder; the ball mill for ball milling is provided with a zirconia lining, a ball milling medium comprises zirconia columns and zirconia balls, the filling rate of the ball milling medium is 30-60%, the number ratio of the zirconia columns to the zirconia balls is 1: 3-5, and the size of the zirconia columns is
The particle size of the calcium oxide ball is 10-40 mm.
Preferably, the zirconia column comprises a first zirconia column, a second zirconia column and a third zirconia column, and the first zirconia column has a size of
The second zirconia column has a size of
The third zirconia column has a size of
The number ratio of the first zirconia column to the second zirconia column to the third zirconia column is (1-4) to (3-5) to (1-6);
the zirconia balls comprise first zirconia balls, second zirconia balls and third zirconia balls, the particle size of the first zirconia balls is 10-15 mm, the particle size of the second zirconia balls is 20-25 mm, the particle size of the third zirconia balls is 30-40 mm, and the number ratio of the first zirconia balls to the second zirconia balls to the third zirconia balls is (6-15): (8-15): (11-15).
Preferably, the wet modification is performed to obtain a wet modification solution, and the wet modification further includes: and drying the wet modification liquid to obtain the modified wollastonite, wherein the drying heat preservation temperature is 80-110 ℃, and the drying heat preservation time is 12-24 h.
The invention provides modified wollastonite prepared by the preparation method in the technical scheme.
The invention provides application of the modified wollastonite in the technical scheme in pure inorganic paint.
The invention provides a preparation method of modified wollastonite, which comprises the following steps: mixing wollastonite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the modulus of the alkali metal silicate is 2.5-3.9, and the mass of the alkali metal silicate accounts for 1-5% of that of the wollastonite raw powder; and carrying out wet modification on the mixed slurry to obtain the modified wollastonite. The preparation method provided by the invention adopts alkali metal silicate with the modulus of 2.5-3.9 as a modifier to carry out wet modification on wollastonite raw powder, hydroxyl groups of the alkali metal silicate react with hydroxyl groups on the surface of the wollastonite to form hydrogen bonds, part of hydroxyl groups on the surface of the wollastonite react with the alkali metal silicate by controlling the modulus of the alkali metal silicate and the mass ratio of the alkali metal silicate to the wollastonite, and the surface of the wollastonite is partially covered by the alkali metal silicate, so that the compatibility of the modified wollastonite and the inorganic coating containing the alkali metal silicate adhesive can be improved; and the surface of the modified wollastonite is passivated due to the reaction of partial hydroxyl and alkali metal silicate, so that the reactivity is reduced, and when the modified wollastonite is used as a filler of a pure inorganic coating, the pure inorganic coating has high stability during storage and high adhesive strength of a paint film during use. The results of the examples show that when the modified wollastonite provided by the invention is used as a filler of a pure inorganic coating, the storage performance, the cracking resistance, the water resistance and the washing and brushing times of the pure inorganic coating are improved.
The preparation method provided by the invention has simple steps and is suitable for industrial production.
Drawings
Fig. 1 is a flow chart of a preparation process provided by an embodiment of the invention.
Detailed Description
The invention provides a preparation method of modified wollastonite, which is characterized by comprising the following steps:
mixing wollastonite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the modulus of the alkali metal silicate is 2.5-3.9, and the mass of the alkali metal silicate accounts for 1-5% of that of the wollastonite raw powder;
and carrying out wet modification on the mixed slurry to obtain the modified wollastonite.
In the present invention, the starting materials used are all commercially available products whose numerical values are within the skill of those in the art, unless otherwise specified.
Mixing wollastonite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the modulus of the alkali metal silicate is 2.5-3.9, and the mass of the alkali metal silicate accounts for 1-5% of that of the wollastonite raw powder.
In the invention, the mass percent of the silicon dioxide in the wollastonite raw powder is preferably not less than 51%, and more preferably 51-90%. D50 of the wollastonite raw powder is preferably 6-6.5 μm.
According to the invention, the content of hydroxyl on the surface of the wollastonite raw powder can be improved by controlling the mass percent of silicon dioxide in the wollastonite raw powder to be preferably more than or equal to 51%.
According to the invention, the D50 of the wollastonite raw powder is preferably controlled to be 6-6.5 μm, so that the hydroxyl on the surface of the wollastonite raw powder can be favorably and fully reacted with the alkali metal silicate.
