CN104261450B - A kind of synthetic method of amorphous cium carbonate nanoparticles of size tunable - Google Patents
A kind of synthetic method of amorphous cium carbonate nanoparticles of size tunable Download PDFInfo
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- CN104261450B CN104261450B CN201410537788.XA CN201410537788A CN104261450B CN 104261450 B CN104261450 B CN 104261450B CN 201410537788 A CN201410537788 A CN 201410537788A CN 104261450 B CN104261450 B CN 104261450B
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- C—CHEMISTRY; METALLURGY
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- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to the noncrystal cium carbonate nanoparticles of a kind of single dispersing, described nano particle has the uniform particle size in the scope of 10 to 300nm.The invention still further relates to a kind of method preparing the noncrystal cium carbonate nanoparticles of single dispersing, said method comprising the steps of: a. prepares the ethanolic soln A of calcium chloride; B. in solution A, add water, obtain reaction solution B; C. reaction solution B is placed in container C and sealed container port, and reserves aperture on sealed membrane; D. bicarbonate of ammonia solid to be loaded in container D and to seal bottleneck, and on sealed membrane reserved aperture; E. container C and container D are jointly inserted in the moisture eliminator of sealing and leave standstill, the liquid in container C becomes suspension E; F. suspension E centrifugation is obtained amorphous cium carbonate nanoparticles.
Description
Technical field
The present invention relates to nano material synthetic technology, especially a kind of preparation method of single dispersing amorphous cium carbonate nanoparticles of size tunable.
Background technology
Calcium carbonate is a kind of natural mineral being prevalent in occurring in nature, has good biocompatibility and biological safety, and component is simple, with low cost, is easy to the advantages such as extensive preparation.Amorphous calcium carbonate, as the one of calcium carbonate existence form, is the precursor that calcium carbonate crystal changes crystal phase into.Relative to the calcium carbonate crystal of micro-meter scale, owing to not possessing specific crystalline network, amorphous calcium carbonate is easier to the material preparing nanoscale.At present, as a kind of base mateiral of excellence, amorphous calcium carbonate nano material is extensively included in numerous applied research, the physical strength enhancement component during biological example is bionical, battery separator, bone tissue restoration support and medicine/gene carrier etc.Therefore, for meeting the demand of different field, the preparation of the amorphous calcium carbonate nano material of size tunable becomes the emphasis in current study on the synthesis.The difficult problem that but due to the thermodynamic phase of amorphous calcium carbonate self, extensive synthesis preparation is stable, single dispersing and the controlled amorphous calcium carbonate nano material of uniform particle diameter are still research at present.
" Material Physics and chemistry " (MaterialsChemistryandPhysics) reports 93 phase in 2005 376 pages and in ethanolic soln, forms precipitation of calcium carbonate by calcium chloride and volatile salt reaction and obtain the method for amorphous cium carbonate nanoparticles by slow heating.This method technique is comparatively complicated, and the amorphous calcium carbonate obtained is difficult to dispersion, particle diameter heterogeneity.
" JACS " (JournaloftheAmericanChemicalSociety) reports 132 phase in 2010 17859 pages and carry out the stable method preparing amorphous calcium carbonate nano material to amorphous calcium carbonate surface by coated with silica in basic solution.But the nanoparticulate dispersed that the method prepares and homogeneity poor.
" chemical communication " (Chemicalcommunications) reports by air plllutant method 49 phase in 2013 9564 pages, the monodispersed amorphous cium carbonate nanoparticles of synthesizing stable in ethanol.Equally, the amorphous cium carbonate nanoparticles uniform particle diameter that this kind of method obtains is poor, does not have particle diameter Modulatory character.
Summary of the invention
One aspect of the present invention provides single dispersing noncrystal cium carbonate nanoparticles, and described nano particle has at 10 to 300nm, preferably 30 to 200nm, more preferred 30 to 150nm, the uniform particle size in the scope of most preferably 70 to 120nm.
