CN106145173A - A kind of preparation method of calcium carbonate self-assembled structures - Google Patents
A kind of preparation method of calcium carbonate self-assembled structures Download PDFInfo
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- CN106145173A CN106145173A CN201610489923.7A CN201610489923A CN106145173A CN 106145173 A CN106145173 A CN 106145173A CN 201610489923 A CN201610489923 A CN 201610489923A CN 106145173 A CN106145173 A CN 106145173A
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- calcium carbonate
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- assembled structures
- solution
- glucosan
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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 58
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 229920001503 Glucan Polymers 0.000 claims abstract description 16
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920002674 hyaluronan Polymers 0.000 claims abstract description 15
- 229960003160 hyaluronic acid Drugs 0.000 claims abstract description 15
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 claims abstract description 15
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000010926 purge Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 12
- FYGDTMLNYKFZSV-URKRLVJHSA-N (2s,3r,4s,5s,6r)-2-[(2r,4r,5r,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5r,6s)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1[C@@H](CO)O[C@@H](OC2[C@H](O[C@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-URKRLVJHSA-N 0.000 description 4
- 229920002498 Beta-glucan Polymers 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 241000446313 Lamella Species 0.000 description 3
- 230000033558 biomineral tissue development Effects 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 208000027418 Wounds and injury Diseases 0.000 description 2
- 230000000035 biogenic effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 208000036626 Mental retardation Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides the preparation method of a kind of calcium carbonate self-assembled structures, it is possible to prepare the calcium carbonate self-assembled structures of high complexity, comprise the following steps: 1) calcium fluoride or calcium nitrate are dissolved in water it are configured to Ca2+Concentration is the solution that PH is 4～5 of 0.01～1mol/L；2) adding hyaluronic acid and glucosan, the addition of the acid of bright matter and glucosan is step 1) solution quality 1～5%, stir at 40～50 DEG C to after being completely dissolved, continue stirring 30～60min；3) stopping heating, be cooled to room temperature, take and be placed in right amount in open glass container, the described appropriate finger liquid level height away from container bottom is 10～20mm, to the NH that liquid level wind drift is dynamic3: CO2=1:(0.8～1.2) mixed gas, flow is 0.01～0.1ml/min, react 4～24h；4) filtering, being washed to PH is 6～7；5) alcohol is washed, and dries, grinds.
Description
[technical field]
The present invention relates to biomineralization field, particularly relate to the preparation method of a kind of calcium carbonate self-assembled structures.
[background technology]
In nature, have been found that more than 60 kind of biogenic mineral is active in each quasi-life body, as magnetic is thin up to now
Magnetic crystal in bacterium and the skeleton of mammal and tooth, this inorganic mineral and organic material combinations in vivo exists
Together, build the special life process based on inorganic matter and be referred to as biomineralization.The natural biological produced by this process
Mineral are with calcium, phosphorus, magnesium, silicon, oxygen, carbon, hydrogen, sulfur, manganese and ferrum for mainly comprising element, at pattern, size, degree of crystallinity, homoatomic
The aspect such as isomer and trace constituent is had nothing in common with each other and has the complicated composition of special higher structure.
In numerous biogenic minerals, calcium carbonate is played the part of different with its different crystal structure in different organisms
Functional role, such as the shell being made up of aragonite crystals and organic substrate, it not only has the mechanical property of excellence, and after damaging
Can regenerate at injury region, this has inspired significance to medical science very much.Therefore, the complicated calcium carbonate of new method preparation is developed certainly
Package assembly, it will offer thinking is studied in the regeneration for skeleton and tooth, it is also possible to provides and can be used for giving treatment to skeleton
Material with injury of teeth.
[summary of the invention]
For the problems referred to above of the prior art, the present invention provides the preparation method of a kind of calcium carbonate self-assembled structures, energy
Enough prepare the calcium carbonate self-assembled structures of high complexity.