In the present invention, the preparation method of the wollastonite raw powder preferably includes the following steps:
ball milling wollastonite to obtain wollastonite raw powder; the ball milling cylinder for ball milling is provided with a zirconia lining, a ball milling medium comprises zirconia columns and zirconia balls, the filling rate of the ball milling medium is 30-60%, the number ratio of the zirconia columns to the zirconia balls is 1: 3-5, and the size of the zirconia columns is
The particle size of the calcium oxide ball is 10-40 mm.
In the invention, the mass percent of the silicon dioxide in the wollastonite is preferably not less than 51%, and more preferably 51-90%. In the invention, the particle size of the wollastonite is preferably 1 to 2 cm. The invention has no special requirement on the source of the wollastonite, and in the specific embodiment of the invention, the wollastonite is wollastonite concentrate.
In the present invention, the wollastonite is preferably subjected to a pretreatment, and in the present invention, the pretreatment preferably includes: and washing, drying and coarsely crushing the wollastonite in sequence. In the invention, the wollastonite is preferably mixed with water for washing, in the invention, the washing frequency is preferably 2, the invention has no special requirement on the specific implementation process of the washing, and the impurities on the surface of the wollastonite are removed by washing. The washed wollastonite is preferably dried in the present invention, and the specific manner of drying is preferably drying in the air. In the invention, the wollastonite after being dried is preferably coarsely crushed. In the present invention, the number of times of the coarse crushing is preferably 2, and the coarse crushing is preferably performed in a jaw crusher. The invention has no special requirements on the specific implementation process of the coarse crushing. The particle size of the wollastonite is controlled to be 1-2 cm through coarse crushing.
In the present invention, the ball mill for ball milling preferably has a zirconia lining. In the embodiment of the present invention, the size of the ball mill barrel for ball milling is preferably set to be the same
In the invention, the filling rate of the ball milling medium is preferably 30-60%, and more preferably 35-55%.
In the present invention, the ball milling medium preferably includes zirconia columns and zirconia balls, and the number ratio of the zirconia columns to the zirconia balls is preferably 1:3 to 5, and in a specific embodiment of the present invention, the number ratio of the zirconia columns to the zirconia balls is specifically 1:3, 1:4, or 1: 5.
In the present invention, the zirconia column is preferably sized
In the present invention, the zirconia column preferably includes a first zirconia column, a second zirconia column and a third zirconia column, and the first zirconia column preferably has a size of
In a particular embodiment of the invention, the first zirconia column is specifically dimensioned
In the present invention, the second zirconia column is preferably sized
In an embodiment of the present invention, the second zirconia column has a size of
In the present invention, the size of the third zirconia column is preferably set to be the same as that of the first zirconia column
In a particular embodiment of the invention, the third zirconia column is specifically dimensioned as
In the present invention, the number ratio of the first zirconia column, the second zirconia column and the third zirconia column is preferably (1-4): (3-5): (1-6), and in a specific embodiment of the present invention, the number ratio of the first zirconia column, the second zirconia column and the third zirconia column is specifically 1:1:2, 3:3:4 or 3:5: 6.
In the invention, the particle size of the calcium oxide ball is preferably 10-40 mm. In the invention, the zirconia balls preferably comprise first zirconia balls, second zirconia balls and third zirconia balls, the particle size of the first zirconia balls is preferably 10-15 mm, and in the specific implementation of the invention, the particle size of the first zirconia balls is preferably 10 mm. In the present invention, the particle size of the second zirconia balls is preferably 20 to 25mm, and in a specific embodiment of the present invention, the particle size of the second zirconia columns is preferably 20 mm. In the invention, the particle size of the third zirconia ball is preferably 30-40 mm, and in a specific embodiment of the invention, the particle size of the third zirconia ball is preferably 30 mm.
In the invention, the number ratio of the first zirconia balls, the second zirconia balls and the third zirconia balls is preferably (6-15): 8-15): 11-15, and in a specific embodiment of the invention, the number ratio of the first zirconia balls, the second zirconia balls and the third zirconia balls is specifically 4:5:6, 5:6:7 or 12:14: 15.
The invention has no special requirements on the specific implementation process of the ball milling.
According to the invention, the zirconium oxide column and the zirconium oxide ball are preferably matched as a ball milling medium, meanwhile, the zirconium oxide column adopts three-level size gradation, and the zirconium oxide adopts three-level size gradation, so that the ball milling efficiency can be improved, the ball milling time can be shortened, the damage to the appearance of the wollastonite needle crystal in the ball milling process can be effectively reduced, and the influence on the modification reaction effect caused by agglomeration caused by the appearance damage of wollastonite can be avoided.