Another aspect of the present invention provides a kind of method preparing the noncrystal cium carbonate nanoparticles of single dispersing, said method comprising the steps of:
A. the ethanolic soln A of calcium chloride is prepared;
B. in solution A, add water, obtain reaction solution B;
C. reaction solution B is placed in container C and sealed container port, and reserves aperture on sealed membrane;
D. bicarbonate of ammonia solid to be loaded in container D and to seal bottleneck, and on sealed membrane reserved aperture;
E. container C and container D are jointly inserted in the moisture eliminator of sealing and leave standstill, the liquid in container C becomes suspension E;
F. suspension E centrifugation is obtained amorphous cium carbonate nanoparticles.
In one embodiment of the invention, the concentration of the ethanolic soln A of described calcium chloride is 0.25g/l to 8g/l, preferred 0.5g/l to 2g/l, more preferred 1g/l to 2g/l, most preferably 2g/l.
In one embodiment of the invention, in reaction solution B, the volume ratio of ethanol and water is 400: 1 to 50: 1, preferably 400: 3 to 200: 3, more preferably 400: 3 to 100: 1, most preferably 100: 1.
In one embodiment of the invention, the volume of container C is 50ml to 150ml, preferred 50ml to 120ml, more preferred 80ml to 120ml, most preferably 120ml.
In one embodiment of the invention, the volume of container D is 10ml to 40ml, preferred 10ml to 30ml, more preferred 20ml to 30ml, most preferably 20ml.
In one embodiment of the invention, the time of repose in described moisture eliminator is 6h to 48h, preferred 12h to 36h, more preferred 12h to 24h, most preferably 24h.
In one embodiment of the invention, the temperature in moisture eliminator is 20 DEG C to 50 DEG C, preferably 20 DEG C to 40 DEG C, more preferably 20 DEG C to 30 DEG C, most preferably 30 DEG C.
In one embodiment of the invention, the method preparing the noncrystal cium carbonate nanoparticles of single dispersing also comprises the amorphous cium carbonate nanoparticles absolute ethanol washing will obtained from suspension E centrifugation.
Another aspect of the present invention relates to the noncrystal cium carbonate nanoparticles of a kind of single dispersing, and the noncrystal cium carbonate nanoparticles of described single dispersing is according to the method preparation preparing the noncrystal cium carbonate nanoparticles of single dispersing of the present invention.
Accompanying drawing explanation
Fig. 1 is the X-ray electron diffraction collection of illustrative plates of the amorphous cium carbonate nanoparticles of preparation in embodiment 1.In FIG, X-coordinate is rotational angle 2 θ (°), and ordinate zou is diffracted intensity (a.u.).
Fig. 2 is transmission electron microscope (TEM) photo of the amorphous cium carbonate nanoparticles of preparation in embodiment 1.
Fig. 3 is transmission electron microscope (TEM) photo of the amorphous cium carbonate nanoparticles of preparation in embodiment 2.
Fig. 4 is transmission electron microscope (TEM) photo of the amorphous cium carbonate nanoparticles of preparation in embodiment 3.
Fig. 5 is transmission electron microscope (TEM) photo of the amorphous cium carbonate nanoparticles of preparation in embodiment 4.
Embodiment
A specific embodiment of the present invention provides that a kind of method is simple, mild condition, can be used for the preparation method of the amorphous cium carbonate nanoparticles of grain-size.
A specific embodiment of the present invention is by the regulatable amorphous cium carbonate nanoparticles of gas phase diffusion reaction a kind of uniform particle diameter of preparation.The carbon dioxide solubility volatilized by bicarbonate of ammonia is in the ethanolic soln of calcium chloride, and synthesis obtains cium carbonate nanoparticles.
Demonstrate the characteristic spectrum of amorphous in X ray diffracting spectrum, there is no the diffractive features peak of crystal, prove that this kind of cium carbonate nanoparticles exists with noncrystalline state.
