CN114149019B - Preparation method of high-purity heavy calcium carbonate - Google Patents
Preparation method of high-purity heavy calcium carbonate Download PDFInfo
- Publication number
- CN114149019B CN114149019B CN202111393777.5A CN202111393777A CN114149019B CN 114149019 B CN114149019 B CN 114149019B CN 202111393777 A CN202111393777 A CN 202111393777A CN 114149019 B CN114149019 B CN 114149019B
- Authority
- CN
- China
- Prior art keywords
- potassium silicate
- calcium carbonate
- raw powder
- calcite
- precipitation reaction
- 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.)
- Active
Links
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 126
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910021532 Calcite Inorganic materials 0.000 claims abstract description 93
- 239000000843 powder Substances 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000001556 precipitation Methods 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000005406 washing Methods 0.000 claims abstract description 32
- 239000011268 mixed slurry Substances 0.000 claims abstract description 23
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 18
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 15
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 15
- 239000004111 Potassium silicate Substances 0.000 claims description 37
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 37
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 37
- 235000019353 potassium silicate Nutrition 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 25
- 239000002002 slurry Substances 0.000 claims description 24
- 238000000498 ball milling Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 239000000919 ceramic Substances 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 3
- 229910052910 alkali metal silicate Inorganic materials 0.000 abstract description 66
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 abstract description 15
- 239000001095 magnesium carbonate Substances 0.000 abstract description 15
- 229910000021 magnesium carbonate Inorganic materials 0.000 abstract description 15
- 238000000576 coating method Methods 0.000 abstract description 12
- 239000011248 coating agent Substances 0.000 abstract description 11
- 239000000945 filler Substances 0.000 abstract description 6
- 239000000047 product Substances 0.000 description 19
- 238000001035 drying Methods 0.000 description 13
- 238000000227 grinding Methods 0.000 description 13
- 239000003973 paint Substances 0.000 description 13
- 238000003825 pressing Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 235000013539 calcium stearate Nutrition 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 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
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 125000002467 phosphate group Chemical class [H]OP(=O)(O[H])O[*] 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000001038 titanium pigment Substances 0.000 description 1
- 239000013053 water resistant agent Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/185—After-treatment, e.g. grinding, purification, conversion of crystal morphology
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Landscapes
- 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)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to the technical field of calcium carbonate fillers, and particularly relates to a preparation method of high-purity heavy calcium carbonate. According to the preparation method provided by the invention, calcite raw powder, alkali metal silicate and water are mixed to obtain mixed slurry, wherein the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98%, and the modulus of the alkali metal silicate is more than or equal to 3.5; and carrying out precipitation reaction on the mixed slurry, and washing the obtained precipitation reaction liquid with water to obtain the high-purity heavy calcium carbonate. The preparation method provided by the invention utilizes the property that the solubility of magnesium carbonate in water is far greater than that of calcium carbonate, so that the alkali metal silicate and magnesium carbonate are subjected to precipitation reaction to generate magnesium hydroxide large particle precipitation, then the magnesium hydroxide large particle precipitation is removed, and the rest alkali metal silicate is removed through water washing, so that a high-purity heavy calcium carbonate product is obtained, and the high-purity heavy calcium carbonate product is very suitable for being applied to inorganic coating as a high-purity inert filler.
Description
Technical Field
The invention belongs to the technical field of calcium carbonate fillers, and particularly relates to a preparation method of high-purity heavy calcium carbonate.
Background
The traditional indoor roof and wall finishing materials mainly take emulsion paint, and the flame retardant grade can only reach the B1 grade generally due to higher organic components in the emulsion paint formula, which is far from the A-grade fireproof required by the standard, and how to improve the flame retardant grade of the interior wall coating becomes a troublesome problem facing the indoor finishing industry.
The inorganic paint is prepared by taking silicate and phosphate compounds as binders and adding various pigments, fillers and auxiliaries, wherein the silicate can be divided into alkali metal silicate and silica sol, and the existing product mainly takes a potassium silicate system; because the organic components in the formula system are relatively low, and the main film forming substance is an inorganic silicate material, the paint has excellent fireproof performance and weather resistance, and because the system is relatively alkaline and the pH value is generally about 12, the system almost does not need to be added with bactericide, and the paint is a very green environment-friendly paint. However, since potassium silicate itself is sensitive to polyvalent metal ions, it is liable to react with metals such as Mg in the system 2+ Reactions occur, resulting in poor storage stability of the product, thereby affecting the end-use properties of the product.