According to the invention, the wollastonite is ground by using the grinding medium with the zirconia lining ball mill cylinder and the zirconia material, so that the defects that the purity of a modified wollastonite product is influenced and the storage stability of a pure inorganic coating is influenced when the wollastonite product is used as a pure inorganic coating filler because iron ion impurities are introduced due to the abrasion of the grinding machine and the grinding medium in the grinding process of a traditional metal grinding machine and the metal grinding medium can be effectively avoided.
In the invention, the ball-milled powder is obtained after ball milling, the invention preferably performs grading screening and demagnetization on the ball-milled powder in sequence to obtain the wollastonite raw powder, and the invention has no special requirements on the specific implementation processes of the decomposition screening and the demagnetization.
In the present invention, the modulus of the alkali metal silicate is 2.5 to 3.9, preferably 2.6 to 3.5. In a particular embodiment of the invention, the alkali metal silicate is in particular potassium silicate.
According to the invention, the modulus of the alkali metal silicate is controlled to be 2.5-3.9, so that the alkali metal silicate has high reactivity and reacts with hydroxyl on the surface of the wollastonite, and the condition that the modulus of the alkali metal silicate is too high and the reactivity is too strong to completely passivate the surface of the wollastonite is avoided.
In the present invention, the alkali metal silicate is preferably 1 to 5% by mass, more preferably 2 to 4% by mass, of the wollastonite raw powder.
In the present invention, the alkali silicate preferably includes a first alkali silicate and a second alkali silicate, and the modulus of the first alkali silicate is preferably 2.5 to 3, and in a specific embodiment of the present invention, the modulus of the first alkali silicate is specifically 2.5 or 3. In the present invention, the mass of the first alkali metal silicate is preferably 1 to 2%, and more preferably 1.2 to 1.5% of the mass of the wollastonite raw powder.
In the present invention, the modulus of the second alkali silicate is preferably 3.2 to 3.9, and in a specific embodiment of the present invention, the modulus of the second alkali silicate is specifically 3.5 or 3.9. In the present invention, the mass of the second alkali metal silicate is preferably 1 to 2%, preferably 1.2 to 1.5% of the mass of the wollastonite raw powder.
In the present invention, in the mixed slurry, the mass of the wollastonite raw powder is preferably 50 to 60%, more preferably 53 to 55% of the total mass of the wollastonite raw powder and water.
According to the invention, the mass of the wollastonite raw powder is preferably controlled to be 50-60% of the total mass of the wollastonite raw powder and water, so that hydroxyl on the surface of the wollastonite can be more effectively reacted with an alkali metal silicate modifier.
In the present invention, the mixing preferably comprises the steps of: premixing the wollastonite raw powder and water to obtain wollastonite raw powder slurry, and finally mixing the wollastonite raw powder slurry and the alkali metal silicate. In the invention, the temperature of the premixing is preferably 50-60 ℃, the premixing is preferably carried out under the condition of stirring, the stirring time is preferably 10-15 min, and the stirring rotation speed is preferably 600-700 r/min. In the invention, the final mixing temperature is preferably 50-60 ℃, the specific implementation mode of the final mixing is preferably that the alkali metal silicate is pumped into the wollastonite raw powder slurry through an automatic metering pump, the final mixing is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 600-700 r/min.
According to the invention, the wollastonite raw powder, the alkali metal silicate and the water can be uniformly mixed by the mixing method, so that the reaction of hydroxyl on the surface of the wollastonite and the alkali metal silicate is facilitated.
After the mixed slurry is obtained, the wet modification is carried out on the mixed slurry to obtain the modified wollastonite.
In the invention, the heat preservation temperature of the wet modification is preferably 50-60 ℃, and more preferably 52-55 ℃. In the invention, the wet modification is preferably carried out under the condition of stirring, the stirring time is preferably 60-90 min, more preferably 65-80 min, and the stirring rotation speed is preferably 500-800 r/min, more preferably 550-700 r/min.
The temperature of the precipitation reaction is controlled to be 50-60 ℃, so that the reaction rate of hydroxyl on the surface of the alkali metal silicate and wollastonite raw powder is favorably improved. The precipitation reaction time is controlled to be 60-90 min, and the sufficient reaction of the alkali metal silicate and the hydroxyl on the surface of the wollastonite raw powder can be realized.
In the present invention, after the wet modification, a wet modification solution is obtained, and after the wet modification, the present invention preferably further includes: and drying the wet modification liquid to obtain the modified wollastonite, wherein the drying heat preservation temperature is 80-110 ℃, and the drying heat preservation time is 12-24 h.
