CN111349350B - Inorganic composite powder and preparation method thereof - Google Patents
Inorganic composite powder and preparation method thereof Download PDFInfo
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- CN111349350B CN111349350B CN202010177282.8A CN202010177282A CN111349350B CN 111349350 B CN111349350 B CN 111349350B CN 202010177282 A CN202010177282 A CN 202010177282A CN 111349350 B CN111349350 B CN 111349350B
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- 239000000843 powder Substances 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000011049 filling Methods 0.000 claims abstract description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 6
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 3
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 3
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 3
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims description 74
- 239000002002 slurry Substances 0.000 claims description 52
- 239000010456 wollastonite Substances 0.000 claims description 44
- 239000006004 Quartz sand Substances 0.000 claims description 41
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 40
- 229910021532 Calcite Inorganic materials 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 33
- 238000002156 mixing Methods 0.000 claims description 25
- 239000002270 dispersing agent Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 15
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 12
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 12
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 12
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 12
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 12
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 12
- 229910004762 CaSiO Inorganic materials 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 5
- 239000003344 environmental pollutant Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 231100000719 pollutant Toxicity 0.000 claims description 5
- 235000019738 Limestone Nutrition 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 239000006028 limestone Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 16
- 239000000126 substance Substances 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000013329 compounding Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000006148 magnetic separator Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000011246 composite particle Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention relates to inorganic composite powder and a preparation method thereof, belonging to the technical field of preparation and application of superfine functional materials. The inorganic composite powder comprises the following components in percentage by weight: CaSiO3 60‑80%、SiO2 5‑25%、CaCO35 to 25 percent; the specific surface area of the inorganic composite powder is 5-20m2(ii) in terms of/g. The inorganic composite powder has the advantages of obviously improved specific surface area, stronger catalytic performance and surface activity, improved filling and reinforcing performance and expanded application field of products.
Description
Technical Field
The invention relates to inorganic composite powder and a preparation method thereof, belonging to the technical field of preparation and application of superfine functional materials.
Background
The ultrafine grinding process is a high and new technology which is developed rapidly and across subjects and industries, is a difficult point in the deep processing of powder, is also a key in the preparation technology, and plays an important role in promoting the development of modern high-tech and new material industries. The indexes of the ultrafine powder defined in different fields are different, and generally, the mineralogy refers to the material with the granularity ranging from nanometer to micrometer (such as 0.2-10 μm) as the ultrafine powder. The compounding of powder particles is an important way for constructing new substances, and the prepared new substances can change the surface properties of single particles and increase the surface energy of the particles. The particle functionalization is promoted through particle compounding, and the composite powder has good dispersing performance and adsorption performance due to large specific surface area; along with the multiplied increase of the surface atomic number of the particles, the composite superfine powder has stronger catalytic property and surface activity, thereby having the characteristics of good filling property and excellent reinforcing effect.
The preparation methods of the composite powder are various, and the mechanical method is a main preparation method due to low investment, simple process and easy production scale formation. However, most mechanical methods have certain limitations, and have many problems to be solved and perfected, such as low yield of ultrafine powder and relatively large energy consumption; some methods can realize batch industrial production, but have strong selectivity to raw materials; the classification is difficult after some ultrafine powder is prepared; some composite powder is simply formed by mixing and stirring a plurality of materials, cannot form composite particles, and has poor performance.
Disclosure of Invention
The invention generates CaSiO by a mechanochemical method3-SiO2-CaCO3The inorganic composite powder with the structure is easy to maintain the crystal form of the acicular wollastonite aggregate, and forms a micro-nano fiber structure after being ultra-refined, so that the specific surface area is increased by geometric multiple, the purpose of optimizing the performance is achieved, and the problems are solved.
The invention provides inorganic composite powder, which consists of the following components in percentage by weight:
CaSiO3 60-80%
SiO2 5-25%
CaCO3 5-25%;
the specific surface area of the inorganic composite powder is 5-20m2/g。
The particle size x of the inorganic composite powder is preferably selected in the invention50Is 0.1-2 um.
The particle size x of the inorganic composite powder is preferably selected in the invention90Is 0.2-5 um.
