CN114291835B - Preparation method of large-small cubic dispersion precipitated calcium carbonate - Google Patents
Preparation method of large-small cubic dispersion precipitated calcium carbonate Download PDFInfo
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- CN114291835B CN114291835B CN202111664054.4A CN202111664054A CN114291835B CN 114291835 B CN114291835 B CN 114291835B CN 202111664054 A CN202111664054 A CN 202111664054A CN 114291835 B CN114291835 B CN 114291835B
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 262
- 229940088417 precipitated calcium carbonate Drugs 0.000 title claims abstract description 116
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000006185 dispersion Substances 0.000 title abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 64
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 61
- 239000002002 slurry Substances 0.000 claims abstract description 61
- 239000000725 suspension Substances 0.000 claims abstract description 58
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 56
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 56
- 239000004571 lime Substances 0.000 claims abstract description 56
- 238000002156 mixing Methods 0.000 claims abstract description 23
- 239000013078 crystal Chemical group 0.000 claims abstract description 21
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000007873 sieving Methods 0.000 claims abstract description 18
- 238000009423 ventilation Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims abstract description 14
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000008117 stearic acid Substances 0.000 claims abstract description 13
- 238000007127 saponification reaction Methods 0.000 claims abstract description 12
- 238000004381 surface treatment Methods 0.000 claims abstract description 12
- 235000021357 Behenic acid Nutrition 0.000 claims abstract description 10
- 229940116226 behenic acid Drugs 0.000 claims abstract description 10
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [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 abstract description 8
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims abstract description 8
- 159000000009 barium salts Chemical class 0.000 claims abstract description 7
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims abstract description 7
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims abstract description 7
- 229940048086 sodium pyrophosphate Drugs 0.000 claims abstract description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 32
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 23
- 239000001569 carbon dioxide Substances 0.000 claims description 22
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 22
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 16
- 239000000920 calcium hydroxide Substances 0.000 claims description 16
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 16
- 239000000292 calcium oxide Substances 0.000 claims description 13
- 235000012255 calcium oxide Nutrition 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 9
- 230000005484 gravity Effects 0.000 claims description 9
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007670 refining Methods 0.000 claims description 8
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical group [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 6
- 229910001626 barium chloride Inorganic materials 0.000 claims description 6
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 5
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 4
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 claims description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 3
- 229960003237 betaine Drugs 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 3
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 3
- 238000011085 pressure filtration Methods 0.000 claims description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims 1
- 239000000565 sealant Substances 0.000 abstract description 18
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 238000012856 packing Methods 0.000 abstract description 4
- 230000003014 reinforcing effect Effects 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 2
- 229910021532 Calcite Inorganic materials 0.000 description 19
- 239000000047 product Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000002245 particle Substances 0.000 description 9
- 238000003825 pressing Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 235000019738 Limestone Nutrition 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
- 239000006028 limestone Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000000945 filler Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000004590 silicone sealant Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 230000033558 biomineral tissue development Effects 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000012265 solid product Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- IVKNZCBNXPYYKL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO)C=C1 IVKNZCBNXPYYKL-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 238000001016 Ostwald ripening Methods 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000010797 grey water Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 235000015170 shellfish Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of large and small cubic dispersion precipitated calcium carbonate, which comprises the steps of firstly adding sodium hexametaphosphate or a crystal form control agent compounded by sodium pyrophosphate and soluble barium salt into lime slurry, and stopping ventilation when carbonation reaction is carried out until pH is 8.0 to obtain rod-shaped precipitated calcium carbonate suspension; adding a crystal form control agent into lime slurry, stopping ventilation when the pH value of a reaction system is 7.5, and obtaining cubic precipitated calcium carbonate suspension; mixing rod-shaped precipitated calcium carbonate suspension and cubic precipitated calcium carbonate suspension according to a proportion, adding behenic acid, uniformly mixing, performing surface treatment by stearic acid saponification liquid, press-filtering, drying and sieving to obtain the large-small cubic dispersed precipitated calcium carbonate powder. The precipitated calcium carbonate prepared by the invention has the advantages of monodispersed morphology, smooth large-particle-diameter surface, low oil absorption value and the like; when used as packing of sealant products, the nano calcium carbonate has better compatibility, and the flowability of the sealant is greatly improved while the reinforcing performance of the nano calcium carbonate with small vertical diameter is ensured.
Description
Technical Field
The invention relates to the technical field of inorganic materials, in particular to a preparation method of large and small cubic dispersion precipitated calcium carbonate.