While Mg is 2+ Mainly from inorganic filler in the system, heavy calcium carbonate is used as the most common inorganic filler in pure inorganic paint, wherein Mg 2+ The impurity content is generally 1.0%, and the content is high, which seriously affects the stability of the inorganic coating system. Chinese patent CN105001674a discloses a high purity active heavy calcium carbonate, which is modified by wet grinding, stearic acid and calcium stearate mixture as modifier, and finally the heavy calcium carbonate obtained by secondary wet grinding has white color, but no report is made on how to reduce Mg in heavy calcium carbonate 2+ Is contained in the composition.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing high purity heavy calcium carbonate, which can effectively reduce Mg in heavy calcium carbonate 2+ When the obtained high-purity heavy calcium carbonate is applied to inorganic paint, the inorganic paint has good storage stability.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of high-purity heavy calcium carbonate, which comprises the following steps:
mixing calcite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98%, and the modulus of the alkali metal silicate is more than or equal to 3.5;
carrying out precipitation reaction on the mixed slurry to obtain precipitation reaction liquid and magnesium hydroxide precipitate;
and washing the precipitation reaction liquid to obtain the high-purity heavy calcium carbonate.
Preferably, the alkali metal silicate comprises a first alkali metal silicate, a second alkali metal silicate and a third alkali metal silicate, wherein the modulus of the first alkali metal silicate is 3.5-3.9, the modulus of the second alkali metal silicate is 4-4.4, and the modulus of the third alkali metal silicate is 4.5-4.8.
Preferably, the mass of the first alkali metal silicate accounts for 30-40% of the total mass of the alkali metal silicate, the mass of the second alkali metal silicate accounts for 30-40% of the total mass of the alkali metal silicate, and the mass of the third alkali metal silicate accounts for 20-40% of the total mass of the alkali metal silicate.
Preferably, the mass of the alkali metal silicate accounts for 1-3% of the mass of the calcite raw powder.
Preferably, in the mixed slurry, the mass of the calcite raw powder accounts for 45-55% of the total mass of the calcite raw powder and water.
Preferably, the heat preservation temperature of the precipitation reaction is 45-55 ℃, and the heat preservation time of the precipitation reaction is 5-9 days.
Preferably, the precipitation reaction is carried out under stirring, and the stirring speed is 300-400 r/min.
Preferably, the mixing comprises the steps of: and premixing the calcite raw powder and water to obtain calcite raw powder slurry, and finally mixing the calcite raw powder slurry and the alkali metal silicate, wherein the temperature of the premixing and the final mixing is normal temperature, and the time of the premixing and the final mixing is independently 30-60 min.
Preferably, the number of times of washing with water is 3 to 5, and the solid-liquid ratio at each washing with water is (2 to 3): 1.
Preferably, the preparation method of the calcite raw powder comprises the following steps:
ball milling calcite to obtain calcite raw powder, wherein the ball mill for ball milling is provided with a ceramic lining, the ball milling medium is made of ceramic, and the mass percentage of calcium carbonate in calcite is more than or equal to 98%.
The invention provides a preparation method of high-purity heavy calcium carbonate, which comprises the following steps: mixing calcite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98%, and the modulus of the alkali metal silicate is more than or equal to 3.5; carrying out precipitation reaction on the mixed slurry to obtain precipitation reaction liquid and magnesium hydroxide precipitate; and washing the precipitation reaction liquid to obtain the high-purity heavy calcium carbonate. According to the preparation method provided by the invention, the calcite raw powder with the mass percentage of calcium carbonate being more than or equal to 98% is adopted as a raw material, meanwhile, the property that the solubility of magnesium carbonate in water is far greater than that of calcium carbonate is utilized, so that magnesium carbonate in the calcite raw powder can be dissolved in water, and the high-activity alkali metal silicate with the modulus being more than or equal to 3.5 is adopted to carry out precipitation reaction with the magnesium carbonate to generate magnesium hydroxide large-particle precipitation and precipitation reaction liquid, so that the content of magnesium carbonate in a heavy calcium carbonate product is greatly reduced, and then the residual alkali metal silicate is removed through water washing. According to the results of the examples, the weight percentage of the magnesium oxide of the heavy calcium carbonate product prepared by the preparation method provided by the invention is not more than 0.31%, the weight percentage of the ferric oxide is not more than 0.01%, and when the heavy calcium carbonate product is applied to the pure inorganic interior wall coating, the annual increase of the pure inorganic interior wall coating is small, and the storage stability is high.
The preparation method provided by the invention has simple steps and is suitable for industrial production.
Drawings
Fig. 1 is a flowchart of a preparation process provided in an embodiment of the present invention.