The invention also aims to provide a preparation method of the inorganic composite powder, which comprises the following steps: s1, preparing wollastonite slurry from wollastonite powder, a dispersing agent I and water, adjusting the pH to 6.0-6.5, and grinding, wherein the particle size X of the wollastonite powder5030-70um, and CaSiO in the wollastonite powder3The content of (A) is 85-95%; s2, preparing quartz sand, a dispersant II and water into quartz sand slurry, adjusting the pH to 5.5-6.2, and grinding to obtain the quartz sand with the granularity X50Is 10-20um, SiO in the quartz sand2The content of (B) is 92-98%(ii) a S3, separating the grinding media from the product obtained in the step S1 and the product obtained in the step S2, and then mixing, grinding and separating the grinding media, wherein CaSiO in the wollastonite powder3With SiO in quartz sand2The weight ratio of (A) to (B) is 2.4-16: 1; s4, mixing calcite with the particle size X, dispersing agent III and water to form calcite slurry, and mixing and grinding the calcite slurry with the product obtained in the step S35010-20um, CaCO in the calcite3Is 90-99%, the weight ratio of the calcite slurry to the product obtained in step S3 is 1: 4-15; s5, separating the product obtained in the step S4 from grinding media, removing iron pollutants, concentrating, drying and depolymerizing.
In a liquid medium system, by controlling the grinding process conditions, energy input is increased to enable minerals to generate mechanical force chemical solid-state reaction; by means of the mechanical force activation effect generated by the micronization of the particles, the matching size of the particles is controlled, the action behavior among the mineral particles and the form of functional groups on the surfaces of the particles are adjusted, and the interfacial reaction and other strong bonding among the particles are initiated to form the composite particles.
The concentration of wollastonite powder in the wollastonite slurry is preferably 30-40%, the dispersing agent I is sodium hexametaphosphate, and the addition amount of the dispersing agent I is 0.5-0.6% of the mass of the wollastonite powder; the grinding medium of the step S1 is zirconia balls with the diameter of 0.6-0.8mm, the filling rate of the medium is 45-50%, and the grinding is carried out for 90-150min at 1500-1600 rpm.
According to the invention, the concentration of the quartz sand in the quartz sand slurry is preferably 45-55%, the dispersing agent II is sodium polyphosphate, and the addition amount of the dispersing agent II is 0.6-0.7% of the mass of the quartz sand; the grinding medium of the step S2 is zirconia balls with the diameter of 0.4-0.5mm, the filling rate of the medium is 50-55%, and the grinding is carried out for 60-90min at 1600-1700 rpm.
In the present invention, it is preferable that the mixing conditions in step S3 are: stirring at 80-120rpm for 20-30 min; the grinding medium of the step S3 is zirconia balls with the diameter of 0.3-0.4mm, the filling rate of the medium is 50-55%, and the grinding is carried out for 60-90min at 1600-1700 rpm.
According to the invention, the concentration of calcite in the calcite slurry is preferably 40-50%, the dispersant III is sodium polyacrylate, and the addition amount of the dispersant III is 0.7-0.8% of the mass of the calcite; the grinding medium of the step S4 is zirconia balls with the diameter of 0.2-0.3mm, the filling rate of the medium is 55-60%, and the grinding is carried out at 1700-1800rpm for 90-120 min.
The dispersing agent is sodium hexametaphosphate, sodium polyphosphate and sodium polyacrylate, and molecules of the dispersing agent are adsorbed on the surfaces of the particles, so that the surface energy of the particles is reduced, the closure of new cracks is hindered, the agglomeration of the particles is reduced, and the flowability of powder is improved.
The pH is adjusted by 1-3mol/L hydrochloric acid, and the mineral structure of wollastonite and quartz is destroyed by adding hydrochloric acid by a chemical method, so that powder particles are depolymerized and active groups are formed.
The invention has the beneficial effects that:
the inorganic composite powder has the advantages of obviously improved specific surface area, stronger catalytic property and surface activity, improved filling and reinforcing properties and expanded application field of products;
the preparation method provided by the invention overcomes the particle agglomeration phenomenon, improves the ore grinding and sorting efficiency, and effectively reduces the energy consumption required by ore grinding;
the preparation method of the invention obviously reduces the energy consumption of the superfine powder grinding after multi-stage continuous grinding and compounding, and reduces the production and operation cost compared with the traditional single grinding process.
Drawings
In the figure 1 of the attached drawings of the invention,
FIG. 1 is a schematic view of a polishing process.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The stirring mill is provided with a baffle or a pin on the inner wall of the cylinder body so as to increase the speed difference of the grinding medium in the cylinder body, increase the speed gradient and strengthen the crushing effect.
The performance of the inorganic composite powder is mainly detected by granularity, specific surface area, whiteness and chemical components, and in the following embodiment, the determination method of each index is as follows:
the particle size detection method comprises the following steps: according to GB/T19077-2016 (particle size distribution laser diffraction method), a BT-2000 type laser particle size analyzer produced by Liaoning Dandongbeit instrument Limited is adopted to detect a test sample, and the basic principle is the Mie scattering theory and the approximate theory thereof.