The technical scheme is that
The preparation method of a kind of calcium carbonate self-assembled structures, it is characterised in that comprise the following steps:
(1) calcium fluoride or calcium nitrate are dissolved in water and are configured to Ca2+Concentration is the solution of 0.01～1mol/L, adds nitric acid by molten
The PH of liquid is adjusted to 4～5；
(2) adding hyaluronic acid and glucosan in the solution of step (1) gained, the addition of described hyaluronic acid is step
Suddenly the 1～5% of (1) solution quality, the addition of described glucosan is the 1～5% of step (1) solution quality, at 40～50 DEG C
Under the conditions of, stir to after being completely dissolved, continue stirring 30～60min；
(3) stop heating, the solution of step (2) gained is cooled to room temperature, takes and be placed in right amount in open glass container, institute
State and refer to that the liquid level height away from container bottom is 10～20mm in right amount, to the NH that liquid level wind drift is dynamic3And CO2Mixed gas, described mixing
The flow of gas is 0.01～0.1ml/min, NH3And CO2Volume ratio be 1:(0.8～1.2), react 4～24h；
(4) being filtered by the mixture of step (3) gained, it is 6～7 that filter cake is washed to PH；
(5) the filter cake alcohol of step (4) gained is washed, dry, grind, obtain final products.
Preferably, the molecular weight of above-mentioned hyaluronic acid is 1,000,000～2,200,000.
Preferably, above-mentioned glucosan is beta glucan.
Preferably, the addition of above-mentioned hyaluronic acid is the 1～3% of step (1) solution quality, the addition of described glucosan
Amount is the 1～3% of step (1) solution quality.
Preferably, the blow-out position distance liquid level 5～10mm of the mixed gas in above-mentioned steps (3).
Preferably, NH in the mixed gas of above-mentioned steps (3)3And CO2Volume ratio be 1:1.
Preferably, the flow of above-mentioned steps (3) mixed gas is 0.01～0.02ml/min.
Preferably, the alcohol of above-mentioned steps (5) is washed as ethanol purge.
Preferably, the drying temperature of above-mentioned steps (5) is 80～90 DEG C.
Preferably, the crystal habit of the said goods is vaterite.
The present invention has a following useful technique effect:
1) present invention is by suitable formula, proportioning and step, uses the bionic process of very mental retardation, prepares and have height
The calcium carbonate self-assembled structures that degree is complicated, the growth behavior of its crystal is by the hyaluronic acid being widely present in cell and glucosan
Induction regulating controlling；Hyaluronic acid contains substantial amounts of hydroxyl and carboxyl, has extremely strong hydrophilic, and to Ca2+Have bigger affine
Power, and there is good viscoelasticity, the raw material in crystallization process can be controlled and migrate and migration rate, and glucosan has solely
Special helical structure, gelling ability and pharmacological property, can form certain grafting with hyaluronic acid synergism, collect two
The advantage of person is that the research of biological mineralization process provides thinking；2) raw material of the present invention is easy to get, and technique is simple, preparation condition temperature
With, post processing is simple, and without any residual, the biocompatibility of material is good；3) can not be steady during the present invention is prepared for natural process
The fixed vaterite crystal habit existed, pattern is regular, and uniformity is good；4) present invention directly can be controlled by duration of ventilation
The growth size of crystal, and again ventilation after can be with continued growth.
[accompanying drawing explanation]
Fig. 1 is the stereoscan photograph of embodiment one.
[detailed description of the invention]
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment provided below also is not used to limit the scope that the present invention is contained, and described step is not to use
To limit its execution sequence.Those skilled in the art combine existing common knowledge and are the present invention conspicuously improved, also fall
Within entering the protection domain of application claims.