Detailed Description
The invention provides a preparation method of high-purity heavy calcium carbonate, which comprises the following steps:
mixing calcite raw powder, alkali metal silicate and water to obtain mixed slurry, wherein the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98%, and the modulus of the alkali metal silicate is more than or equal to 3.5;
carrying out precipitation reaction on the mixed slurry to obtain precipitation reaction liquid and magnesium hydroxide precipitate;
and washing the precipitation reaction liquid to obtain the high-purity heavy calcium carbonate.
In the present invention, unless otherwise specified, all raw materials used are commercially available products of values to those skilled in the art.
According to the invention, calcite raw powder, alkali metal silicate and water are mixed to obtain mixed slurry, wherein the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98%, and the modulus of the alkali metal silicate is more than or equal to 3.5.
In the invention, the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98 percent, preferably 98 to 99.5 percent. In the present invention, the particle diameter of the calcite raw powder is preferably 10 μm or less, more preferably 8 μm or less, in a specific embodiment of the present invention, the D50 of the calcite raw powder is preferably 4.5 μm or more, and the D97 of the calcite raw powder is preferably 9.7 or more.
According to the invention, the purity of heavy calcium carbonate can be improved by controlling the mass percentage of calcium carbonate in the calcite raw powder to be more than or equal to 98 percent.
The invention is beneficial to dissolving as much magnesium carbonate in water as possible and is beneficial to separating magnesium hydroxide large-particle sediment and sediment reaction liquid generated by the sediment reaction subsequently by controlling the grain diameter of the calcite raw powder to be less than or equal to 10 mu m.
In the invention, the preparation method of the calcite raw powder preferably comprises the following steps:
grinding calcite to obtain calcite raw powder, wherein the grinding is ball milling, the ball milling ball mill is provided with a ceramic lining, the ball milling medium is ceramic, and the mass percentage of calcium carbonate in the calcite is more than or equal to 98%.
In the invention, the mass percentage of calcium carbonate in calcite is preferably more than or equal to 98%, more preferably 98-99.5%. In the present invention, the calcite preferably has a particle size of 1 to 1.5cm. The invention has no special requirements on the source of calcite.
The calcite is preferably subjected to a pretreatment according to the present invention, in which the pretreatment preferably comprises: and (3) washing, drying and coarse crushing the calcite in sequence. In the present invention, the washing is preferably performed by mixing the calcite with water, and in the present invention, the number of times of the washing is preferably 2, and there is no particular requirement for the specific implementation of the washing, and the impurities on the calcite surface are removed by the washing. The calcite after washing is preferably dried in the present invention, and the drying mode is preferably air drying in the present invention. The invention preferably breaks the dried calcite coarse. In the present invention, the number of times of the rough crush is preferably 2, and the present invention has no special requirement for the specific implementation of the rough crush. The particle size of calcite is controlled to be 1-1.5 cm through coarse crushing.
In the invention, the grinding is preferably ball milling, the ball mill for ball milling is preferably provided with a ceramic lining, the material of the ball milling medium is preferably ceramic, and the specific implementation process of the ball milling is not particularly required. In a specific embodiment of the present invention, the ball-milling pot used in the ball-milling is preferably provided with a ceramic lining, and the size of the ball-milling pot is preferablyThe invention adopts the ball mill with the ceramic lining and the ceramic grinding medium to grind the calcite, and can effectively avoid the iron ion impurities introduced by the abrasion of the grinding machine and the grinding medium in the grinding process of the traditional metal grinding machine and the metal grinding medium, thereby affecting the purity of heavy calcium carbonate products.
In the invention, ball milling powder is obtained after ball milling, and the ball milling powder is preferably classified and screened to obtain the calcite raw powder, and the invention has no special requirement on the specific implementation process of decomposition screening.
In the present invention, the modulus of the alkali metal silicate is not less than 3.5, preferably 3.5 to 4.5. In a specific embodiment of the invention, the alkali metal silicate is specifically potassium silicate.
According to the invention, the modulus of the alkali metal silicate is controlled to be more than or equal to 3.5, so that the reactivity of the alkali metal silicate and magnesium carbonate in the mixed slurry can be improved, the usage amount of the alkali metal silicate is reduced as much as possible while the reaction with the magnesium carbonate in the mixed slurry is ensured, and the purity of the heavy calcium carbonate is improved.
In the present invention, the alkali metal silicate preferably includes a first alkali metal silicate, a second alkali metal silicate, and a third alkali metal silicate, and the modulus of the first alkali metal silicate is preferably 3.5 to 3.9, more preferably 3.6 to 3.8, and in a specific embodiment of the present invention, the modulus of the first alkali metal silicate is 3.5. In the present invention, the modulus of the second alkali metal silicate is preferably 4 to 4.4, more preferably 4.1 to 4.2, and in a specific embodiment of the present invention, the modulus of the second alkali metal silicate is 4. In the present invention, the modulus of the third alkali metal silicate is preferably 4.5 to 4.8, more preferably 4.6 to 4.7, and in a specific embodiment of the present invention, the modulus of the third alkali metal silicate is 4.5.