The preparation method for amorphous cium carbonate nanoparticles of a specific embodiment of the present invention is as follows:
1) 0.025 ~ 0.8g CALCIUM CHLORIDE DIHYDRATE is added in 100ml dehydrated alcohol, after dissolving completely, obtain the ethanolic soln A of calcium chloride;
2) in solution A, add 0.25 ~ 2.0ml water, after mixing, obtain reaction solution B;
3) reaction solution B is placed in the glass jar of 50 ~ 150ml, with sealed membrane sealing bottleneck, and reserves aperture on sealed membrane, obtain reactor C;
4) bicarbonate of ammonia solid is loaded in the glass jar of 10 ~ 40ml, with sealed membrane sealing bottleneck, and reserve aperture on sealed membrane, obtain reactor D;
5) jointly inserted in the moisture eliminator of sealing by reactor C and reactor D, 20 ~ 50 DEG C of constant temperature leave standstill 6-48 hour, and the liquid rotating in reactor C becomes suspension E;
6) by suspension E centrifugation, collect white precipitate and with absolute ethanol washing, obtain amorphous cium carbonate nanoparticles, be kept in dehydrated alcohol.
The amorphous cium carbonate nanoparticles size tunable prepared in a specific embodiment of the present invention, respectively at 135nm, 86nm, 56nm and 38nm.In the sample of often kind of particle diameter, amorphous cium carbonate nanoparticles all has monodispersity, uniform particle diameter and can steady in a long-termly preserve in ethanol.This kind of synthetic method step is simple, with low cost, mild condition, be easy to manipulation.And do not relate to any additive in reaction, the amorphous calcium carbonate grain fraction finally obtained is simple, friendly to environmental and biological materials, poisons low, possesses the application prospect in more wide multiple fields.
Below in conjunction with specific embodiment, specific description is done to the present invention.
Embodiment
Embodiment 1
0.2g CALCIUM CHLORIDE DIHYDRATE is added in 100ml dehydrated alcohol, after dissolving completely, add 1ml water.Aforesaid liquid is placed in the glass jar of 150ml, with sealed membrane sealing bottleneck, and reserves aperture on sealed membrane.Bicarbonate of ammonia solid is loaded in the glass jar of 20ml, with sealed membrane sealing bottleneck, and reserve aperture on sealed membrane.Jointly inserted in the moisture eliminator of sealing by above-mentioned two kinds of reactors, 30 DEG C of constant temperature leave standstill 24 hours, obtain translucent white liquid.This centrifugal is separated (8,000rpm, 10 minutes), collects white precipitate and with absolute ethanol washing, obtain amorphous cium carbonate nanoparticles, be kept in dehydrated alcohol.Characterize with X ray diffracting spectrum, as shown in Figure 1, in collection of illustrative plates, demonstrate the characteristic spectrum of amorphous, there is no the characteristic diffraction peak of crystal, prove the amorphous existing forms of this kind of cium carbonate nanoparticles.As shown in Figure 2, particle diameter is 135nm to the pattern of this kind of nano particle, and grain diameter is homogeneous, becomes monodisperse status.
Embodiment 2
0.1g CALCIUM CHLORIDE DIHYDRATE is added in 100ml dehydrated alcohol, after dissolving completely, add 1ml water.Aforesaid liquid is placed in the glass jar of 150ml, with sealed membrane sealing bottleneck, and reserves aperture on sealed membrane.Bicarbonate of ammonia solid is loaded in the glass jar of 20ml, with sealed membrane sealing bottleneck, and reserve aperture on sealed membrane.Jointly inserted in the moisture eliminator of sealing by above-mentioned two kinds of reactors, 30 DEG C of constant temperature leave standstill 24 hours, obtain translucent white liquid.This centrifugal is separated (10,000rpm, 10 minutes), collects white precipitate and with absolute ethanol washing, obtain amorphous cium carbonate nanoparticles, be kept in dehydrated alcohol.As shown in Figure 3, particle diameter is 86nm to the pattern of this kind of nano particle, and grain diameter is homogeneous, becomes monodisperse status.
Embodiment 3
0.05g CALCIUM CHLORIDE DIHYDRATE is added in 100ml dehydrated alcohol, after dissolving completely, add 0.75ml water.Aforesaid liquid is placed in the glass jar of 150ml, with sealed membrane sealing bottleneck, and reserves aperture on sealed membrane.Bicarbonate of ammonia solid is loaded in the glass jar of 20ml, with sealed membrane sealing bottleneck, and reserve aperture on sealed membrane.Jointly inserted in the moisture eliminator of sealing by above-mentioned two kinds of reactors, 30 DEG C of constant temperature leave standstill 24 hours, obtain translucent white liquid.This centrifugal is separated (12,000rpm, 10 minutes), collects white precipitate and with absolute ethanol washing, obtain amorphous cium carbonate nanoparticles, be kept in dehydrated alcohol.As shown in Figure 4, particle diameter is 56nm to the pattern of this kind of nano particle, and grain diameter is homogeneous, becomes monodisperse status.