Specific surface area detection method: according to GB/T19587-.
The whiteness is detected by GB/T5950 + 2008 'method for measuring whiteness of building materials and non-metallic mineral products'.
And (4) detecting chemical components according to a silicate rock chemical analysis method (GB/T14506.3-2010).
Example 1
A method for preparing inorganic composite powder by wet superfine grinding comprises the following steps:
s1, mixing wollastonite powder, water and sodium hexametaphosphate into wollastonite slurry in a slurry mixing tank A, adding 1mol/L hydrochloric acid, adjusting the pH to 6.0, pumping into a stirring mill I, adding a zirconia ball with the diameter of 0.6mm serving as a grinding medium into the stirring mill I, wherein the medium filling rate is 45%, grinding at 1500rpm for 90min, and the particle size X of the wollastonite powder5030um, CaSiO in the wollastonite powder3The content of the sodium hexametaphosphate is 91%, the concentration of wollastonite powder in the wollastonite slurry is 32%, and the addition amount of the sodium hexametaphosphate is 0.5% of the mass of the wollastonite powder;
s2, mixing quartz sand, water and sodium polyphosphate into quartz sand slurry in a slurry mixing tank B, adding 1mol/L hydrochloric acid, adjusting the pH to 5.5, pumping into a stirring mill II, adding a zirconia ball with the diameter of 0.4mm serving as a grinding medium into the stirring mill II, wherein the medium filling rate is 50%, and the quartz sand is ground at 1600rpm for 60min, and the granularity X of the quartz sand is50Is 10um, SiO in the quartz sand2The content of the sodium polyphosphate is 94%, the concentration of the quartz sand in the quartz sand slurry is 46%, and the addition amount of the sodium polyphosphate is 0.6% of the mass of the quartz sand;
s3, mixing the product obtained in the step S1 and the stepSeparating grinding media from the product obtained in S2, pumping the product into a slurry storage tank C90 rpm, stirring for 20min, pumping into a stirring mill III, grinding, adding 0.3mm zirconia balls into the stirring mill III as grinding media, wherein the media filling rate is 50%, grinding at 1600rpm for 60min, separating the grinding media, and pumping into a stirring mill IV, wherein CaSiO in the wollastonite powder3With SiO in quartz sand2The weight ratio of (A) to (B) is 8.07: 1;
s4, preparing calcite slurry from calcite, water and sodium polyacrylate in a slurry mixing tank D, pumping the calcite slurry into a stirring mill IV, adding zirconia balls with the diameter of 0.3mm into the stirring mill IV as grinding media, grinding the products obtained in the step S3 at the medium filling rate of 55% at 1700rpm for 90min, wherein the particle size X of the calcite is5010um, CaCO in the calcite3The content of the sodium polyacrylate is 98%, the concentration of the calcite in the calcite slurry is 41%, the addition amount of the sodium polyacrylate is 0.7% of the mass of the calcite, and the weight ratio of the calcite slurry to the product obtained in the step S3 is 1: 8.7;
s5, separating the product obtained in the step S4 from grinding media, removing iron pollutants by a magnetic separator, concentrating, drying, dehydrating and depolymerizing.
The results of the performance test of the obtained composite ultrafine powder are shown in Table 1.