In the present invention, the mass of the first alkali metal silicate is preferably 30 to 40% and more preferably 32 to 38% of the total mass of the alkali metal silicate, and in a specific embodiment of the present invention, the mass of the first alkali metal silicate is preferably 30%, 35% or 40% of the total mass of the alkali metal silicate. In the present invention, the mass of the second alkali metal silicate is preferably 30 to 40% and more preferably 32 to 38% of the total mass of the alkali metal silicate, and in a specific embodiment of the present invention, the mass of the second alkali metal silicate is preferably 30%, 35% or 40% of the total mass of the alkali metal silicate. In the present invention, the mass of the third alkali metal silicate is preferably 20 to 40% and more preferably 21 to 38% of the total mass of the alkali metal silicate, and in a specific embodiment of the present invention, the mass of the third alkali metal silicate is preferably 20%, 30% or 40% of the total mass of the alkali metal silicate.
In the present invention, the mass of the alkali metal silicate is preferably 1 to 3% of the mass of the calcite raw powder, more preferably 1.2 to 2.5%.
In the present invention, the mass of the calcite raw powder in the mixed slurry is preferably 45 to 55%, more preferably 48 to 53% of the total mass of the calcite raw powder and water.
According to the invention, the mass of the calcite raw powder is controlled to be 45-55% of the total mass of the calcite raw powder and water, so that the magnesium carbonate in the calcite raw powder can be ensured to be dissolved in the mixed slurry as much as possible, and the magnesium carbonate reacts with the alkali metal silicate to be removed, so that the purity of the heavy calcium carbonate is improved.
In the present invention, the mixing preferably includes the steps of: premixing the calcite raw powder and water to obtain calcite raw powder slurry, and finally mixing the calcite raw powder slurry and the alkali metal silicate. In the invention, the temperature of the premixing is preferably normal temperature, the time of the premixing is preferably 30-60 min, more preferably 35-50 min, the premixing is preferably carried out under the condition of stirring, and the specific implementation process of the stirring is not particularly required. In the invention, the temperature of the final mixing is preferably normal temperature, the time of the final mixing is preferably 30-60 min, more preferably 35-50 min, the final mixing is preferably carried out under the condition of stirring, and the specific implementation process of the stirring is not particularly required.
The invention can mix the calcite raw powder, the alkali metal silicate and the water uniformly by the mixing method, which is favorable for the magnesium carbonate in the calcite raw powder to be fully dissolved and react with the alkali metal silicate.
After the mixed slurry is obtained, the mixed slurry is subjected to precipitation reaction to obtain precipitation reaction liquid and magnesium hydroxide precipitate.
In the present invention, the temperature for the precipitation reaction is preferably 45 to 55 ℃, more preferably 48 to 50 ℃. In the present invention, the heat-retaining time of the precipitation reaction is 5 to 9 days, more preferably 5.5 to 8 days. In the present invention, the precipitation reaction is preferably carried out under stirring at a rotation speed of preferably 300 to 400r/min, more preferably 350r/min.
The invention controls the temperature of the precipitation reaction to be 45-55 ℃, which is beneficial to improving the reaction rate of alkali metal silicate and magnesium carbonate. The invention controls the time of the precipitation reaction to 5-9 days, and can realize the full reaction of alkali metal silicate and magnesium carbonate. The stirring speed is controlled to be preferably 300-400 r/min during the precipitation reaction, so that the growth of magnesium hydroxide generated by the reaction of alkali metal silicate and magnesium carbonate can be prevented from being influenced when the rotating speed is too high, and the heavy calcium carbonate in the mixed slurry can be prevented from sinking when the rotating speed is too low.
In the invention, the system obtained by the precipitation reaction is preferably subjected to solid-liquid separation to obtain a precipitation reaction liquid and magnesium hydroxide precipitate. In the present invention, the solid-liquid separation is preferably performed by a vibrating screen, and in the present invention, the pore diameter of the filter pores in the vibration screening is preferably larger than the particle diameter of the calcite raw powder and smaller than the particle diameter of the magnesium hydroxide precipitate. In the invention, the magnesium hydroxide precipitate is preferably removed by solid-liquid separation to obtain a precipitation reaction liquid.
After the precipitation reaction liquid is obtained, the high-purity heavy calcium carbonate is obtained by washing the precipitation reaction liquid with water.
