CN102583482B - Preparation method of flake-shaped aragonite calcium carbonate - Google Patents
Preparation method of flake-shaped aragonite calcium carbonate Download PDFInfo
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- CN102583482B CN102583482B CN201210032142.7A CN201210032142A CN102583482B CN 102583482 B CN102583482 B CN 102583482B CN 201210032142 A CN201210032142 A CN 201210032142A CN 102583482 B CN102583482 B CN 102583482B
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- calcium carbonate
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- shaped aragonite
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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 175
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001238 wet grinding Methods 0.000 claims abstract description 11
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006210 lotion Substances 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 238000009775 high-speed stirring Methods 0.000 claims description 10
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 10
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 10
- 210000000434 stratum corneum Anatomy 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 241000237536 Mytilus edulis Species 0.000 claims description 9
- 235000020638 mussel Nutrition 0.000 claims description 8
- 241000237502 Ostreidae Species 0.000 claims description 5
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 5
- 239000004310 lactic acid Substances 0.000 claims description 5
- 235000014655 lactic acid Nutrition 0.000 claims description 5
- 235000020636 oyster Nutrition 0.000 claims description 5
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims description 5
- 239000004584 polyacrylic acid Substances 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 241000237509 Patinopecten sp. Species 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 239000013505 freshwater Substances 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- 235000020637 scallop Nutrition 0.000 claims description 4
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 4
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000004566 building material Substances 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 abstract description 2
- -1 papermaking Polymers 0.000 abstract description 2
- 229920003023 plastic Polymers 0.000 abstract description 2
- 239000004033 plastic Substances 0.000 abstract description 2
- 239000005060 rubber Substances 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 239000000976 ink Substances 0.000 abstract 1
- 231100000614 poison Toxicity 0.000 abstract 1
- 230000007096 poisonous effect Effects 0.000 abstract 1
- 239000002002 slurry Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000001000 micrograph Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940058344 antitrematodals organophosphorous compound Drugs 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000003278 mimic effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The invention discloses a preparation method of flake-shaped aragonite calcium carbonate. The preparation method comprises the following steps: (1) performing dry method coarse grinding to a shell raw material, soaking the shell raw material in lotion for 4-48h at normal temperature, utilizing roller watering to remove a cuticle layer and a prismatic layer, and obtaining nacreous layer calcium carbonate by washing; (2) adding water to the nacreous layer calcium carbonate, performing high-speed agitation to prepare slurry with the concentration to be 30-80wt%, adding a grinding aid with the weight being 0.5-5% that of the nacreous layer calcium carbonate, and using a stripping machine to perform wet grinding for 60-180min with zirconia ball, alumina balls or ceramic balls serving as grinding mediums; and (3) performing filter pressing and drying grinding to obtain the flake-shaped aragonite calcium carbonate. The preparation method of the flake-shaped aragonite calcium carbonate is simple in process and does not use a poisonous harmful reagent, the operation conditions are mild, the surface activity of the prepared flake-shaped aragonite calcium carbonate is good, and the flake-shaped aragonite calcium carbonate can be widely applied to industries such as plastics, papermaking, rubber, ink, coating, building materials, medicines and food.
Description
Technical field
The present invention relates to shell and utilize field, particularly a kind of preparation method of flake-shaped aragonite calcium carbonate.
Background technology
Flaky calcium carbonate has that whiteness is high, slickness is high, glossiness advantages of higher.At present, the method of preparing flaky calcium carbonate mainly contains microemulsion method, conversion method and milk of lime carborization, general organo phosphorous compounds, boride, organic amine or the organic acids etc. of adopting are done morphology control agent, morphology control agent is expensive, toxicity is large, has secondary pollution, complex process, the problems such as speed of response is slow, and yield rate is low.
On the other hand, aragonite calcium carbonate is a kind of type material occurring in recent years, has that intensity is high, modulus is high, a feature such as heat-resisting and heat-proof quality is good.Aragonite calcium carbonate and matrix have good consistency, can improve processing characteristics and the mechanical property of goods, give surface smoothness and wear resistance that goods are high.At present, while utilizing aragonite forming process in bionics mimic biology body to prepare aragonite crystals, adopt the replacement(metathesis)reaction of solubility salt, main method has Ca (HCO more
3)
2conversion method, urea water solution and MgCl
2method etc., it is low that these methods are prepared aragonite productive rate, and most of calcium carbonate configuration is to take calcite as main, and raw materials cost is high simultaneously, and process energy consumption is larger, and processing condition are difficult to control, and are difficult to realize suitability for industrialized production.And the aragonite goods of synthetic are mostly needle-like or rhabdolith, synthetic aragonite flaky calcium carbonate has no report.