Background
Precipitated calcium carbonate is an inorganic material that forms a precipitate by chemical reaction. Precipitated calcium carbonate is widely used as a filler or extender in various industries, such as paper, paint, plastics, polymers, foods, food materials, pharmaceuticals, cosmetics, and the like. Precipitated calcium carbonate produced by precipitation processes has three anhydrous crystalline forms of calcite, aragonite and vaterite, wherein calcite is the most thermodynamically stable form at room temperature and pressure, aragonite is in a semi-stable state and vaterite is unstable, and both become stable calcite in the final stage of mineralization, and commercially, aragonite and vaterite are also converted to more stable calcite. Of these three crystalline forms, only aragonite and calcite are commercially available, the aragonite being of orthorhombic (needle-like) crystal structure, whereas calcite is of hexagonal-rhombohedral structure, which can be any of 300 different forms. In precipitated calcium carbonate, diamond (cubic), truncated prism, bevel (rhombohedral), spherical and chain-like agglomerates and the like may occur.
Precipitated calcium carbonate may be produced in a number of ways, such as lime soda, double decomposition and carbonation, the latter being the only method in which precipitated calcium carbonate is considered the main product, in both lime soda and double decomposition PCC is a by-product, in all of which limestone raw material is used directly or indirectly as a calcium source. Multiphase (gas-solid-liquid) carbonation is today the most common method for producing precipitated calcium carbonate, in the process by adding CO to the process 2 The mixed gas is blown into the lime slurry suspension to produce precipitated calcium carbonate.
At present, nano calcium carbonate (precipitated calcium carbonate with the particle size smaller than 100 nm) is mainly used as a filling material in the sealant, the viscosity and tensile strength of the sealant can be greatly improved by filling the nano calcium carbonate, but the thixotropic property and the fluidity are greatly reduced while the excellent strength of the sealant is given, and a part of many industrial solutions are to add more expensive thixotropic agents and plasticizers, and the other part is to add heavy calcium carbonate (GCC) to adjust the rheological property. In addition, the heavy calcium carbonate also greatly reduces the storage time of the sealant because of the hydrophilic surface. Precipitated calcium carbonate is more advantageous than natural and ground calcium carbonate relative to ground calcium carbonate. For example, it has unique characteristics of submicron particle size, organized crystalline form, narrow particle size distribution range, and high purity. If heavy calcium carbonate is replaced by large cubic calcite precipitated calcium carbonate with low specific surface area in the filler, whether nano calcium carbonate can be ensured to be reinforced and simultaneously the thixotropy and the fluidity are improved is a significant study. The aragonite type calcium carbonate is unstable and is easy to be converted into calcite, but similar reports are mostly reported in research on rock-soil minerals or biomineralization, and industrial methods for converting aragonite into calcite and application effects after conversion are rarely reported. The commercially produced aragonite calcium carbonate is relatively stable and the conversion of aragonite to calcite requires special treatment methods.
Patent CN104087029B discloses a preparation method of active calcium carbonate special for silicone sealant, which mainly comprises the steps of mixing nano calcium carbonate and rod-shaped calcium carbonate slurry through grading, and then performing secondary surface treatment, filter pressing and drying to obtain mixed powder of nano cubes and rods. The powder obtained by the method is simply mixed and does not relate to crystal form transformation.
Patent CN110451545a discloses a preparation method of rod-shaped calcium carbonate for PE breathable film, which comprises calcining limestone at 1100-1250 ℃ to form quicklime, digesting the quicklime to obtain Ca (OH) 2, and preparing refined Ca (OH) 2 into Ca (OH) 2 suspension with specific gravity of 1.030-1.050; delivering Ca (OH) 2 suspension into a carbonation reaction kettle, adding tetrasodium pyrophosphate solution, starting stirring, introducing mixed gas containing carbon dioxide, adding tween-20 when the pH value of a reaction system is reduced to 10.5, continuing to react until the pH value of the reaction system is reduced to 6.5-7.0, and finishing carbonation reaction to obtain calcium carbonate slurry; aging calcium carbonate slurry at 60-80deg.C for 5-8 hr, surface treating with sodium stearate, respectively drying, pulverizing, grading, and packaging to obtain rod-like calcium carbonate. The rod-shaped calcium carbonate prepared by the method is relatively stable, and does not have the phenomenon of conversion into calcite.