In the present invention, the precipitation reaction liquid is preferably dehydrated to obtain a cake, and the cake is washed with water. In the present invention, the dehydration means is preferably filter pressing. The invention has no special requirements on the specific implementation process of the filter pressing. In the present invention, the number of times of washing with water is 3 to 5. In the present invention, the solid-to-liquid ratio per washing is preferably (2 to 3): 1, more preferably (2.3 to 2.8): 1. In the present invention, it is preferable to perform the mixing washing under stirring for a period of preferably 60 to 80 minutes for each washing with water. The invention has no special requirement on the stirring rotation speed. In the present invention, after each water washing, the present invention preferably removes the washed water by press filtration.
The invention removes the residual alkali metal silicate in the filter cake by water washing.
In the invention, after the water washing, the invention preferably carries out post-treatment on the alcohol extraction product obtained by filter pressing after the water washing to obtain the high-purity heavy calcium carbonate finished product. In the present invention, the post-treatment preferably includes: sequentially drying, scattering, demagnetizing, sieving, detecting and packaging. In the invention, the drying is preferably flash drying, the specific implementation process of the flash drying is not particularly required, and the specific implementation process of the breaking, demagnetizing, sieving, detecting and packaging is not particularly required.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
According to the process flow shown in FIG. 1, the main calcite raw ore with the calcium carbonate content of more than or equal to 98 percent is selected, washed twice, dried and coarsely crushed into small particles with the diameter of 1 to 1.5cm by twice, and then conveyed to a spiral reamerGrinding in a ceramic lining ball milling tank for 30min, classifying, sieving and collecting to obtain 10 μm calcite raw powder, detecting D50 of 4.51 μm and D97 of 9.87 μm by a Markov laser particle analyzer, premixing calcite raw powder and water to obtain calcite raw powder slurry with solid content of 45%, adding 1% potassium silicate with solid content of 70% into the calcite raw powder slurry, wherein the potassium silicate with modulus of 3.5 accounts for 40%, the potassium silicate with modulus of 4.0 accounts for 40%, the potassium silicate with modulus of 4.5 accounts for 20%, stirring for 30min at room temperature, pumping the fully mixed slurry into a reaction kettle, controlling the temperature of the reaction kettle to 45 ℃ and stirring speed to 300r/min, after the reaction is completed, filtering and drying the slurry in the reaction kettle by a vibrating screen, scattering and adding water to prepare slurry with solid content of 70% and repeating waterWashing, filter pressing, water washing and filter pressing, removing residual potassium silicate in the slurry, stirring for 60min when washing each time, flash drying the filter cake after the last filter pressing, then feeding the filter cake into a collector, scattering, demagnetizing, sieving, detecting and packaging to obtain the final high-purity heavy calcium carbonate finished product.
Example 2
According to the process flow shown in FIG. 1, the main calcite raw ore with the calcium carbonate content of more than or equal to 98 percent is selected, washed twice, dried and coarsely crushed into small particles with the diameter of 1 to 1.5cm by twice, and then conveyed to a spiral reamerGrinding in a ceramic lining ball milling tank for 30min, classifying, sieving and collecting to obtain 10 mu m calcite raw powder, detecting that D50 is 4.59 mu m and D97 is 9.97 mu m by a Markov laser particle analyzer, premixing calcite raw powder and water to obtain calcite raw powder slurry with the solid content of 50%, adding potassium silicate accounting for 2% of the mass of the calcite raw powder, wherein the potassium silicate with the modulus of 3.5 accounts for 35%, the potassium silicate with the modulus of 4.0 accounts for 35%, the potassium silicate with the modulus of 4.5 accounts for 30% and the room temperature stirring time is 45min, pumping the fully mixed slurry into a reaction kettle, controlling the temperature of the reaction kettle to be 50 ℃ and the stirring speed to be 400r/min, vibrating the slurry in the reaction kettle for 7 days, scattering the slurry after the filter press drying, adding water to prepare the slurry, performing filter press, repeating the water washing, the filter press, removing the residual potassium silicate in the slurry, the water for 60min, the stirring time, the potassium silicate with the modulus of 4.5 accounts for 30min, the stirring time for 45min, the stirring time, and the completely stirring time, pumping the slurry into the reaction kettle, the stirred slurry after the stirring time is detected, the high-purity, and the obtained after the flash-drying, and the high-purity finished product is obtained after the flash-drying, and the high-purity, and the finished product is obtained after the flash-packaged.