Example 2
A method for preparing inorganic composite powder by wet superfine grinding comprises the following steps:
s1, mixing wollastonite powder, water and sodium hexametaphosphate into wollastonite slurry in a slurry mixing tank A, adding 3mol/L hydrochloric acid, adjusting the pH to 6.5, pumping into a stirring mill I, adding a zirconia ball of 0.8mm serving as a grinding medium into the stirring mill I, wherein the medium filling rate is 50%, the mixture is ground at 1600rpm for 150min, and the particle size X of the wollastonite powder is5070um, CaSiO in the wollastonite powder3The content of the sodium hexametaphosphate is 91%, the concentration of wollastonite powder in the wollastonite slurry is 40%, and the addition amount of the sodium hexametaphosphate is 0.6% of the mass of the wollastonite powder;
s2, mixing quartz sand, water and sodium polyphosphate into quartz sand slurry in a slurry mixing tank B, adding 3mol/L hydrochloric acid, adjusting pH to 6.2, pumping into a stirring mill II, and stirring in a stirring mill IIAdding 0.4mm zirconia balls as grinding media into the stirring mill II, wherein the filling rate of the media is 55%, grinding at 1700rpm for 90min, and the granularity X of the quartz sand50Is 20um, SiO in the quartz sand2The content of the sodium polyphosphate is 94%, the concentration of the quartz sand in the quartz sand slurry is 55%, and the addition amount of the sodium polyphosphate is 0.7% of the mass of the quartz sand;
s3, separating the grinding medium from the product obtained in the step S1 and the product obtained in the step S2, pumping the product into a slurry storage tank C120rpm, stirring the product for 30min, pumping a stirring mill III for grinding, adding zirconia balls with the diameter of 0.4mm into the stirring mill III as the grinding medium, enabling the medium filling rate to be 55 percent, grinding the mixture at 1700rpm for 90min, separating the grinding medium, and pumping a stirring mill IV, wherein CaSiO in the wollastonite powder3With SiO in quartz sand2In a weight ratio of 3.29: 1;
s4, preparing calcite slurry from calcite, water and sodium polyacrylate in a slurry mixing tank D, pumping the calcite slurry into a stirring mill IV, adding zirconia balls with the diameter of 0.3mm into the stirring mill IV as grinding media, grinding the products obtained in the step S3 at the medium filling rate of 55% at 1700rpm for 90min, wherein the particle size X of the calcite is5020um, CaCO in the calcite3The content of the sodium polyacrylate is 98%, the concentration of the calcite in the calcite slurry is 50%, the addition amount of the sodium polyacrylate is 0.8% of the mass of the calcite, and the weight ratio of the calcite slurry to the product obtained in the step S3 is 1: 4.12;
s5, separating the product obtained in the step S4 from grinding media, removing iron pollutants by a magnetic separator, concentrating, drying, dehydrating and depolymerizing.
The results of the performance test of the obtained composite ultrafine powder are shown in Table 1.
Example 3
A method for preparing inorganic composite powder by wet superfine grinding comprises the following steps:
s1, mixing wollastonite powder, water and sodium hexametaphosphate into wollastonite slurry in a slurry mixing tank A, adding 1mol/L hydrochloric acid, adjusting the pH to 6.2, pumping into a stirring mill I, adding 0.7mm zirconia balls serving as grinding media into the stirring mill I, wherein the filling rate of the media is 48%, the mixture is ground at 1550rpm for 120min, and the wollastonite powder particles are groundDegree X5045um, CaSiO in the wollastonite powder3The content of the sodium hexametaphosphate is 91%, the concentration of wollastonite powder in the wollastonite slurry is 35%, and the addition amount of the sodium hexametaphosphate is 0.55% of the mass of the wollastonite powder;
s2, mixing quartz sand, water and sodium polyphosphate into quartz sand slurry in a slurry mixing tank B, adding 2mol/L hydrochloric acid, adjusting the pH to 5.8, pumping into a stirring mill II, adding a zirconia ball of 0.45mm serving as a grinding medium into the stirring mill II, wherein the medium filling rate is 53%, grinding at 1650rpm for 75min, and the granularity X of the quartz sand is50Is 15um, SiO in the quartz sand2The content of the sodium polyphosphate is 94%, the concentration of the quartz sand in the quartz sand slurry is 50%, and the addition amount of the sodium polyphosphate is 0.65% of the mass of the quartz sand;
s3, separating the grinding medium from the product obtained in the step S1 and the product obtained in the step S2, pumping the product into a slurry storage tank C100rpm, stirring for 25min, pumping into a stirring mill III, grinding, adding zirconia balls with the diameter of 0.35mm into the stirring mill III as the grinding medium, enabling the filling rate of the medium to be 53 percent, grinding at 1650rpm for 75min, separating the grinding medium, and pumping into a stirring mill IV, wherein CaSiO in the wollastonite powder3With SiO in quartz sand2In a weight ratio of 4.84: 1;
s4, preparing calcite slurry from calcite, water and sodium polyacrylate in a slurry mixing tank D, pumping the calcite slurry into a stirring mill IV, adding zirconia balls with the diameter of 0.3mm into the stirring mill IV as grinding media, grinding the products obtained in the step S3 at the medium filling rate of 53% at 1700rpm for 90min, wherein the particle size X of the calcite is50Is 15um, CaCO in the calcite3The content of the sodium polyacrylate is 98%, the concentration of the calcite in the calcite slurry is 45%, the addition amount of the sodium polyacrylate is 0.75% of the mass of the calcite, and the weight ratio of the calcite slurry to the product obtained in the step S3 is 1: 5.98 of;
s5, separating the product obtained in the step S4 from grinding media, removing iron pollutants by a magnetic separator, concentrating, drying, dehydrating and depolymerizing.
