CN104692439A - Vaterite calcium carbonate microspheres and preparation method thereof - Google Patents
Vaterite calcium carbonate microspheres and preparation method thereof Download PDFInfo
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- CN104692439A CN104692439A CN201510113545.8A CN201510113545A CN104692439A CN 104692439 A CN104692439 A CN 104692439A CN 201510113545 A CN201510113545 A CN 201510113545A CN 104692439 A CN104692439 A CN 104692439A
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- calcium carbonate
- vaterite
- carbonate microspheres
- sericin solution
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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 144
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 48
- 239000004005 microsphere Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 108010013296 Sericins Proteins 0.000 claims abstract description 32
- 239000013078 crystal Substances 0.000 claims abstract description 16
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000011575 calcium Substances 0.000 claims abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000000502 dialysis Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims description 3
- 241000382353 Pupa Species 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000047 product Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 235000010216 calcium carbonate Nutrition 0.000 abstract 5
- 238000001035 drying Methods 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 5
- 229910021532 Calcite Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229920000587 hyperbranched polymer Polymers 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000003519 biomedical and dental material Substances 0.000 description 2
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 241000237858 Gastropoda Species 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000011157 advanced composite material Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000003592 biomimetic effect Effects 0.000 description 1
- 229920001222 biopolymer Polymers 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000003278 egg shell Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a method for simply preparing vaterite calcium carbonate microspheres. The preparation method comprises the steps of 1, preparing a sericin solution; 2, preparing a sericin solution with a certain concentration as a template regulation system through the dialyzed sericin solution according to the chemical equation shown in the specification, and dropping calcium salt and carbonate which have the same concentration into a reaction system in a certain proportion; 3, agitating the reaction system for a period of time, centrifuging to remove precipitate, and washing with water at three times; 4, drying the CaCO3 precipitate through a drying box after water washing, so as to obtain the finished product of vaterite calcium carbonate microspheres. The granularity of the CaCO3 microspheres is 1 to 1.5 microns; the vaterite calcium crystal form in the obtained material is more than 80%; the natural sericin solution is used as the template regulation system to regulate CaCO3 crystal form.
Description
Technical field
The present invention relates to field of biomedical materials, be specifically related to a kind of Synthesis and applications of vaterite phase calcium carbonate microspheres, specifically, under relating to a kind of condition being template with sericin, the method for the calcium carbonate microspheres of synthesis vaterite crystal formation.
Background technology
Biomineralization is a mild condition, consumes energy low, free of contamination physical and chemical process, therefore utilizes the mineralising mechanism of OM adjustment can carry out the organic and inorganic matrix material of external effective bio-mimetic syntheses.Biomineralization material is dominated the growth of OM adjustment inorganics by life entity and is formed, generally all there is meticulous microtexture, the structure of these uniquenesses imparts the incomparable performance of their conventional pure inorganic materials, the biopolymer energy induced synthesis different-shape of different structure and the inorganics of crystal formation, especially the most outstanding for the regulation and control of inorganics pattern with protein.Sericin is a kind of globular preteins, and have the biocompatibility of the anti-oxidant and height of Yi Rong, water suction, gelation, correctability, the characteristics such as biodegradability, have a good application prospect in makeup, food, medicine and biomaterial etc.