The wet modification liquid is preferably conveyed to a drying chamber for drying.
In the invention, the drying heat preservation temperature is preferably 80-110 ℃, and more preferably 85-105 ℃. The drying heat preservation time is preferably 12-24 hours, and more preferably 15-20 hours.
According to the invention, the drying heat preservation temperature is controlled to be 80-110 ℃, and the heat preservation time is controlled to be 12-24 h, so that the alkali metal silicate and the hydroxyl on the surface of the wollastonite raw powder which are completely reacted in the wet modification reaction liquid can be further subjected to modification reaction in the appropriate drying and dehydration process, and compared with the conventional flash evaporation drying, the drying method disclosed by the invention can ensure the sufficiency of the modification effect.
In the invention, the drying is carried out to obtain a blocky solid product, and the blocky solid product is preferably subjected to post-treatment to obtain the modified wollastonite powder. In the present invention, the post-treatment preferably comprises dispersion, classification screening, detection and packaging. In the invention, the belt is preferably adopted to convey the blocky solid product to the ball mill for ball milling and dispersion, and in the invention, the size and the material of the ball milling cylinder for ball milling and dispersion are preferably the same as those of the ball milling cylinder described above, and further description is omitted. In the invention, the time for ball milling and dispersing is preferably 15-20 min. The present invention has no special requirements for the specific implementation process of the classification screening, detection and packaging.
The invention provides modified wollastonite prepared by the preparation method in the technical scheme.
The invention provides application of the modified wollastonite in the technical scheme in pure inorganic paint.
In the present invention, the modified wollastonite is preferably used as a filler for preparing the pure inorganic coating. The invention has no special requirements on the dosage of the modified wollastonite in the pure inorganic coating.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Selecting wollastonite ore concentrate with silicon dioxide content not less than 51 percent according to the process flow shown in figure 1, cleaning, naturally drying, crushing by two sections of jaw to obtain wollastonite crushed aggregates with the diameter of about 2cm, conveying the wollastonite crushed aggregates to a ball mill with the specification of 1.83m multiplied by 7.2m for superfine grinding by a screw feed, wherein the ball mill is a full zirconia lining, a grinding medium is a zirconia column and zirconia balls which are compounded, the filling rate is 32 percent, and the zirconia column and the zirconia balls are filled in the ball millThe zirconia balls have a number ratio of 1:3, wherein the size is
Zirconia column of size
Zirconia column and size of
The quantity ratio of zirconia columns is 2:2:4, the quantity of zirconia balls with the diameter of 10mm, the quantity of zirconia balls with the diameter of 20mm and the quantity of zirconia balls with the diameter of 30mm are 8:10:12, the grinding time is 30min, wollastonite raw powder is obtained after grading, sieving and demagnetizing, the detection of a Malvern laser particle size analyzer shows that the average particle size D50 is 6.52 mu m, the wollastonite raw powder and water are stirred at the rotating speed of 600r/min at the temperature of 55 ℃ for 10min to obtain wollastonite raw powder slurry, the wollastonite raw powder slurry has the mass percentage of 50%, potassium silicate with the mass percentage of 1 percent and the modulus of 2.5 in the wollastonite and potassium with the mass percentage of 1 percent and the modulus of 3.2 in the wollastonite raw powder are added by an automatic metering pump, the rotating speed of the stirring paddle is kept at 600r/min, the wet-process modified reaction liquid is obtained after continuous stirring for 60min, then the wet process modified reaction liquid is conveyed to a drying chamber by a diaphragm pump for drying treatment, the temperature of the drying chamber is 85 ℃, the drying time is 24 hours, and the dried block materials are conveyed to the drying chamber through a belt
The full zirconia lining ball mill is used for grinding and dispersing for 15min, and the modified wollastonite powder product is obtained through grading, sieving, detecting and packaging.