The results of the performance test of the obtained composite ultrafine powder are shown in Table 1.
Comparative example 1
Wollastonite raw ore which is the same as that in example 3 is used as a raw material, and wollastonite powder is added into an LHL-60 type fluidized bed type airflow mill (manufactured by Weifang Zhengyuan powder engineering equipment Co., Ltd.), and the production line comprises an air compressor, an air source purification system, a feeding system, a mill body, a finished product collection system, an electric appliance control cabinet and the like. Controlling technological parameters: the jet milling pressure is 0.8MPa, the rotational speed of the grader is 12000r/min, and the detection results of the wollastonite powder product processed by the device are shown in Table 1.
TABLE 1
Claims (7)
1. An inorganic composite powder characterized in that: the inorganic composite powder is CaSiO3-SiO2-CaCO3The inorganic composite powder with the structure comprises the following components in percentage by weight:
CaSiO3 60-80%
SiO2 5-25%
CaCO3 5-25%;
the CaSiO3-SiO2-CaCO3The specific surface area of the inorganic composite powder with the structure is 5-20m2/g;
The preparation method of the inorganic composite powder comprises the following steps:
s1, preparing wollastonite slurry from wollastonite powder, a dispersing agent I and water, adjusting the pH to 6.0-6.5, and grinding, wherein the particle size X of the wollastonite powder5030-70um, and CaSiO in the wollastonite powder3The content of (A) is 85-95%;
s2, preparing quartz sand, a dispersant II and water into quartz sand slurry, adjusting the pH to 5.5-6.2, and grinding to obtain the quartz sand with the granularity X50Is 10-20um, SiO in the quartz sand2The content of (A) is 92-98%;
s3, separating the product obtained in the step S1 and the product obtained in the step S2 from grinding media, and then mixing, grinding and separating the grinding media, wherein the silicon isCaSiO in limestone powder3With SiO in quartz sand2The weight ratio of (A) to (B) is 2.4-16: 1;
s4, mixing calcite with the particle size X, dispersing agent III and water to form calcite slurry, and mixing and grinding the calcite slurry with the product obtained in the step S35010-20um, CaCO in the calcite3Is 90-99%, the weight ratio of the calcite slurry to the product obtained in step S3 is 1: 4-15;
s5, separating the product obtained in the step S4 from grinding media, removing iron pollutants, concentrating, drying and depolymerizing.
2. The inorganic composite powder according to claim 1, characterized in that: the particle diameter x of the inorganic composite powder50Is 0.1-2 um.
3. The inorganic composite powder according to claim 2, characterized in that: the particle diameter x of the inorganic composite powder90Is 0.2-5 um.
4. The method for preparing an inorganic composite powder according to claim 1, wherein the method comprises the steps of: the concentration of wollastonite powder in the wollastonite slurry is 30-40%, the dispersing agent I is sodium hexametaphosphate, and the addition amount of the dispersing agent I is 0.5-0.6% of the mass of the wollastonite powder;
the grinding medium of the step S1 is zirconia balls with the diameter of 0.6-0.8mm, the filling rate of the medium is 45-50%, and the grinding is carried out for 90-150min at 1500-1600 rpm.
5. The method for preparing an inorganic composite powder according to claim 1, wherein the method comprises the steps of: the concentration of quartz sand in the quartz sand slurry is 45-55%, the dispersing agent II is sodium polyphosphate, and the addition amount of the dispersing agent II is 0.6-0.7% of the mass of the quartz sand;
the grinding medium of the step S2 is zirconia balls with the diameter of 0.4-0.5mm, the filling rate of the medium is 50-55%, and the grinding is carried out for 60-90min at 1600-1700 rpm.
6. The method for preparing an inorganic composite powder according to claim 1, wherein the method comprises the steps of: the mixing conditions of the step S3 are as follows: stirring at 80-120rpm for 20-30 min;
the grinding medium of the step S3 is zirconia balls with the diameter of 0.3-0.4mm, the filling rate of the medium is 50-55%, and the grinding is carried out for 60-90min at 1600-1700 rpm.
7. The method for preparing an inorganic composite powder according to claim 1, wherein the method comprises the steps of: the concentration of calcite in the calcite slurry is 40-50%, the dispersant III is sodium polyacrylate, and the addition amount of the dispersant III is 0.7-0.8% of the mass of the calcite;
the grinding medium of the step S4 is zirconia balls with the diameter of 0.2-0.3mm, the filling rate of the medium is 55-60%, and the grinding is carried out at 1700-1800rpm for 90-120 min.
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