Patent CN107445188A discloses a preparation method of rod-shaped precipitated calcium carbonate, which is to obtain lime slurry by slaking after limestone calcination; placing lime slurry into a carbonation reaction tower, stirring, controlling the temperature of the reaction system to 40-80 ℃, introducing mixed gas with the concentration of carbon dioxide of 5-15vol% and the flow of 2-4m in the early reaction period of 0-30min 3 And (3) introducing mixed gas with the concentration of carbon dioxide of 25-40vol% and the flow of 4-6m < 3 >/h in the later stage of the carbonation reaction, stopping ventilation when the pH value of the reaction system reaches 7.5, and stopping the carbonation reaction to obtain a precipitated calcium carbonate suspension; and dehydrating the precipitated calcium carbonate suspension, and drying to obtain the rod-shaped precipitated calcium carbonate. The obtained rod-like calcium carbonate is stable powder, and has no rod-like cubic shapeAnd (3) converting.
CN106430272a discloses a preparation method of rod-shaped aragonite calcium carbonate, (1) crushing limestone, calcining for 2-7 h at 900-1400 ℃, and then digesting the calcined limestone with a gray water mass ratio of 1:3-8 to obtain lime slurry; (2) Sieving the lime slurry obtained in the step (1) with a sieve of 80-100 meshes, filtering to remove slag, and adding water to adjust the solid content of the lime slurry to 7-20% to obtain refined lime slurry for later use; (3) Controlling the temperature of refined lime slurry to be 30-60 ℃, adding a composite crystal form control agent which is 0.5-2.0% of the mass of calcium hydroxide in the lime slurry, conveying the lime slurry to a carbonization tower, starting stirring, introducing kiln gas to carry out carbonation reaction until the pH value is 8.0, stopping ventilation, and stopping carbonation reaction to obtain a precipitated calcium carbonate suspension; the composite crystal form control agent consists of three components, wherein the first component is polycarboxylic acid and/or polycarboxylic acid soluble salt, and the second component is one or a combination of more of calcium chloride, barium chloride, zinc chloride, calcium nitrate, barium nitrate, zinc nitrate, calcium sulfate, barium sulfate and zinc sulfate; the third component is one or a combination of more of polyethylene glycol, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and OP-10; the first component in the composite crystal form control agent comprises: and a second component: the mass ratio of the third component is 1:1.5-2:0.2-0.5; (4) And (3) dehydrating and drying the precipitated calcium carbonate suspension obtained in the step (3) according to a conventional method to obtain the rod-shaped aragonite type calcium carbonate. The rod-shaped calcium carbonate prepared by the method exists as stable powder, and the transformation from a rod shape to a cubic shape is not involved.
CN108299811a discloses a preparation method of a calcium carbonate rod-shaped nanoparticle composite material, dispersing calcium oxide particles in deionized water, adding a composite surfactant, stirring uniformly, treating feed liquid under microwaves, introducing feed liquid into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, spraying the feed liquid under ultrasonic conditions, centrifuging to separate the feed liquid, taking a clear liquid, centrifuging at a high speed, washing with deionized water, and drying, wherein the obtained calcium carbonate rod-shaped nanoparticle and polycaprolactone are subjected to melt coextrusion to obtain the calcium carbonate rod-shaped nanoparticle composite material. The method is to prepare rod-shaped particles and mix the particles with a polymer, and does not involve the conversion of the rod-shaped particles into cubes.
CN201911403399.7 discloses a preparation method of hollow rod-like calcium carbonate, firstly weighing calcium oxide, and dissolving the calcium oxide in water to prepare raw material calcium hydroxide slurry; then adding D-sodium gluconate and introducing CO 2 Gas reaction and carbonation to obtain product slurry; and (3) carrying out suction filtration and washing on the product slurry, carrying out vacuum drying on the separated solid product, and finally taking out and grinding the solid product into powder to obtain the hollow rod-shaped calcium carbonate. The hollow rod-shaped calcium carbonate prepared by the method is not converted into cubic calcite-type calcium carbonate.
The conversion of aragonite prepared using shellfish, ores, metathesis to calcite by DTA-TG heating (SAYOKO YOSHIOKA et al, geochemical Journal vol.19, pp.245to 249,1985) was reported, the dehydration of water during heating was investigated with the concomitant conversion of the crystalline form, and the sample was not XRD characterized in this study.
In summary, currently, few studies are made industrially on the method of converting the rod-shaped aragonite form into the cubic calcite form, and few reports are made abroad only on the research of converting marine organisms into aragonite form, and remain on experimental studies. In order to obtain cubic dispersed precipitated calcium carbonate with good dispersibility, a method which is easy to operate and can be used for industrial production is needed.
Disclosure of Invention
Aiming at the problems of greatly reducing the viscosity and storage stability of the sealant by doping heavy calcium carbonate in order to improve the flow property of the nano calcium carbonate used in the sealant, the invention provides a preparation method of large-small cubic dispersion precipitated calcium carbonate. The precipitated calcium carbonate prepared by the invention has the advantages of monodispersed morphology, smooth large-particle-diameter surface, low oil absorption value and the like; when used as packing of sealant products, the nano calcium carbonate has better compatibility, and the flowability of the sealant is greatly improved while the reinforcing performance of the nano calcium carbonate with small vertical diameter is ensured.