Example 2
Selecting wollastonite ore concentrate with silicon dioxide content not less than 51%, cleaning, naturally drying, crushing by two sections of jaw to obtain wollastonite crushed material with diameter of about 2cm, feeding by a screw to a ball mill with specification of 1.83m × 7.2m for superfine grinding, wherein the ball mill is a full zirconia lining, and grinding medium is addedThe filling rate is 50%, the quantity ratio of the zirconia column to the zirconia ball is 1:4, and the size is
Zirconia column of size
Zirconia column and size of
The quantity ratio of zirconia columns is 3:3:4, the quantity of zirconia balls with the diameter of 10mm, the quantity of zirconia balls with the diameter of 20mm and the quantity of zirconia balls with the diameter of 30mm are 10:12:14, the grinding time is 25min, wollastonite raw powder is obtained after grading, sieving and demagnetizing, the detection of a Malvern laser particle size analyzer shows that the average particle size D50 is 6.37 mu m, the wollastonite raw powder and water are stirred at the rotating speed of 600r/min at the temperature of 55 ℃, wollastonite raw powder slurry is obtained after 15min, the wollastonite raw powder slurry has the mass percentage of 55%, potassium silicate with the modulus of 2.5 and 1.5 of the wollastonite raw powder are added into dry powder by an automatic metering pump, the potassium silicate with the modulus of 2.5 and the potassium silicate with the modulus of 3.5 are added into the dry powder, the rotating speed of 55 ℃, a diaphragm pump is kept at the rotating speed of 600r/min, the wet modification reaction liquid is obtained after continuous stirring for 65min, and then the wet modification reaction liquid is conveyed into a drying chamber for drying treatment, the temperature of the drying chamber is 95 ℃, the drying time is 18h, and the dried block materials are conveyed to the drying chamber through a belt
The full zirconia lining ball mill is used for grinding and dispersing for 15min, and the modified wollastonite powder product is obtained through grading, sieving, detecting and packaging.
Example 3
Selecting wollastonite ore concentrate with silicon dioxide content not less than 51% according to the process flow shown in figure 1, cleaning, naturally drying, crushing by two sections of Eschericia to obtain wollastonite crushed aggregates with diameter of about 2cm, conveying the wollastonite crushed aggregates to a ball milling barrel by a screw feed with specification of 1.83mCarrying out superfine grinding by a 7.2m ball mill, wherein the ball mill is a full zirconia lining, a grinding medium is formed by compounding a zirconia column and zirconia balls, the filling rate is 32 percent, the number ratio of the zirconia column to the zirconia balls is 1:5, and the size is
Zirconia column of size
Zirconia column and size of
The quantity ratio of zirconia columns is 3:5:6, the quantity of zirconia balls with the diameter of 10mm, the quantity of zirconia balls with the diameter of 20mm and the quantity of zirconia balls with the diameter of 30mm are 12:14:15, the grinding time is 20min, wollastonite raw powder is obtained after grading, sieving and demagnetizing, the detection of a Malvern laser particle size analyzer shows that the average particle size D50 is 6.21 mu m, the wollastonite raw powder and water are stirred at 60 ℃ and the stirring paddle rotating speed is 600r/min for 15min to obtain wollastonite raw powder slurry, the wollastonite raw powder slurry mass percentage is 60%, potassium silicate with the modulus of 3 accounting for 2 mass percent of the wollastonite and potassium silicate with the modulus of 3.9 accounting for 2 mass percent of the wollastonite raw powder are added by an automatic metering pump, the potassium silicate with the modulus of 3 accounting for 2 mass percent of the wollastonite and the stirring paddle rotating speed is kept at 600r/min, the wet-process modified reaction liquid is obtained after continuous stirring for 60min, then the wet-process modified reaction liquid is conveyed to a drying chamber by a diaphragm pump for drying treatment, the temperature of the drying chamber is 105 ℃, the drying time is 12 hours, and the dried block material is conveyed to
The full zirconia lining ball mill is used for grinding and dispersing for 15min, and the modified wollastonite powder product is obtained through grading, sieving, detecting and packaging.
Test example 1
The modified wollastonite powder products prepared in examples 1-3 are subjected to related index detection according to JC/T535-2007, and the related indexes and the test results are shown in Table 1.
TABLE 1 Performance test data for modified wollastonite powder products produced in examples 1 to 3
| Detecting the index | Example 1 | Example 2 | Example 3 |
| Whiteness degree | 91.0 | 91.3 | 91.5 |
| D50(μm) | 6.52 | 6.37 | 6.21 |
| Oil absorption (mL/100g) | 33 | 31 | 28 |
| Moisture (%) | 0.21 | 0.14 | 0.12 |
| Aspect ratio | 1:14 | 1:15 | 1:16 |
| Magnetic substance content (ppm) | 12 | 10 | 6 |
As can be seen from Table 1, the ancient properties of the modified wollastonite powder product prepared by the present invention are all at a superior level.