Embodiment one
The preparation method of a kind of calcium carbonate self-assembled structures, it is characterised in that comprise the following steps:
(1) calcium fluoride or calcium nitrate are dissolved in water and are configured to Ca2+Concentration is the solution of 0.2mol/L, adds nitric acid by solution
PH be adjusted to 4.5；
(2) in the solution of step (1) gained, hyaluronic acid and the beta glucan that molecular weight is 1,800,000 is added, described
Addition is step (1) solution quality the 3% of bright matter acid, the addition of described glucosan is step (1) solution quality
3%, under the conditions of 45 DEG C, stir to after being completely dissolved, continue stirring 45min；
(3) stop heating, the solution of step (2) gained is cooled to room temperature, takes and be placed in right amount in open glass container, institute
State and refer to that the liquid level height away from container bottom is 15mm in right amount, to the NH that liquid level wind drift is dynamic3And CO2Mixed gas, described mixed gas
Flow be 0.02ml/min, NH3And CO2Volume ratio be 1:1, react 10h；In order to make nucleation, growth close to certainly
Assembling process, the blow-out position distance liquid level 8mm of mixed gas, the flow of mixed gas is 0.02ml/min, the most permissible
Ensure crystalline environment, the biggest disturbance will not be brought to crystallizing system again, the most just can be formed complexity and rule from group
Assembling structure；
(4) being filtered by the mixture of step (3) gained, it is 6～7 that filter cake is washed to PH；
(5) by the filter cake of step (4) gained ethanol purge 3 times, 85 DEG C of drying, grind, obtain final products.
Being detected by XRD, the crystal habit of final products is vaterite, and for cubic system, its pattern is as it is shown in figure 1, be
Lamella assembles the calcium carbonate structure that the complexity formed is orderly.
Embodiment two
The preparation method of a kind of calcium carbonate self-assembled structures, it is characterised in that comprise the following steps:
(1) calcium fluoride or calcium nitrate are dissolved in water and are configured to Ca2+Concentration is the solution of 0.01mol/L, adds nitric acid by solution
PH be adjusted to 4；
(2) in the solution of step (1) gained, hyaluronic acid and the beta glucan that molecular weight is 1,000,000 is added, described
Addition is step (1) solution quality the 1% of bright matter acid, the addition of described glucosan is step (1) solution quality
1%, under the conditions of 40 DEG C, stir to after being completely dissolved, continue stirring 30min；
(3) stop heating, the solution of step (2) gained is cooled to room temperature, takes and be placed in right amount in open glass container, institute
State and refer to that the liquid level height away from container bottom is 10mm in right amount, to the NH that liquid level wind drift is dynamic3And CO2Mixed gas, described mixed gas
Flow be 0.01ml/min, NH3And CO2Volume ratio be 1:0.8, react 4h；In order to make nucleation, growth close to
Self assembling process, the blow-out position distance liquid level 5mm of mixed gas, the flow of mixed gas is 0.01ml/min, the most both may be used
To ensure crystalline environment, the biggest disturbance will not be brought to crystallizing system again, the most just can form complexity and rule oneself
Package assembly；
(4) being filtered by the mixture of step (3) gained, it is 6～7 that filter cake is washed to PH；
(5) by the filter cake of step (4) gained ethanol purge 3 times, 80 DEG C of drying, grind, obtain final products.
Being detected by XRD, final products are the crystal habit that lamella assembles the orderly calcium carbonate structure of the complexity formed, vertical
Side's vaterite.
Embodiment three
The preparation method of a kind of calcium carbonate self-assembled structures, it is characterised in that comprise the following steps:
(1) calcium fluoride or calcium nitrate are dissolved in water and are configured to Ca2+Concentration is the solution of 1mol/L, adds nitric acid by the PH of solution
It is adjusted to 4～5；
(2) in the solution of step (1) gained, hyaluronic acid and the beta glucan that molecular weight is 2,200,000 is added, described
Addition is step (1) solution quality the 5% of bright matter acid, the addition of described glucosan is step (1) solution quality
5%, under the conditions of 50 DEG C, stir to after being completely dissolved, continue stirring 60min；
(3) stop heating, the solution of step (2) gained is cooled to room temperature, takes and be placed in right amount in open glass container, institute
State and refer to that the liquid level height away from container bottom is 20mm in right amount, to the NH that liquid level wind drift is dynamic3And CO2Mixed gas, described mixed gas
Flow be 0.1ml/min, NH3And CO2Volume ratio be 1:1.2, react 24h；In order to make nucleation, growth close to
Self assembling process, the blow-out position distance liquid level 10mm of mixed gas, the flow of mixed gas is 0.1ml/min, the most both may be used
To ensure crystalline environment, the biggest disturbance will not be brought to crystallizing system again, the most just can form complexity and rule oneself
Package assembly；
(4) being filtered by the mixture of step (3) gained, it is 6～7 that filter cake is washed to PH；
(5) by the filter cake of step (4) gained ethanol purge 3 times, 90 DEG C of drying, grind, obtain final products.