Shell is the masterpiece of biomineralization, the composite minerals being formed by calcium carbonate and biomacromolecule, because calcium carbonate crystal deposits in order at shell pearl layer, form multilevel ordered nano-superstructure, aragonite plate is the basic comprising unit of nacreous layer, it between lamella, is organic substrate, flake-shaped aragonite calcium carbonate is that the form with aragonite stack of slabs exists, rather than exist with the form of single sheet, by the layering of peeling off to shell pearl layer, it is divided into comparatively single laminar, thereby obtain flake-shaped aragonite calcium carbonate.
As mentioned above, the preparation method of the flake-shaped aragonite calcium carbonate part that still comes with some shortcomings, the invention provides a kind of method that adopts shell to prepare flake-shaped aragonite calcium carbonate.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of flake-shaped aragonite calcium carbonate is provided.
The preparation method's of flake-shaped aragonite calcium carbonate step is as follows:
1) by the coarse reduction of shell dry method, under normal temperature, in washing lotion, soak 4～48 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate is added to water high-speed stirring and make the slip that mass percent concentration is 30～80 %, the grinding aid that adds 0.5～5 % that is equivalent to nacreous layer weight of calcium carbonate, with machine for cutting charge into pieces, take zirconia ball, alumina balls or Ceramic Balls as grinding medium, wet grinding 60～180 minutes;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Described shell is mussel shell, scallop shell, oyster shells, pearl shell or freshwater mussel shell.Described washing lotion is dilute hydrochloric acid, dilute sulphuric acid, dilute acetic acid, rare lactic acid, diluted sodium hydroxide solution or liquor sodii hypochloritis dilutus.Described grinding aid is polyacrylic acid, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, water glass, stearic acid or its mixture.
Operational condition of the present invention is gentle, and raw material sources are wide, and technique is simple, and facility investment and energy consumption are little; The flake-shaped aragonite calcium carbonate good surface activity of preparation, can be widely used in the industries such as plastics, papermaking, rubber, coating, chemical building material, medicine, food, feed, ink, has good economic and social benefit.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of embodiment 1;
Fig. 2 is the electron-microscope scanning figure of embodiment 1;
Fig. 3 is the electron-microscope scanning figure of embodiment 2;
Fig. 4 is the electron-microscope scanning figure of embodiment 3;
Fig. 5 is the microphotograph (amplifying 400 times) of embodiment 4;
Fig. 6 is the microphotograph (amplifying 400 times) of embodiment 5;
Fig. 7 is the lens scan figure of embodiment 6;
Fig. 8 is the lens scan figure of embodiment 7.
Embodiment
The preparation method's of flake-shaped aragonite calcium carbonate step is as follows:
1) by the coarse reduction of shell dry method, under normal temperature, in washing lotion, soak 4～48 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate is added to water high-speed stirring and make the slip that mass percent concentration is 30～80 %, the grinding aid that adds 0.5～5 % that is equivalent to nacreous layer weight of calcium carbonate, with machine for cutting charge into pieces, take zirconia ball, alumina balls or Ceramic Balls as grinding medium, wet grinding 60～180 minutes;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Described shell is mussel shell, scallop shell, oyster shells, pearl shell or freshwater mussel shell.Described washing lotion is dilute hydrochloric acid, dilute sulphuric acid, dilute acetic acid, rare lactic acid, diluted sodium hydroxide solution or liquor sodii hypochloritis dilutus.Described grinding aid is polyacrylic acid, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, water glass, stearic acid or its mixture.
The present invention is further described in conjunction with following instance, but content of the present invention is not limited only to content related in embodiment.
Embodiment 1:
1) by the coarse reduction of Mytilus edulis shell dry method, under normal temperature, in being the dilute hydrochloric acid of 0.1 %, concentration soaks 4 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 30 wt% slips, adds the polyacrylic acid of 0.5 % that is equivalent to nacreous layer weight of calcium carbonate, take zirconia ball as grinding medium, wet grinding 60 minutes with machine for cutting charge into pieces;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Sample XRD figure is shown in accompanying drawing 1, and electron-microscope scanning is shown in accompanying drawing 2.