Calcium carbonate is that a kind of consumption is very large, the new inorganic material of having many uses, the industrial circles such as widespread use and rubber, plastics, papermaking, ink, coating, foods and cosmetics, and due to the biological characteristics of its excellence, also receive in new diseases field and pay close attention to widely.The value of calcium carbonate depends primarily on the chemical constitution of product, morphological specificity, the parameters such as globule size, wherein the most important thing is pattern and the crystal formation of calcium carbonate particles, the calcium carbonate applications of different shape and different field.The calcium carbonate crystal formation of the most stable existence of occurring in nature is calcite, also has ball aragonite, vaterite and amorphous three kinds of morphological structures in addition.Calcite belongs to hexagonal system, and it hides, and performance is good, and whiteness is high, and purity is good, heat-resisting, corrosion-resistant, and stable chemical performance is the important source material of the industry such as metallurgy, cement, glass.Aragonite belongs to rhombic system, is meta crystal formation at normal temperatures and pressures, has higher length-to-diameter ratio, can as the strengthening and toughening agent of desirable biomedical material and advanced composite material.Vaterite is least stable, is often spherical, in the eggshell of gastropod and the spicule of ascidean, has existence, can spontaneous transformation be calcite or aragonite usually, but the life and health of vaterite to biology plays very important effect.Simultaneously in view of the calcium carbonate particles of vaterite crystal formation has unique spherical morphology, particle monodispersity is good, not easily assemble, and there is larger specific surface area, higher dispersing property and less proportion, at raising coating, filling properties, improve the aspects such as the physicals of product, glossiness, whiteness, mobility and printing performance and there is huge application potential.Therefore extremely need a kind of easy method preparing vaterite crystal form calcium carbonate.
The method preparing vaterite phase calcium carbonate at present has multiple, as the patent No. be announce in CN1631792A generate needle-like short fiber d type vaterite phase calcium carbonate with water-miscible organic solvent to regulate and control calcium carbonate crystal formation, vaterite content is greater than 90%, also have the patent No. be announce in CN102557099A with a kind of parents' water type hyperbranched polymer molecule for template regulates and controls to prepare vaterite phase calcium carbonate microspheres, Microsphere Size is again between 2-4.5 μm.Although parents' water type hyperbranched polymer used can reclaim in preparation, but the hyperbranched polymer in the calcium carbonate microspheres of synthesis or containing 7wt-10wt%, still there is certain cytotoxicity, may can only be limited to industrial application, the vaterite phase calcium carbonate/sericin matrix material regulating and controlling preparation with natural protein sericin then has good biocompatibility and degradability, expands its range of application.And more above-mentioned two examples of reaction process are all wanted simply, without the need to control pH and temperature, at room temperature can complete reaction.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the object of this invention is to provide a kind of easy method preparing vaterite phase calcium carbonate microspheres.The sericin used can extract from silk mill's waste water, and the problem solving silk mill's contaminated wastewater has again larger economic benefit.
Concrete technical scheme of the present invention is as follows:
A kind of vaterite calcium carbonate microspheres, calcium carbonate microspheres particle diameter is at 1-1.5 μm, and in resulting materials, the content of vaterite crystal formation is greater than 80%.
A kind of preparation method of described vaterite calcium carbonate microspheres, comprise the steps for: at ambient temperature, prepare sericin solution, getting certain density sericin solution is template to regulate system, under agitation the calcium salt of same concentrations and carbonate are instilled reaction system with certain proportion simultaneously, after continuing stirring reaction system certain hour after being added dropwise to complete again, centrifugal collecting precipitation, wash three times, by the CaCO after washing
3it is dry that precipitation is placed in baking oven, obtains vaterite calcium carbonate microspheres finished product.
Further, described sericin solution of preparing is the Na using 1%-2% massfraction after removing pupa by silk cocoon
2cO
3take mass ratio as 1:15(silk cocoon: Na
2cO
3solution) ratio boil the boiling liquid obtained and namely slightly carry sericin solution.
Further, the sericin solution that template to regulate system is used is dialysed obtain for 3 days by boiling the sericin solution dialysis tubing of 3500 Da of slightly carrying obtained.
Further, the concentration of the sericin solution that adjustment and control system is used is 3-5 mg/mL.
Further, described calcium salt is calcium chloride or nitrocalcite, and described carbonate is sodium carbonate or salt of wormwood.
Further, the calcium salt of described same concentrations and the concentration of carbonate are 1-3 mol/L.
Further, described certain proportion refers to CO
3 2-and Ca
2+ratio be 1:1.
Further, drip rear continuation stirring certain hour described in and refer to that 30-60 min is stirred in continuation.