Embodiment 4
0.025g CALCIUM CHLORIDE DIHYDRATE is added in 100ml dehydrated alcohol, after dissolving completely, add 0.75ml water.Aforesaid liquid is placed in the glass jar of 150ml, with sealed membrane sealing bottleneck, and reserves aperture on sealed membrane.Bicarbonate of ammonia solid is loaded in the glass jar of 20ml, with sealed membrane sealing bottleneck, and reserve aperture on sealed membrane.Jointly inserted in the moisture eliminator of sealing by above-mentioned two kinds of reactors, 30 DEG C of constant temperature leave standstill 24 hours, obtain translucent white liquid.This centrifugal is separated (14,000rpm, 30 minutes), collects white precipitate and with absolute ethanol washing, obtain amorphous cium carbonate nanoparticles, be kept in dehydrated alcohol.As shown in Figure 5, particle diameter is 38nm to the pattern of this kind of nano particle, and grain diameter is homogeneous, becomes monodisperse status.
Claims (9)
1. prepare a method for the noncrystal cium carbonate nanoparticles of single dispersing, said method comprising the steps of:
A. the ethanolic soln A of calcium chloride is prepared;
B. in solution A, add water, obtain reaction solution B;
C. reaction solution B is placed in container C and sealed container port, and reserves aperture on sealed membrane;
D. bicarbonate of ammonia solid to be loaded in container D and to seal bottleneck, and on sealed membrane reserved aperture;
E. container C and container D are jointly inserted in the moisture eliminator of sealing and leave standstill, the liquid in container C becomes suspension E;
F. suspension E centrifugation is obtained amorphous cium carbonate nanoparticles.
2. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, the concentration of the ethanolic soln A of wherein said calcium chloride is 0.25g/L to 8g/L.
3. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, in wherein said reaction solution B, the volume ratio of ethanol and water is 400: 1 to 50: 1.
4. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, the volume of wherein said container C is 50mL to 150mL.
5. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, the volume of wherein said container D is 10mL to 40mL.
6. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, the time of repose wherein in described moisture eliminator is 6h to 48h.
7. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, the temperature in wherein said moisture eliminator is 20 to 50 DEG C.
8. the method preparing the noncrystal cium carbonate nanoparticles of single dispersing according to claim 1, the amorphous cium carbonate nanoparticles absolute ethanol washing wherein will obtained from suspension E centrifugation.
9. the noncrystal cium carbonate nanoparticles of single dispersing, the method preparation of the noncrystal cium carbonate nanoparticles of described single dispersing according to any one in claim 1-8.
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| CN111377473A (en) * | 2018-12-27 | 2020-07-07 | 上海元颉新材料科技有限公司 | Monodisperse bionic pollen-shaped calcium carbonate nano material with porous polycrystalline structure and preparation method thereof |
| CN109771379A (en) * | 2019-03-06 | 2019-05-21 | 常州大学 | A kind of calcium carbonate solid dispersion of curcumin and preparation method thereof |
| CN112458534B (en) * | 2020-10-15 | 2022-05-13 | 中国科学技术大学 | Magnesium calcite mesoscopic crystal and preparation method of magnesium calcite crystal with adjustable morphology |
| CN113350510B (en) * | 2021-05-11 | 2022-05-17 | 内蒙古工业大学 | Amorphous nano calcium carbonate capable of stably existing and preparation method and application thereof |
| CN115025109A (en) * | 2022-06-28 | 2022-09-09 | 南通大学 | Gemcitabine and Triapine-encapsulated calcium carbonate nanoparticles |
| CN114988452A (en) * | 2022-07-25 | 2022-09-02 | 宁远华创粉体材料有限公司 | Production method of calcium carbonate for food |
| CN116350791A (en) * | 2023-03-13 | 2023-06-30 | 清华大学 | Universal preparation method for increasing drug loading rate by using ACC-entrapped metal ions |
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