Application example
The modified wollastonite powder products prepared in examples 1 to 3 and commercially available ordinary wollastonite products are applied to pure inorganic coatings. Wherein, the pure inorganic coating comprises the following components in percentage by weight: 162.9g of water, 6g of cellulose, 1g of dispersing agent, 0.1g of defoaming agent, 3g of stabilizing agent, 400g of potassium silicate, 150g of titanium dioxide, 275g of filler and 2g of preservative. The filler is the modified wollastonite powder product prepared in the embodiment 1-3 and the common wollastonite product with the corresponding fineness sold in the market. The preparation method of the pure inorganic coating comprises the following steps: mixing the above materials uniformly.
Test example 2
And carrying out related index detection on the pure inorganic coating prepared according to the application example of GB/T9755-. Wherein: storage stability test evaluation: after 30 days of thermal storage at 50 ℃, the smaller the viscosity increase, the better the stability of the coating; and (3) water resistance evaluation: after the sample plate is soaked in water for 30 days, the powder is easy to fall off when the sample plate is wiped by fingers, and the water resistance is poorer; cracking resistance: the thicker the cracking thickness, the better the cracking resistance of the coating. The test results are shown in table 2, and it can be seen from table 2 that when the modified wollastonite powder products produced in examples 1 to 3 of the present invention are applied to pure inorganic coatings, the storage stability, the times of washing and brushing resistance, the water resistance and the crack resistance of the modified wollastonite powder products are obviously superior to those of common wollastonite products, and the storage and use requirements of the inorganic coatings are completely met.
TABLE 2 data of performance tests on pure inorganic coatings produced from examples 1-3 and commercially available wollastonite powder as filler
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of modified wollastonite is characterized by comprising the following steps:
mixing wollastonite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the modulus of the alkali metal silicate is 2.5-3.9, and the mass of the alkali metal silicate accounts for 1-5% of that of the wollastonite raw powder;
and carrying out wet modification on the mixed slurry to obtain the modified wollastonite.
2. The preparation method according to claim 1, wherein the alkali metal silicate comprises a first alkali metal silicate and a second alkali metal silicate, the modulus of the first alkali metal silicate is 2.5-3, the modulus of the second alkali metal silicate is 3.2-3.9, the mass of the first alkali metal silicate is 1-2% of the mass of the wollastonite raw powder, and the mass of the second alkali metal silicate is 1-2% of the mass of the wollastonite raw powder.
3. The method according to claim 1, characterized in that the mass of the wollastonite raw powder in the mixed slurry accounts for 50-60% of the total mass of the wollastonite raw powder and water.
4. The preparation method of claim 1, wherein the temperature of the wet modification is 50-60 ℃, the wet modification is performed under stirring, the stirring time is 60-90 min, and the stirring speed is 500-800 r/min.
5. The preparation method of claim 1, wherein the mass percent of silicon dioxide in the wollastonite raw powder is not less than 51%, and the D50 of the wollastonite raw powder is 6-6.5 μm.
6. The preparation method of claim 1, wherein the preparation method of the wollastonite raw powder comprises the following steps:
ball milling wollastonite to obtain wollastonite raw powder; the ball mill for ball milling is provided with a zirconia lining, a ball milling medium comprises zirconia columns and zirconia balls, the filling rate of the ball milling medium is 30-60%, the number ratio of the zirconia columns to the zirconia balls is 1: 3-5, and the size of the zirconia columns is
The particle size of the calcium oxide ball is 10-40 mm.
7. The method according to claim 6, wherein the zirconia column comprises a first zirconia column, a second zirconia column and a third zirconia column, and the first zirconia column has a size of
The second zirconia column has a size of
The third zirconia column has a size of
The number ratio of the first zirconia column to the second zirconia column to the third zirconia column is (1-4) to (3-5) to (1-6);
the zirconia balls comprise first zirconia balls, second zirconia balls and third zirconia balls, the particle size of the first zirconia balls is 10-15 mm, the particle size of the second zirconia balls is 20-25 mm, the particle size of the third zirconia balls is 30-40 mm, and the number ratio of the first zirconia balls to the second zirconia balls to the third zirconia balls is (6-15): (8-15): (11-15).
8. The preparation method according to claim 1, wherein a wet modification solution is obtained after the wet modification, and the preparation method further comprises the following steps: and drying the wet modification liquid to obtain the modified wollastonite, wherein the drying heat preservation temperature is 80-110 ℃, and the drying heat preservation time is 12-24 h.
9. Modified wollastonite produced by the production method according to any one of claims 1 to 8.
10. Use of the modified wollastonite of claim 9 in a pure inorganic coating.
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