Further, the centrifugal taking-up of 8000 rpm of the described precipitation of calcium carbonate prepared, dries after washing three times in 60-70 DEG C of baking oven.Without the need to adopting any other organic solvent to wash in aftertreatment.
The invention has the beneficial effects as follows:
(1) the sericin abundance of the present invention's use, solves the problem of silk mill's waste water purposes, supports environmental protection.
(2) the present invention selects sericin as template to regulate system, and the calcium carbonate prepared/sericin matrix material has biocompatibility and the biodegradability of height, and favorable dispersity, size uniformity, vaterite crystal formation content is high.
(3) preparation feedback of vaterite phase calcium carbonate microspheres is in room temperature, and carry out in water solution system, mild condition, the reaction times is short, and program is simple, and without the need to temperature control and adjustment pH, equipment requirements is low, is easy to industrialization.
(4) each the vaterite phase calcium carbonate microspheres prepared by the present invention there is one or more aperture, with the biocompatibility of its height and biodegradability, except being applied to coating, outside the industrial production such as filler, bio-medical material can also be applied to further.
Accompanying drawing explanation
Fig. 1 is the large area scanning electromicroscopic photograph of the vaterite phase calcium carbonate microspheres that embodiment 1 obtains.
Fig. 2 is the stereoscan photograph of the vaterite phase calcium carbonate microspheres that embodiment 1 obtains.
Fig. 3 is the XRD figure spectrum of the vaterite phase calcium carbonate that embodiment 1 obtains.
Fig. 4 is the infared spectrum of the vaterite phase calcium carbonate that embodiment 1 obtains.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
As Figure 1-4, the sericin solution in the embodiment of the present invention obtains by the following method:
Get 12 g Na
2cO
3join in 800 mL water the sodium carbonate solution being configured to 1.5%, taking the dried silk cocoon of 53.3g joins in this solution, boil half an hour and take out boiling liquid, the sodium carbonate solution adding 800 mL 1.5% again boils for the second time gets above-mentioned silk cocoon, boil half an hour and take out boiling liquid, twice boiling liquid one is reinstated 3500 Da dialysis tubings and is dialysed in deionized water 3 days, within every 8 hours, changes a deionized water, to remove sodium carbonate wherein and other foreign ions.It is for subsequent use that sericin strength of solution after dialysis is concentrated into 30 mg/mL.In-20 DEG C of preservations.
Embodiment 1
(1) configuration of calcium saline solution: by the Calcium Chloride Powder Anhydrous of 2 mol, is dissolved in 1 L deionized water, obtains the calcium chloride solution that concentration is 2 mol/L, for subsequent use.
(2) aqueous sodium carbonate configuration: by the sodium carbonate of 2 mol, be dissolved in the deionized water of 1L, obtain the sodium carbonate solution that concentration is 2 mol/L, for subsequent use.
(3) sericin solution allocation: sericin strong solution 25 mL getting above-mentioned simmer down to 30 mg/mL, adds deionized water 125 mL., be configured to sericin solution 150 mL that concentration is 5 mg/mL.
(4) by sodium carbonate solution 5 mL in calcium chloride solution 5 mL in step (1) and step (2) under agitation, be added dropwise in the sericin solution that step (3) configures simultaneously, drip rear continuation and stir half an hour.
(5) by the centrifugal taking-up of 8000 rpm of the precipitation of gained, rear deionization washes three times, and precipitation is got in centrifuge dehydration, dries and namely obtain vaterite phase Paris white powder material under 70 DEG C of conditions.Products obtained therefrom particle diameter is the microballoon of about 1.1 μm, and vaterite crystal formation content is greater than 80%.
Embodiment 2
The configuration of step (1) calcium saline solution is changed into: the nitrocalcite of 2mol, be dissolved in 1L deionized water, obtain the ca nitrate soln that concentration is 2 mol/L, for subsequent use.
Subsequent step is with embodiment 1, and obtained product cut size is the microballoon of about 1.3 μm, and vaterite crystal formation content is greater than 80%.