Example 3
According to the process flow shown in FIG. 1, the main calcite raw ore with the calcium carbonate content of more than or equal to 98 percent is selected, washed twice, dried and coarsely crushed into small particles with the diameter of 1 to 1.5cm by twice, and then conveyed to a spiral reamerGrinding in a ceramic lining ball milling tank for 30min, classifying, sieving and collecting to obtain 10 μm calcite raw powder, detecting D50 of 4.52 μm and D97 of 9.79 μm by a Markov laser particle analyzer, premixing calcite raw powder and water to obtain calcite raw powder slurry with the solid content of 55%, adding potassium silicate accounting for 3% of the mass of the calcite raw powder, wherein the potassium silicate with the modulus of 3.5 accounts for 30%, the potassium silicate with the modulus of 4.0 accounts for 30%, the potassium silicate with the modulus of 4.5 accounts for 40%, stirring time at room temperature is 60min, pumping the fully mixed slurry into a reaction kettle, the temperature of the reaction kettle is controlled at 55 ℃, the stirring speed is 500r/min, the reaction time is 9 days, slurry in the reaction kettle passes through a vibrating screen after the reaction is finished, the filtrate is subjected to filter pressing and drying, then the slurry is dispersed and added with water to prepare slurry again, the solid content of the slurry is 70%, the water washing, the filter pressing, the water washing and the filter pressing are repeated, the residual potassium silicate in the slurry is removed, the stirring time is 60 minutes during each water washing, the filter cake after the last filter pressing is subjected to flash evaporation and drying and then enters a collector, the dispersed, the demagnetized, sieved and detected and packaged to obtain the final high-purity heavy calcium carbonate finished product.
Comparative example 1
Selecting a main calcite raw ore with the calcium carbonate content of more than or equal to 98 percent, cleaning the main calcite raw ore twice, air-drying the main calcite raw ore, coarsely crushing the main calcite raw ore into small particles with the diameter of 1-1.5 cm after the main calcite raw ore is dried, and conveying the main calcite raw ore to a spiral reamerGrinding in a metal lining ball milling tank for 30min, classifying, sieving and collecting to obtain 10 μm calcite powder, sieving, detecting and packaging to obtain the final heavy calcium carbonate finished product.
Test example 1
The high purity heavy calcium carbonate powder prepared in examples 1 to 3 and the corresponding fineness calcite powder produced in comparative example 1 by the conventional production process were subjected to correlation index detection according to HG/T3249-2013, and the correlation indexes are shown in Table 1:
TABLE 1 Performance test data for heavy calcium carbonate produced in examples 1-3 and comparative example 1
| Detection index | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Whiteness degree | 95.5 | 95.4 | 95.5 | 95.1 |
| D50(μm) | 4.51 | 4.59 | 4.52 | 4.55 |
| D97(μm) | 9.87 | 9.97 | 9.79 | 9.92 |
| Oil absorption (mL/100 g) | 25 | 24 | 24 | 26 |
| Moisture (%) | 0.3 | 0.3 | 0.3 | 0.3 |
| MgO content (%) | 0.31 | 0.20 | 0.27 | 0.98 |
| Fe 2 O 3 Content (%) | 0.01 | 0.01 | 0.01 | 0.08 |
As can be seen from Table 1, compared with comparative example 1, the preparation method of the present invention provides a heavy calcium carbonate product having MgO content and Fe 2 O 3 The content is obviously reduced, and the high-purity inert filler is very suitable for being applied to inorganic coating.
Application example
The heavy calcium carbonate prepared in examples 1 to 3 and comparative example 1 was applied to an inorganic interior wall coating. The formula of the inorganic interior wall coating comprises the following components: 258.5g of water, 5g of cellulose, 4g of dispersing agent, 1g of wetting agent, 2g of defoamer, 3g of stabilizer, 150g of titanium pigment, 200g of heavy calcium, 75g of sericite, 75g of bentonite, 1.5g of defoamer, 4g of thickener, 70g of odor-free emulsion, 220g of potassium silicate and 3g of water-resistant agent. The preparation method of the inorganic interior wall coating comprises the following steps: mixing the above materials uniformly.
Test example 2
And carrying out related index detection on the inorganic interior wall coating prepared in the application example according to GB/T9756-2014. Wherein: storage stability test evaluation: the smaller the viscosity increase after 30 days of heat storage at 50 ℃, the better the paint stability, and the worse the paint storage stability is when the viscosity increase value is more than or equal to 10 KU; evaluation of Water resistance: after the template is soaked in water for 30 days, the more easily the powder is dropped, the poorer the water resistance is; cracking resistance: the thicker the crack thickness, the better the crack resistance of the coating. The test results are shown in Table 2, and it can be seen from Table 2 that the high-purity heavy calcium carbonate products produced by using the examples 1-3 of the invention are applied to pure inorganic paint, and the storage stability of the high-purity heavy calcium carbonate products is obviously better than that of the ordinary calcite product (comparative example 1), so that the use requirements of the inorganic paint are completely met.