Being detected by XRD, final products are the crystal habit that lamella assembles the orderly calcium carbonate structure of the complexity formed, vertical
Side's vaterite.
Claims (10)
1. the preparation method of a calcium carbonate self-assembled structures, it is characterised in that comprise the following steps:
(1) calcium fluoride or calcium nitrate are dissolved in water and are configured to Ca2+Concentration is the solution of 0.01～1mol/L, adds nitric acid by solution
PH is adjusted to 4～5；
(2) adding hyaluronic acid and glucosan in the solution of step (1) gained, the addition of described hyaluronic acid is step
(1) the 1～5% of solution quality, the addition of described glucosan is the 1～5% of step (1) solution quality, at 40～50 DEG C of bars
Under part, stir to after being completely dissolved, continue stirring 30～60min；
(3) stop heating, the solution of step (2) gained is cooled to room temperature, takes and be placed in right amount in open glass container, described suitable
Amount refers to that the liquid level height away from container bottom is 10～20mm, to the NH that liquid level wind drift is dynamic3And CO2Mixed gas, described mixed gas
Flow be 0.01～0.1ml/min, NH3And CO2Volume ratio be 1:0.8～1:1.2, react 4～24h；
(4) being filtered by the mixture of step (3) gained, it is 6～7 that filter cake is washed to PH；
(5) the filter cake alcohol of step (4) gained is washed, dry, grind, obtain final products.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that described hyaluronic acid
Molecular weight is 1,000,000～2,200,000.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that described glucosan be β-
Glucosan.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that described hyaluronic acid
Addition is the 1～3% of step (1) solution quality, and the addition of described glucosan is the 1～3% of step (1) solution quality.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that in described step (3)
Mixed gas blow-out position distance liquid level 5～10mm.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that described step (3)
NH in mixed gas3And CO2Volume ratio be 1:1.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that described step (3) is mixed
The flow closing gas is 0.01～0.02ml/min.
The preparation method of calcium carbonate self-assembled structures the most according to claim 1, it is characterised in that described step (5)
Alcohol is washed as ethanol purge.
The preparation method of calcium carbonate self-assembled structures the most according to claim 8, it is characterised in that described step (5)
Drying temperature is 80～90 DEG C.
10. according to the preparation method of the calcium carbonate self-assembled structures described in any one of claim 1-9, it is characterised in that described
The crystal habit of product is vaterite.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0360427A (en) * | 1989-07-28 | 1991-03-15 | Maruo Calcium Co Ltd | Vaterite type calcium carbonate |
| CN101033075A (en) * | 2007-04-13 | 2007-09-12 | 安徽工业大学 | Method of preparing ultra-fine lightweight calcium carbonate |
| CN101844789A (en) * | 2010-06-18 | 2010-09-29 | 苏州大学 | Method for preparing calcium carbonate microspheres |
-
2016
- 2016-06-24 CN CN201610489923.7A patent/CN106145173B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0360427A (en) * | 1989-07-28 | 1991-03-15 | Maruo Calcium Co Ltd | Vaterite type calcium carbonate |
| CN101033075A (en) * | 2007-04-13 | 2007-09-12 | 安徽工业大学 | Method of preparing ultra-fine lightweight calcium carbonate |
| CN101844789A (en) * | 2010-06-18 | 2010-09-29 | 苏州大学 | Method for preparing calcium carbonate microspheres |
Non-Patent Citations (1)
| Title |
|---|
| 赵丽娜等: "自组装片状纳米碳酸钙的制备及表面改性", 《化工进展》 * |
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