Embodiment 3
The configuration of step (2) carbonate solution is changed into: the salt of wormwood of 2 mol, be dissolved in 1 L deionized water, obtain the solution of potassium carbonate that concentration is 2 mol/L, for subsequent use.
Subsequent step is with embodiment 1, and obtained product cut size is the microballoon of about 1.2 μm, and vaterite crystal formation content is greater than 80%.
Claims (10)
1. a vaterite calcium carbonate microspheres, is characterized in that: calcium carbonate microspheres particle diameter is at 1-1.5 μm, and in resulting materials, the content of vaterite crystal formation is greater than 80%.
2. a vaterite calcium carbonate microspheres preparation method as claimed in claim 1, it is characterized in that: comprise the steps into: at ambient temperature, prepare sericin solution, getting certain density sericin solution is template to regulate system, under agitation the calcium salt of same concentrations and carbonate are instilled reaction system with certain proportion simultaneously, after continuing stirring reaction system certain hour after being added dropwise to complete again, centrifugal collecting precipitation, wash three times, by the CaCO after washing
3it is dry that precipitation is placed in baking oven, obtains vaterite calcium carbonate microspheres finished product.
3. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: described sericin solution of preparing is the Na using 1%-2% massfraction after removing pupa by silk cocoon
2cO
3take mass ratio as 1:15(silk cocoon: Na
2cO
3solution) ratio boil the boiling liquid obtained and namely slightly carry sericin solution.
4. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: template to regulate system sericin solution used is dialysed obtain for 3 days by boiling the sericin solution dialysis tubing of 3500 Da of slightly carrying obtained.
5. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: the concentration of the sericin solution that adjustment and control system is used is 3-5 mg/mL.
6. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, it is characterized in that: described calcium salt is calcium chloride or nitrocalcite, described carbonate is sodium carbonate or salt of wormwood.
7. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: the calcium salt of described same concentrations and the concentration of carbonate are 1-3 mol/L.
8. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: described certain proportion refers to CO
3 2-and Ca
2+ratio be 1:1.
9. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: described in drip rear continuations and stir certain hour and refer to and continue stirring 30-60 min.
10. vaterite calcium carbonate microspheres preparation method as claimed in claim 2, is characterized in that: the centrifugal taking-up of the described precipitation of calcium carbonate prepared 8000 rpm, dries after washing three times in 60-70 DEG C of baking oven.
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Cited By (4)
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|---|---|---|---|---|
| CN104961115A (en) * | 2015-06-24 | 2015-10-07 | 浙江理工大学 | Hollow hydroxyapatite microsphere and preparation method thereof |
| CN108358229A (en) * | 2018-03-12 | 2018-08-03 | 兰州大学 | One kind preparing micropore CaCO by biomineralization template of recombined collagen3The method of nano-particle |
| CN110550647A (en) * | 2019-09-27 | 2019-12-10 | 泉州师范学院 | Method for preparing nano calcium carbonate by using chitinase as crystal form control agent |
| CN112274695A (en) * | 2020-09-22 | 2021-01-29 | 西北大学 | Preparation method of vaterite-containing hydrogel scaffold material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104961115A (en) * | 2015-06-24 | 2015-10-07 | 浙江理工大学 | Hollow hydroxyapatite microsphere and preparation method thereof |
| CN108358229A (en) * | 2018-03-12 | 2018-08-03 | 兰州大学 | One kind preparing micropore CaCO by biomineralization template of recombined collagen3The method of nano-particle |
| CN110550647A (en) * | 2019-09-27 | 2019-12-10 | 泉州师范学院 | Method for preparing nano calcium carbonate by using chitinase as crystal form control agent |
| CN110550647B (en) * | 2019-09-27 | 2022-02-15 | 泉州师范学院 | Method for preparing nano calcium carbonate by using chitinase as crystal form control agent |
| CN112274695A (en) * | 2020-09-22 | 2021-01-29 | 西北大学 | Preparation method of vaterite-containing hydrogel scaffold material |
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