In order to achieve the above object, the present invention adopts the following technical principle:
since the general precipitated rod-shaped calcium carbonate is relatively stable, industrially produced rod-shaped calcium carbonate is generally used directly for downstream applications. In the process of carbonating lime slurry, the crystal form control can be adjusted to enable the rod-shaped calcium carbonate to be in a metastable state, and in the subsequent heat treatment process, the aragonite-shaped calcium carbonate in the metastable state overcomes the internal energy, and the heat state unit cell expands to gradually change into a more stable calcite-type cube. In the heat treatment process, the aragonite in a metastable state is dissolved in preference to cubic calcite, the surface of the cubic nano calcium carbonate is gradually grown according to Ostwald ripening through the action of dissolution and recrystallization, the rod-shaped structure overcomes the internal energy of particles at high temperature, and phase transition is rapidly formed under the condition of existence of calcite crystal nucleus, so that the aragonite is converted into stable large-particle calcite.
In order to achieve the above object, the present invention adopts the following technical scheme:
a preparation method of cubic dispersed precipitated calcium carbonate comprises the following steps:
s1, slaking quicklime, sieving, refining and preparing lime slurry with the specific gravity of 1.040-1.050, and aging for 12-24 hours for later use;
s2, adding a crystal form control agent into the lime slurry, wherein the crystal form control agent is compounded by sodium hexametaphosphate or sodium pyrophosphate and soluble barium salt, introducing carbon dioxide mixed gas into the lime slurry, stopping ventilation when the pH value of a reaction system is 8.0, and ending the carbonation reaction to obtain a rod-shaped precipitated calcium carbonate suspension;
s3, adding a crystal form control agent into the lime slurry, wherein the crystal form control agent is one or more of sodium dodecyl sulfate, dodecyl trimethyl betaine and sodium polystyrene sulfonate; introducing carbon dioxide mixed gas into lime slurry, stopping ventilation when the pH value of a reaction system is 7.5, and ending carbonation reaction to obtain cubic precipitated calcium carbonate suspension;
s4, mixing the rod-shaped precipitated calcium carbonate suspension obtained in the step S2 and the cubic precipitated calcium carbonate suspension obtained in the step S3 in proportion, adding behenic acid, uniformly mixing, heating to 90-95 ℃ and maintaining for 1.0 hour to obtain a large-small cubic dispersed precipitated calcium carbonate suspension;
and S5, carrying out surface treatment on the precipitated calcium carbonate suspension through stearic acid saponification liquid, carrying out pressure filtration, drying and sieving to obtain the cubic dispersed precipitated calcium carbonate powder.
Preferably, the addition amount of the crystal form control agent in the step S2 is 0.3-1.5% of the dry content of the calcium hydroxide.
Preferably, the mass ratio of sodium hexametaphosphate or sodium pyrophosphate to soluble barium salt in step S2 is 4-10:1.
Preferably, the soluble barium salt is barium chloride or/and barium nitrate.
Preferably, the addition amount of the crystal form control agent in the step S3 is 0.1-0.4% of the dry content of the calcium hydroxide.
Preferably, the carbonation reaction in the step S2 controls the initial carbonation temperature of lime slurry to be 45.0-55.0 ℃, the concentration of carbon dioxide mixed gas to be 15-18% and the air inlet flow to be 2.0-3.0m 3 /h。
Preferably, the carbonation reaction in the step S3 controls the initial carbonation temperature of lime slurry to be 18.0-23.0 ℃, the concentration of carbon dioxide mixed gas to be 30-33% and the air inlet flow to be 2.0-3.0m3/h.
Preferably, the consumption of the behenic acid is 0.5-0.8% of the dry weight of the calcium carbonate.
Preferably, the dosage of the stearic acid saponification liquid is 3.0-3.5% of the dry mass of the calcium carbonate. The stearic acid saponification liquid is prepared by sodium hydroxide accounting for 15% of the mass of stearic acid.
Preferably, the surface modification in step S5 is carried out at a temperature of 90-95 ℃ and a rotation speed of 2500-3000r/min for 30-60min.
Preferably, the mass ratio of the rod-shaped precipitated calcium carbonate suspension to the cubic precipitated calcium carbonate suspension is 1:1-10.
Compared with the prior art, the invention has the advantages that:
1. the method of the invention utilizes the unstable characteristic of the rod-shaped aragonite type precipitated calcium carbonate to control the rod-shaped forming process, so that the aragonite mixed with the nano calcium carbonate slurry can be quickly converted into calcite at a lower temperature.