Table 2 performance test data for inorganic interior wall coatings produced from heavy calcium carbonate of examples 1 to 3 and comparative example 1 as filler
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (7)
1. The preparation method of the high-purity heavy calcium carbonate is characterized by comprising the following steps of:
mixing calcite raw powder, potassium silicate and water to obtain mixed slurry, wherein the mass percentage of calcium carbonate in the calcite raw powder is more than or equal to 98%, and the modulus of the potassium silicate is more than or equal to 3.5; the mass of the potassium silicate accounts for 1-3% of the mass of the calcite raw powder;
carrying out precipitation reaction on the mixed slurry to obtain precipitation reaction liquid and magnesium hydroxide precipitate; the heat preservation temperature of the precipitation reaction is 45-55 ℃, and the heat preservation time of the precipitation reaction is 5-9 days; the precipitation reaction is carried out under the condition of stirring, and the rotating speed of the stirring is 300-400 r/min; carrying out solid-liquid separation on the system obtained by the precipitation reaction to obtain precipitation reaction liquid and magnesium hydroxide precipitate, wherein the solid-liquid separation mode is that a vibrating screen is used for filtering, and the pore diameter of a filtering hole during the filtering of the vibrating screen is larger than the particle diameter of the calcite raw powder and smaller than the particle diameter of the magnesium hydroxide precipitate;
and washing the precipitation reaction liquid to obtain the high-purity heavy calcium carbonate.
2. The method according to claim 1, wherein the potassium silicate comprises a first potassium silicate, a second potassium silicate and a third potassium silicate, the modulus of the first potassium silicate is 3.5 to 3.9, the modulus of the second potassium silicate is 4 to 4.4, and the modulus of the third potassium silicate is 4.5 to 4.8.
3. The method according to claim 2, wherein the first potassium silicate accounts for 30 to 40% of the total mass of the potassium silicate, the second potassium silicate accounts for 30 to 40% of the total mass of the potassium silicate, and the third potassium silicate accounts for 20 to 40% of the total mass of the potassium silicate.
4. The preparation method according to claim 1, wherein the mass of the calcite raw powder in the mixed slurry is 45-55% of the total mass of the calcite raw powder and water.
5. The method of preparing according to claim 1, wherein the mixing comprises the steps of: premixing the calcite raw powder and water to obtain calcite raw powder slurry, and finally mixing the calcite raw powder slurry and the potassium silicate, wherein the temperature of the premixing and final mixing is normal temperature, and the time of the premixing and final mixing is independently 30-60 min.
6. The method according to claim 1, wherein the number of times of washing with water is 3 to 5, and the solid-to-liquid ratio per washing with water is (2 to 3): 1.
7. The preparation method according to claim 1, wherein the preparation method of calcite raw powder comprises the following steps:
ball milling calcite to obtain calcite raw powder, wherein the ball mill for ball milling is provided with a ceramic lining, the ball milling medium is made of ceramic, and the mass percentage of calcium carbonate in calcite is more than or equal to 98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111393777.5A CN114149019B (en) | 2021-11-23 | 2021-11-23 | Preparation method of high-purity heavy calcium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111393777.5A CN114149019B (en) | 2021-11-23 | 2021-11-23 | Preparation method of high-purity heavy calcium carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114149019A CN114149019A (en) | 2022-03-08 |
| CN114149019B true CN114149019B (en) | 2024-02-06 |
Family
ID=80457444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111393777.5A Active CN114149019B (en) | 2021-11-23 | 2021-11-23 | Preparation method of high-purity heavy calcium carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114149019B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB117483A (en) * | 1917-07-13 | 1918-07-15 | Henry William Coupe Annable | Improvements in or relating to the Separation of Magnesium from Compounds and Mixtures of Magnesium and Calcium Carbonates. |
| GB1539223A (en) * | 1975-11-03 | 1979-01-31 | Woodville Lime & Chem Co | Preparation of pure magnesian values |
| RU2007111601A (en) * | 2007-03-29 | 2008-10-10 | Открытое Акционерное Общество "КАУСТИК" (RU) | MULTIFUNCTIONAL FILLER BASED ON CHEMICALLY DEPOSITED CALCIUM CARBONATE AND METHOD FOR ITS PRODUCTION |