Embodiment 2:
1) by the coarse reduction of scallop shell dry method, under normal temperature, in being the chlorine bleach liquor of 3 %, concentration soaks 48 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 80 wt% slips, adds the water glass that is equivalent to nacreous layer weight of calcium carbonate 5 %, take alumina balls as grinding medium, wet grinding 180 minutes with machine for cutting charge into pieces;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Sample electron-microscope scanning is shown in accompanying drawing 3.
Embodiment 3:
1) by the coarse reduction of oyster shells dry method, under normal temperature, in being the sodium hydroxide solution of 5 %, concentration soaks 36 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 70 wt% slips, adds the Sodium hexametaphosphate 99 that is equivalent to nacreous layer weight of calcium carbonate 4 %, take Ceramic Balls as grinding medium, wet grinding 180 minutes with machine for cutting charge into pieces;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Sample electron-microscope scanning is shown in accompanying drawing 4.
Embodiment 4:
1) by the coarse reduction of pearl shell dry method, under normal temperature, in being the lactic acid solution of 1 %, concentration soaks 24 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 60 wt% slips, adds the tripoly phosphate sodium STPP that is equivalent to nacreous layer weight of calcium carbonate 2 %, with machine for cutting charge into pieces, take alumina balls as grinding medium, with machine for cutting charge into pieces wet grinding 120 minutes;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Sample microphotograph (amplifying 400 times) is shown in accompanying drawing 5.
Embodiment 5:
1) by the coarse reduction of freshwater mussel shell dry method, under normal temperature, in being the lactic acid solution of 1 %, concentration soaks 36 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 50 wt% slips, adds the tripoly phosphate sodium STPP that is equivalent to nacreous layer weight of calcium carbonate 1 %, take Ceramic Balls as grinding medium, wet grinding 80 minutes with machine for cutting charge into pieces;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Sample microphotograph (amplifying 400 times) is shown in accompanying drawing 6.
Embodiment 6:
1) by the coarse reduction of oyster shells dry method, under normal temperature, in being the acetum of 1 %, concentration soaks 40 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 50 wt% slips, adds the polyacrylic acid that is equivalent to nacreous layer weight of calcium carbonate 3 %, take alumina balls as grinding medium, wet grinding 180 minutes with machine for cutting charge into pieces;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Accompanying drawing 7 is shown in sample lens scanning.
Embodiment 7:
1) by the coarse reduction of mussel shell dry method, under normal temperature, in the acetum of 1 %, soak 36 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate being added to water high-speed stirring, to make concentration be 50 wt% slips, adds the stearic acid that is equivalent to nacreous layer weight of calcium carbonate 2 %, take zirconia ball as grinding medium, wet grinding 120 minutes with machine for cutting charge into pieces;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate.
Accompanying drawing 8 is shown in sample lens scanning.
Claims (3)
1. a preparation method for flake-shaped aragonite calcium carbonate, is characterized in that its step is as follows:
1) by the coarse reduction of shell dry method, under normal temperature, in washing lotion, soak 4～48 hours, with cylinder washing, remove stratum corneum and prismatic layer, wash to obtain nacreous layer calcium carbonate;
2) nacreous layer calcium carbonate is added to water high-speed stirring and make the slip that mass percent concentration is 30～80 %, the grinding aid that adds 0.5～5 % that is equivalent to nacreous layer weight of calcium carbonate, with machine for cutting charge into pieces, take zirconia ball, alumina balls or Ceramic Balls as grinding medium, wet grinding 60～180 minutes;
3) press filtration, drying and crushing obtain flake-shaped aragonite calcium carbonate; Described shell is mussel shell, scallop shell, oyster shells, pearl shell or freshwater mussel shell.
2. the preparation method of a kind of flake-shaped aragonite calcium carbonate as claimed in claim 1, is characterized in that described washing lotion is dilute hydrochloric acid, dilute sulphuric acid, dilute acetic acid, rare lactic acid, diluted sodium hydroxide solution or liquor sodii hypochloritis dilutus.
3. the preparation method of a kind of flake-shaped aragonite calcium carbonate as claimed in claim 1, is characterized in that described grinding aid is polyacrylic acid, Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, water glass, stearic acid or its mixture.
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| CN102583482B true CN102583482B (en) | 2014-03-26 |
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| CN1176758A (en) * | 1996-09-13 | 1998-03-25 | 哈尔滨多元超细粉体工程有限责任公司 | Super fine biological calcium carbonate and process for producing same |
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Cited By (2)
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