2. The preparation process of the product is accompanied with an accelerated curing stage, so that the dispersibility of the nano calcium carbonate is improved, the surface of the calcium carbonate is smoother, and the subsequent surface treatment coating is more sufficient.
3. The precipitated calcium carbonate prepared by the invention has the advantages of monodispersed morphology, smooth large-particle-diameter surface, low oil absorption value and the like; when used as packing of sealant products, the nano calcium carbonate has better compatibility, and the flowability of the sealant is greatly improved while the reinforcing performance of the nano calcium carbonate with small vertical diameter is ensured.
4. The method has low production cost, is suitable for industrial production, and the prepared precipitated calcium carbonate has better processing performance when being used as a packing material of the sealant, because the precipitated calcium carbonate replaces heavy calcium carbonate with larger water absorption, the storage stability of the sealant is greatly improved, the sealant is endowed with excellent adhesive property and tensile strength, and the flowability is improved.
Drawings
FIG. 1 is a 500X SEM image of a precipitated rod-shaped calcium carbonate product obtained according to example 1.
Fig. 2 is a 50000-fold SEM image of the cubic dispersed precipitated calcium carbonate product of size obtained in example 1.
Fig. 3 is a 50000-fold SEM image of the cubic dispersed precipitated calcium carbonate product of size obtained in example 1.
Fig. 4 is an XRD image after proportional mixing and transformation of the rod-shaped precipitated calcium carbonate suspension and the cubic precipitated calcium carbonate suspension of example 1.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. 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
A preparation method of cubic dispersed precipitated calcium carbonate comprises the following steps:
s1, carrying out digestion reaction on quicklime and water according to a ratio of 1:6, sieving, refining and preparing lime slurry with a specific gravity of 1.050, and aging for 12 hours for later use;
s2, adding sodium hexametaphosphate with calcium hydroxide dry basis content of 0.5 percent and barium chloride with calcium hydroxide dry basis content of 0.1 percent into lime slurry, controlling the temperature of the lime slurry to be 50 ℃ and controlling the temperature of the lime slurry to be 2.0m 3 Introducing a carbon dioxide mixed gas with the concentration of 16% to the reaction system until the pH value of the reaction system is 8.0, stopping ventilation, and ending the carbonation reaction to obtain a rod-shaped precipitated calcium carbonate suspension;
s3, adding dodecyl trimethyl betaine with calcium hydroxide dry basis content of 0.3% into lime slurry, controlling the temperature of lime slurry at 20 ℃ and 2.0m 3 Introducing a carbon dioxide mixed gas with the concentration of 33% to the reaction system until the pH value of the reaction system is 7.5, stopping ventilation, and ending the carbonation reaction to obtain a cubic precipitated calcium carbonate suspension;
s4, mixing the rod-shaped precipitated calcium carbonate suspension obtained in the step S2 and the cubic precipitated calcium carbonate suspension obtained in the step S3 according to the mass ratio of 4:6, mixing, adding the behenic acid with the dry mass of 0.5% of calcium carbonate, uniformly mixing, heating to 90 ℃ and maintaining for 1.0 hour to obtain a large-small cubic dispersion precipitated calcium carbonate suspension;
s5, carrying out surface treatment on the precipitated calcium carbonate suspension by using stearic acid saponification liquid with the mass of 3.0% of the dry basis of calcium carbonate, carrying out filter pressing, drying and sieving to obtain the large and small cubic dispersed precipitated calcium carbonate powder.
The rod-shaped precipitated calcium carbonate prepared in step S2 of this example 1 and the cubic dispersed precipitated calcium carbonate of the size prepared in step S4 were subjected to scanning electron microscopy and X-ray diffraction detection before and after mixing, and the measurement results are shown in fig. 1 to 4. As is apparent from FIG. 1, the rod-shaped precipitated calcium carbonate prepared by the method has regular appearance, uniform size and good dispersibility. As is evident from figures 2 and 3, the rod-shaped precipitated calcium carbonate mixed product with different shapes, which is obtained by the method of the invention, is converted into a big cube and the small cube is obtained by the step S3, and the dispersibility of the product is good. As can be seen from the XRD pattern of fig. 4, the mixed product of the rod-shaped precipitated calcium carbonate prepared in S2 and the cubic precipitated calcium carbonate prepared in S3 contains aragonite and calcite, and is completely converted into calcite after addition of behenic acid and heating. In combination with scanning electron micrographs and XRD, the rod-shaped precipitated calcium carbonate is converted into large cubic precipitated calcium carbonate in the cubic precipitated calcium carbonate.
Example 2
A preparation method of cubic dispersed precipitated calcium carbonate comprises the following steps:
s1, carrying out digestion reaction on quicklime and water according to a ratio of 1:8, sieving, refining and preparing lime slurry with a specific gravity of 1.050, and aging for 20 hours for later use;
s2, adding sodium pyrophosphate with 1.0 percent of calcium hydroxide dry basis content and barium nitrate with 0.2 percent of calcium hydroxide dry basis content into lime slurry, controlling the temperature of the lime slurry to be 45 ℃ and controlling the temperature of the lime slurry to be 3.0m 3 Introducing a carbon dioxide mixed gas with the concentration of 18% to the reaction system until the pH value of the reaction system is 8.0, stopping ventilation, and ending the carbonation reaction to obtain a rod-shaped precipitated calcium carbonate suspension;
s3, adding sodium polystyrene sulfonate with calcium hydroxide dry basis content of 0.3% into the lime slurry, controlling the temperature of the lime slurry at 20 ℃ and 2.5m 3 Introducing a carbon dioxide mixed gas with the concentration of 30% to the reaction system until the pH value of the reaction system is 7.5, stopping ventilation, and ending the carbonation reaction to obtain a cubic precipitated calcium carbonate suspension;
s4, mixing the rod-shaped precipitated calcium carbonate suspension obtained in the step S2 and the cubic precipitated calcium carbonate suspension obtained in the step S3 according to the mass ratio of 1:4, mixing, adding behenic acid with the mass of 0.6% of the dry basis of calcium carbonate, uniformly mixing, heating to 95 ℃ and maintaining for 1.0 hour to obtain a large-small cubic dispersion precipitated calcium carbonate suspension;
s5, carrying out surface treatment on the precipitated calcium carbonate suspension by using stearic acid saponification liquid with the mass of 3.2% of the dry basis of calcium carbonate, carrying out filter pressing, drying and sieving to obtain the cubic dispersed precipitated calcium carbonate powder with the size.
Example 3
A preparation method of cubic dispersed precipitated calcium carbonate comprises the following steps:
s1, slaking quicklime and water according to the mass ratio of 1:9, sieving, refining and preparing lime slurry with the specific gravity of 1.040, and aging for 24 hours for later use;
s2, adding 0.8 of calcium hydroxide dry basis content into the lime slurry% sodium hexametaphosphate and 0.2% barium chloride, the lime slurry temperature was controlled at 55deg.C at 2.0m 3 Introducing a carbon dioxide mixed gas with the concentration of 15% to the reaction system until the pH value of the reaction system is 8.0, stopping ventilation, and ending the carbonation reaction to obtain a rod-shaped precipitated calcium carbonate suspension;
s3, adding sodium dodecyl sulfate with the dry content of 0.4 percent of calcium hydroxide into the lime slurry, controlling the temperature of the lime slurry at 20 ℃ and 3.0m 3 Introducing a carbon dioxide mixed gas with the concentration of 30% to the reaction system until the pH value of the reaction system is 7.5, stopping ventilation, and ending the carbonation reaction to obtain a cubic precipitated calcium carbonate suspension;
s4, mixing the rod-shaped precipitated calcium carbonate suspension obtained in the step S2 and the cubic precipitated calcium carbonate suspension obtained in the step S3 according to the mass ratio of 1:9, mixing, adding the behenic acid with the dry mass of 0.8% of calcium carbonate, uniformly mixing, heating to 90 ℃ and maintaining for 1.0 hour to obtain a cubic dispersion precipitated calcium carbonate suspension with the size;
s5, carrying out surface treatment on the precipitated calcium carbonate suspension by using stearic acid saponification liquid with the mass of 3.5% of the dry weight of calcium carbonate, carrying out filter pressing, drying and sieving to obtain the cubic dispersed precipitated calcium carbonate powder with the size.
Example 4
A preparation method of cubic dispersed precipitated calcium carbonate comprises the following steps:
s1, slaking quicklime and water according to the mass ratio of 1:7, sieving, refining and preparing lime slurry with the specific gravity of 1.040, and aging for 24 hours for later use;
s2, adding sodium hexametaphosphate with calcium hydroxide dry basis content of 0.5 percent and barium chloride with calcium hydroxide dry basis content of 0.3 percent into lime slurry, controlling the temperature of the lime slurry to 55 ℃ and controlling the temperature of the lime slurry to be 2.0m 3 Introducing a carbon dioxide mixed gas with the concentration of 18% to the reaction system until the pH value of the reaction system is 8.0, stopping ventilation, and ending the carbonation reaction to obtain a rod-shaped precipitated calcium carbonate suspension;
s3, adding sodium dodecyl sulfate with the dry content of 0.2 percent and sodium polystyrene sulfonate with the dry content of 0.2 percent into lime slurry, controlling the temperature of the lime slurry at 20 ℃ and 3.0m 3 Introducing mixed gas of carbon dioxide with the concentration of 33% to the reaction kettleStopping ventilation when the pH value of the reaction system is 7.5, and ending the carbonation reaction to obtain cubic precipitated calcium carbonate suspension;
s4, mixing the rod-shaped precipitated calcium carbonate suspension obtained in the step S2 and the cubic precipitated calcium carbonate suspension obtained in the step S3 according to the mass ratio of 1:4, mixing, adding the behenic acid with the dry mass of 0.6% of calcium carbonate, uniformly mixing, heating to 90 ℃ and maintaining for 1.0 hour to obtain a cubic dispersion precipitated calcium carbonate suspension with the size;
s5, carrying out surface treatment on the precipitated calcium carbonate suspension by using stearic acid saponification liquid with the mass of 3.3% of the dry weight of calcium carbonate, carrying out filter pressing, drying and sieving to obtain the cubic dispersed precipitated calcium carbonate powder with the size.
Comparative example 1
S1, slaking quicklime, sieving, refining and preparing lime slurry with the specific gravity of 1.050, and aging for 12 hours for later use;
s2, controlling the temperature of lime slurry at 20 ℃, and introducing carbon dioxide mixed gas with the concentration of 30% at 3.0m3/h until the pH value of a reaction system is 7.5, stopping ventilation, and ending the carbonation reaction to obtain cubic precipitated calcium carbonate suspension;
s3, mixing the cubic precipitated calcium carbonate suspension obtained in the step S2 with heavy calcium carbonate according to a mass ratio of 6:4, mixing.
S4: and (3) carrying out surface treatment on the precipitated calcium carbonate suspension by using 3.5% stearic acid saponification liquid, carrying out filter pressing, drying and sieving to obtain cubic precipitated calcium carbonate powder.
Comparative example 2
S1, slaking quicklime, sieving, refining and preparing lime slurry with the specific gravity of 1.040, and aging for 12 hours for later use;
s2, controlling the temperature of lime slurry at 20 ℃, and introducing carbon dioxide mixed gas with the concentration of 33% at 2.0m3/h until the pH value of a reaction system is 7.5, stopping ventilation, and ending the carbonation reaction to obtain cubic precipitated calcium carbonate suspension;
s3: and (3) carrying out surface treatment on the precipitated calcium carbonate suspension by using 3.5% stearic acid saponification liquid, carrying out filter pressing, drying and sieving to obtain cubic precipitated calcium carbonate powder.
The precipitated calcium carbonate obtained in the above examples and comparative examples was prepared into silicone sealants according to the formulations shown in table 1 according to conventional methods. The mechanical property test and the storage property test are carried out on the sealant according to the standard GB/T13477-2017, and the test results are shown in Table 2.
Table 1: the precipitated calcium carbonate prepared by the invention is applied to PVC product formula
| Raw materials | Parts by mass (portions) |
| 2w107 resin | 35 |
| 8w107 resin | 45 |
| Filler (precipitated calcium carbonate) | 100 |
| 100cP silicone oil | 5 |
| D20 | 2 |
| KH550 | 0.3 |
| KH560 | 3 |
| D80 | 0.06 |
Table 2: performance test results of the precipitated calcium carbonate applied to silicone sealant
As shown in Table 2, the large and small cubic dispersion precipitated calcium carbonate prepared by the method has an excellent reinforcing effect when being filled in silicone sealant, and compared with the sealant with heavy calcium carbonate as the filler, the sealant after filling has the advantages of higher viscosity, higher strength, obviously better fluidity, better flowability and better storage property.
The foregoing is a further detailed description of the invention in connection with specific/preferred embodiments, and is not intended to limit the practice of the invention to such description. It will be apparent to those skilled in the art that several alternatives or modifications can be made to the described embodiments without departing from the spirit of the invention, and these alternatives or modifications should be considered to be within the scope of the invention.
Claims (6)
1. A preparation method of cubic dispersed precipitated calcium carbonate is characterized in that: the method comprises the following steps:
s1, slaking quicklime, sieving, refining and preparing lime slurry with the specific gravity of 1.040-1.050, and aging for 12-24 hours for later use;
s2, adding a crystal form control agent into the lime slurry, wherein the crystal form control agent is compounded by sodium hexametaphosphate or sodium pyrophosphate and soluble barium salt, introducing carbon dioxide mixed gas into the lime slurry, stopping ventilation when the pH value of a reaction system is 8.0, and ending the carbonation reaction to obtain a rod-shaped precipitated calcium carbonate suspension;
s3, adding a crystal form control agent into the lime slurry, wherein the crystal form control agent is one or more of sodium dodecyl sulfate, dodecyl trimethyl betaine and sodium polystyrene sulfonate; introducing carbon dioxide mixed gas into lime slurry, stopping ventilation when the pH value of a reaction system is 7.5, and ending carbonation reaction to obtain cubic precipitated calcium carbonate suspension;
s4, mixing the rod-shaped precipitated calcium carbonate suspension obtained in the step S2 and the cubic precipitated calcium carbonate suspension obtained in the step S3 in proportion, adding behenic acid, uniformly mixing, heating to 90-95 ℃ and maintaining for 1.0 hour to obtain a large-small cubic dispersed precipitated calcium carbonate suspension;
s5, carrying out surface treatment on the precipitated calcium carbonate suspension through stearic acid saponification liquid, carrying out pressure filtration, drying and sieving to obtain cubic dispersed precipitated calcium carbonate powder;
the addition amount of the crystal form control agent in the step S2 is 0.3-1.5% of the dry content of calcium hydroxide;
in the step S2, the mass ratio of the sodium hexametaphosphate or the sodium pyrophosphate to the soluble barium salt is 4-10:1;
the addition amount of the crystal form control agent in the step S3 is 0.1-0.4% of the dry content of calcium hydroxide;
the mass ratio of the rod-shaped precipitated calcium carbonate suspension to the cubic precipitated calcium carbonate suspension is 1:1-10.
2. The method for preparing the cubic dispersed and precipitated calcium carbonate according to claim 1, wherein the method comprises the following steps: the soluble barium salt is barium chloride or/and barium nitrate.
3. The method for preparing the cubic dispersed and precipitated calcium carbonate according to claim 1, wherein the method comprises the following steps: and (2) controlling the carbonization temperature of lime slurry at 45.0-55.0 ℃ in the initial carbonization reaction of the step (S2), the concentration of the carbon dioxide mixed gas at 15-18%, and the air inlet flow rate at 2.0-3.0m < 3 >/h.
4. The method for preparing the cubic dispersed and precipitated calcium carbonate according to claim 1, wherein the method comprises the following steps: the carbonation reaction in the step S3 controls the initial carbonation temperature of lime slurry to be 18.0-23.0 ℃, the concentration of carbon dioxide mixed gas to be 30-33% and the air inlet flow to be 2.0-3.0m 3 /h。
5. The method for preparing the cubic dispersed and precipitated calcium carbonate according to claim 1, wherein the method comprises the following steps: the consumption of the behenic acid is 0.5-0.8% of the dry mass of the calcium carbonate; the dosage of the stearic acid saponification liquid is 3.0-3.5% of the dry mass of calcium carbonate.
6. The method for preparing the cubic dispersed and precipitated calcium carbonate according to claim 1, wherein the method comprises the following steps: the surface treatment in the step S5 is carried out for 30-60min under the temperature of 90-95 ℃ and the rotating speed of 2500-3000 r/min.
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| JPH0431316A (en) * | 1990-05-28 | 1992-02-03 | Maruo Calcium Co Ltd | Monodispersed plate calcium carbonate and production thereof |
| CN106517285A (en) * | 2016-11-21 | 2017-03-22 | 广西华纳新材料科技有限公司 | Method for preparing bar-shaped nanometer calcium carbonate |
| CN109810294A (en) * | 2019-01-07 | 2019-05-28 | 卢氏国嵩莱纳米科技有限公司 | A kind of preparation method of the high-end nanometer calcium carbonate of butyl rubber product |
| WO2020010689A1 (en) * | 2018-07-12 | 2020-01-16 | 广西华纳新材料科技有限公司 | Preparation method for nanoprecipitated calcium carbonate having core-shell structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0431316A (en) * | 1990-05-28 | 1992-02-03 | Maruo Calcium Co Ltd | Monodispersed plate calcium carbonate and production thereof |
| CN106517285A (en) * | 2016-11-21 | 2017-03-22 | 广西华纳新材料科技有限公司 | Method for preparing bar-shaped nanometer calcium carbonate |
| WO2020010689A1 (en) * | 2018-07-12 | 2020-01-16 | 广西华纳新材料科技有限公司 | Preparation method for nanoprecipitated calcium carbonate having core-shell structure |
| CN109810294A (en) * | 2019-01-07 | 2019-05-28 | 卢氏国嵩莱纳米科技有限公司 | A kind of preparation method of the high-end nanometer calcium carbonate of butyl rubber product |
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