| CN102583482A (en) * | 2012-02-14 | 2012-07-18 | 浙江大学 | Preparation method of flake-shaped aragonite calcium carbonate |
| CN109231249A (en) * | 2018-09-25 | 2019-01-18 | 太原理工大学 | A kind of high efficiency extraction blast furnace slag active constituent and carbonate fixed CO2The method for producing calcium carbonate |
| CN109734114A (en) * | 2018-03-12 | 2019-05-10 | 孙子涵 | A kind of calcite preparation method of high-content calcium carbonate |
| CN111908510A (en) * | 2019-05-16 | 2020-11-10 | 清华大学 | Preparation method of high-purity manganese sulfate |
| CN112694115A (en) * | 2021-01-11 | 2021-04-23 | 湖北三宁化工股份有限公司 | Method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2540248T3 (en) * | 2010-10-26 | 2015-07-09 | Omya Development Ag | Production of high purity precipitated calcium carbonate |
-
2021
- 2021-11-23 CN CN202111393777.5A patent/CN114149019B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB117483A (en) * | 1917-07-13 | 1918-07-15 | Henry William Coupe Annable | Improvements in or relating to the Separation of Magnesium from Compounds and Mixtures of Magnesium and Calcium Carbonates. |
| GB1539223A (en) * | 1975-11-03 | 1979-01-31 | Woodville Lime & Chem Co | Preparation of pure magnesian values |
| RU2007111601A (en) * | 2007-03-29 | 2008-10-10 | Открытое Акционерное Общество "КАУСТИК" (RU) | MULTIFUNCTIONAL FILLER BASED ON CHEMICALLY DEPOSITED CALCIUM CARBONATE AND METHOD FOR ITS PRODUCTION |
| CN102583482A (en) * | 2012-02-14 | 2012-07-18 | 浙江大学 | Preparation method of flake-shaped aragonite calcium carbonate |
| CN109734114A (en) * | 2018-03-12 | 2019-05-10 | 孙子涵 | A kind of calcite preparation method of high-content calcium carbonate |
| CN109231249A (en) * | 2018-09-25 | 2019-01-18 | 太原理工大学 | A kind of high efficiency extraction blast furnace slag active constituent and carbonate fixed CO2The method for producing calcium carbonate |
| CN111908510A (en) * | 2019-05-16 | 2020-11-10 | 清华大学 | Preparation method of high-purity manganese sulfate |
| CN112694115A (en) * | 2021-01-11 | 2021-04-23 | 湖北三宁化工股份有限公司 | Method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114149019A (en) | 2022-03-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101706396B1 (en) | Process for manufacturing calcium carbonate materials having a particle surface with improved adsorption properties | |
| US5910214A (en) | Process for preparing calcium carbonate | |
| CN111269606B (en) | High-purity high-thickening easy-to-disperse nano montmorillonite used in water-based paint field and preparation method thereof | |
| CN101570344A (en) | Preparation method of aragonite crystal form calcium carbonate | |
| CN108928834B (en) | MCM-41 mesoporous molecular sieve, and preparation method and application thereof | |
| EP3738926A1 (en) | Preparation method for nanoprecipitated calcium carbonate having core-shell structure | |
| US2140375A (en) | Method of producing finely divided calcium carbonate which does not agglomerate | |
| CN105271344A (en) | Preparation method of pine-cone-shaped calcite type micron-size calcium carbonate particles | |
| CN114149019B (en) | Preparation method of high-purity heavy calcium carbonate | |
| CN109179471B (en) | Preparation method of light calcium carbonate with anti-sedimentation property | |
| JPH1111941A (en) | Production of light calcium carbonate | |
| CN108946754B (en) | SBA-15 mesoporous molecular sieve, preparation method and application thereof, and method for producing alumina and SBA-15 mesoporous molecular sieve from fly ash | |
| JPH0543815A (en) | Surface-treated calcium carbonate and production thereof | |
| CN103254493B (en) | Noctilucent stone paper and its preparation method and application | |
| CN110510650A (en) | The preparation method and nanometer calcium carbonate of nanometer calcium carbonate | |
| CN102115618B (en) | Extinction barium and preparation method thereof | |
| JP2001270713A (en) | Method for producing calcium carbonate having aragonite crystal system | |
| CN114621605A (en) | Mixed calcium carbonate filler and preparation method thereof | |
| US3653937A (en) | Alumina trihydrate pigment and process for the preparation thereof | |
| JPS63260816A (en) | Manufacture of fine grain calcium sulfate | |
| CA3175598A1 (en) | Calcium carbonate-containing material | |
| CN112358742A (en) | 99-grade heavy calcium carbonate and preparation method thereof | |
| CN109667189B (en) | Preparation method of chrysanthemum-shaped light calcium carbonate filler | |
| CN105819482A (en) | Method for preparing precipitated calcium carbonate having metastable crystal phase | |
| CN115092939B (en) | Preparation method of wollastonite powder |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |