CN106348332A - Method and device for utilizing dynamic magnetic stirring paddle to prepare vaterite - Google Patents
Method and device for utilizing dynamic magnetic stirring paddle to prepare vaterite Download PDFInfo
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- CN106348332A CN106348332A CN201611047883.7A CN201611047883A CN106348332A CN 106348332 A CN106348332 A CN 106348332A CN 201611047883 A CN201611047883 A CN 201611047883A CN 106348332 A CN106348332 A CN 106348332A
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- magnetic stirring
- stirring paddle
- vaterite
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- 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
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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- 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
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method and a device for utilizing a dynamic magnetic stirring paddle to prepare vaterite. The method comprises the following steps of arraying permanent magnets according to the sequence to prepare the magnetic stirring paddle; placing the magnetic stirring paddle into a reactor; under the condition of stirring, feeding a carbonate solution into a calcium salt solution in the reactor at a constant speed; utilizing a high-intensity magnetic field formed by the permanent magnets on the magnetic stirring paddle for enabling the solution in the reactor to cut magnetic lines; then pumping filtering, washing and drying the reaction solution to obtain the vaterite. The method for preparing the vaterite is a pure physical promotion method, which is simple in process, easy to operate, low in cost, dispensed with any additive, and green and environment-friendly in production process compared with traditional methods requiring adding crystal form control agents and regulating pH. A dynamic rotation magnetic stirring method is adopted, so that the action of the magnetic field is strong, the product purity is high, 100 percent of vaterite type calcium carbonate can be generated, and the method and the device can be largely applied in preparing the vaterite type calcium carbonate.
Description
Technical field
The present invention relates to preparing vaterite technical field and in particular to a kind of prepare vaterite using dynamic magnetic stirring paddle
Method and device.
Background technology
Calcium Carbonate as biological Ore, its low cost vdiverse in function, always important industrial production raw material.Paris white
End is widely used in medicine, detergent, biological medicine, rubber, plastics, papermaking, toothpaste, cosmetics, coating and food industry, is used as
Brightening agent, adsorbent, additive and biomedical material.The above purposes is decided by that the feature of prepared calcium carbonate material belongs to
Property, such as mean diameter, particle diameter distribution, specific surface area, pattern or chemical purity.The physicochemical property of winnofil is walked by synthesis
Suddenly, the height impact of method and synthesis condition, therefore passes through to control certain reaction condition, prepares the carbon of different crystal forms and granularity
Sour calcium, will have considerable prospects for commercial application.
Carbon Dioxide calcium is a kind of polymorphic material, respectively calcite, aragonite and vaterite, and calcite and aragonite exist
In nature and in the majority with calcite, vaterite then needs to obtain by synthetic.Calcite is trigonal system, generally
For rhombus；Aragonite is orthorhombic system, usually needle-like；Vaterite is hexagonal crystal system, generally spherical.Under normal temperature and pressure, Fang Xie
Stone is the most stable, and aragonite takes second place, and vaterite is least stable.Vaterite is a kind of unstable phase thermodynamically, especially in aqueous solution
In, precipitation of calcium carbonate is initially formed vaterite, but within several hours, vaterite can be changed into stable side by recrystallization quickly
Xie Shi, and it is spherical generally to lose it.
Although vaterite is unstable, with respect to calcite and aragonite, its soft texture, color and luster are good, proportion is little, compare table
Area is big, good dispersion, has critically important purposes in industries such as coating, plastics and rubber, can effectively improve the power of composite
Learn performance, mechanical strength and gloss etc., improve physical property, filling capacity and the printing performance of target product, particularly in tooth
It is used as grinding agent, supply falls short of demand in cream product.
The preparation method of Calcium Carbonate includes solid phase method and liquid-phase precipitation method, mainly based on the latter.Document and patent report
Vaterite preparation method have a lot, be mostly (protein, ionic liquid, polyelectrolyte, hyperbranched using adding chemical additives
Polymer and polysaccharide etc.) and regulate and control the methods such as ph, regulating and controlling temperature to stop the transformation to calcite for the vaterite.Patent
The mixed solution of calcium chloride, gelatin and carbamide is freezed 24h at 4 DEG C by us20100215564 in advance, is then incubated at 70 DEG C
24h, prepared vaterite content is 98% Calcium Carbonate.Patent cn102249281 is by aqueous sodium carbonate and calcium chloride water
Add Ionic Liquid as Surface Active Agent 1- butyl -3- Methylimidazole. laurilsulfate solution, prepared content is 100%
Vaterite.Patent cn102583485 and patent cn102557099 add hyperbranched glycidyl ether respectively in calcium saline solution
With end carboxyl super branched polyethers, it is subsequently adding carbonate or bicarbonate is obtained vaterite.Patent cn104692437 is passed through to control
Temperature is obtained different morphologies Calcium Carbonate, and temperature is that vaterite is obtained when 15 DEG C.
For adding chemical additives and regulating and controlling the preparation method of ph, its final product needs to remove controlling agent with purification
Product, not only technique is loaded down with trivial details, and increases production cost, and the stability of chemical additives, reliability affect very on product quality
Greatly.And the method for regulating and controlling temperature, operating process complexity, limited by temperature control energy consumption, not only economy is impacted, and a lot of situation
The vaterite of 100% purity can't be obtained down.
Content of the invention
It is an object of the invention to, a kind of method and device being prepared vaterite using dynamic magnetic stirring paddle is provided.Research and development
New without additive, high-purity, low cost vaterite preparation method it is achieved that the greenization of vaterite preparation process.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of method preparing vaterite using dynamic magnetic stirring paddle, the method is: permanent magnet is arranged in order and makes
Magnetic stirring paddle, described magnetic stirring paddle is placed in reactor, under agitation, carbonate solution is at the uniform velocity introduced in reactor
Calcium salt soln in, using on magnetic stirring paddle permanent magnet constitute high-intensity magnetic field, make the reaction solution in reactor carry out cut magnetic
The line of force is moved, and then reaction solution is obtained vaterite through sucking filtration, washing, dried.
Preferably, the stir speed (S.S.) of described magnetic stirring paddle is 300-1000 rev/min.
Preferably, described magnetic stirring paddle by 2 to or 2 above permanent magnet is formed, the magnetic induction of described permanent magnet
For 2000-6000 Gauss.
Preferably, described carbonate solution is the na of 0.005-1.0mol/l2co3Or nahco3Solution, described calcium salt soln
Cacl for 0.005-0.5mol/l2Solution.
Preferably, the speed that described carbonate solution at the uniform velocity introduces calcium salt soln is 1.0-7.5ml/min.
Preferably, described reaction solution adopts deionized water wash；Described baking temperature is 105 DEG C, and drying time is 2h.
Preferably, the time that described reaction solution stirs cutting magnetic line is 0.5-2h.
In technical scheme, paddle method is stirred using dynamic magnetic, reaction solution is passed through stirring of magnetic stirring paddle
Mix and produce dynamic rotary high-intensity magnetic field, make solution cutting magnetic line being magnetized in high-intensity magnetic field, the effect of Lorentz force is by pole
The big nucleation promoting Calcium Carbonate, thus the generation of thermodynamic instability phase vaterite-type calcium carbonate is facilitated in strengthening, prepares high-purity
The vaterite of degree.The vaterite of the inventive method preparation, its particle size range is 1-5 μm, and purity is 100%.
Present invention also offers a kind of device preparing vaterite using dynamic magnetic stirring paddle, this device includes: reactor,
Magnetic stirring paddle and controller；
Magnetic stirring paddle is installed in described reactor, magnetic stirring paddle is connected with controller, to control the rotation speed of magnetic stirring paddle
Degree, makes the reaction solution mix homogeneously in reactor using the stirring of magnetic stirring paddle；
Described magnetic stirring paddle by 2 to or 2 above permanent magnet is rearranged from top to bottom, in each pair permanent magnet, one piece forever
Upward, the s pole of another piece of permanent magnet is upward for the n pole of magnet.
Preferably, n, s pole of each pair permanent magnet on described magnetic stirring paddle is along stirring loom central axis direction and with center
Axial symmetry is arranged.
Preferably, the magnetic induction of described permanent magnet is 2000-6000 Gauss.
The specific implementation step preparing vaterite using said apparatus is as follows:
The first step, in reactor, magnetic stirring paddle is installed, and magnetic stirring paddle is connected with controller, to control magnetic stirring paddle
Rotary speed, make reaction solution mix homogeneously using the stirring of magnetic stirring paddle.On magnetic stirring paddle, permanent magnet magnetic induction is
2000-6000 Gauss.
Second step, opening controller, under the conditions of stir speed (S.S.) is for 300-1000 rev/min, concentration are 0.005-
The na of 1mol/l2co3Or nahco3With the speed of 1.0-7.5ml/min, at the uniform velocity introduce concentration in reactor is 0.005- to solution
The cacl of 0.5mol/l2In solution.Reaction solution cuts under the stirring action of magnetic stirring paddle and is made up of permanent magnet on stirring paddle
High-intensity magnetic field, the stirring magnetic field of rotation promotes the one-tenth nuclear reaction of Calcium Carbonate, and provides vaterite stable required energy.
3rd step, reaction solution stirring 0.5-2h after, closing control device, solution through sucking filtration, deionized water wash, 105
Vaterite-type calcium carbonate powder is obtained after DEG C 2h being dried.Analyze through x-ray diffraction (xrd) instrument and electronic scanner microscope (sem),
Its particle size range of this calcium carbonate powder is 1-5 μm, and vaterite purity is 100%.
Compared with prior art, the invention has the benefit that
1, what the present invention adopted prepare the method for vaterite and tradition adds chemical additives and compared with regulating and controlling the methods such as ph,
For pure physical method, need not any additive, process is simple, easy to operate, low cost, production process environmental protection.
2, the inventive method adopts dynamic magnetic stirring paddle to produce permanent magnetic strong magnetic field, compared with traditional static permanent magnetic field, magnetic
Field action is strong, and product purity is high, can generate the vaterite-type calcium carbonate of 100% content, can be applied to vaterite on a large scale
The preparation of Calcium Carbonate.
Brief description
Fig. 1 prepares the structural representation of vaterite device for the present invention using dynamic magnetic stirring paddle.
Fig. 2 a is the xrd figure of the vaterite that the embodiment of the present invention 1 is obtained.
Fig. 2 b is the sem figure of the vaterite that the embodiment of the present invention 1 is obtained.
Specific embodiment
With specific embodiment, technical scheme to be described below in conjunction with the accompanying drawings.
Referring to Fig. 1, this figure is that the present invention prepares the structural representation of vaterite device using dynamic magnetic stirring paddle, real below
Apply the vaterite being related in example to prepare all using this device.As shown in figure 1, this device includes: reactor 1, magnetic stirring paddle 2 and control
Device 3 processed.In described reactor 1, magnetic stirring paddle 2 is installed, magnetic stirring paddle 2 is connected with controller 3, to control the rotation of magnetic stirring paddle 2
Speed, makes reaction solution mix homogeneously using the stirring of magnetic stirring paddle 2, and makes reaction solution cutting magnetic line.Described magnetic stirs
Mix oar 2 by 2 to or 2 above permanent magnet is rearranged from top to bottom, in each pair permanent magnet the n pole of one piece of permanent magnet upward,
The s pole of another piece of permanent magnet is upward.N, s pole of each pair permanent magnet on described magnetic stirring paddle is along stirring loom central axis direction simultaneously
With setting substantially symmetrical about its central axis.
Embodiment 1
The present embodiment is directed to the na of low concentration2co3Reaction solution carries out the preparation of vaterite.
In reactor, magnetic stirring paddle is installed, and magnetic stirring paddle is connected with controller, to control the rotation of magnetic stirring paddle
Speed, makes reaction solution mix homogeneously using the stirring of magnetic stirring paddle.On magnetic stirring paddle, permanent magnet magnetic induction is 2000 height
This.
Opening controller, under the conditions of stir speed (S.S.) is 300 revs/min, by the na of 15ml concentration 0.005mol/l2co3Molten
Liquid, with the speed of 1.0ml/min, at the uniform velocity introduces the 15ml cacl that the concentration in reactor is 0.005mol/l2In solution.Reaction
Solution cuts the high-intensity magnetic field being made up of permanent magnet on stirring paddle under the stirring action of magnetic stirring paddle, and the stirring magnetic field of rotation promotes
The one-tenth nuclear reaction of Calcium Carbonate, and provide vaterite stable required energy.
Reaction solution stirring 0.5h after, closing control device, solution through sucking filtration, deionized water wash, 105 DEG C be dried after 2h
Obtain vaterite-type calcium carbonate powder.Through x-ray diffraction (xrd) instrument and electronic scanner microscope (sem) analysis, result such as Fig. 2 a
With shown in Fig. 2 b, Fig. 2 a is the xrd figure of prepared vaterite；Fig. 2 b is the sem figure of prepared vaterite.To powder xrd diffraction
Peak calculates and shows that this vaterite purity is that 100%, sem image particle size range is 1-5 μm.
This example demonstrates that, using the na of low concentration 0.005mol/l2co3Solution and the cacl of 0.005mol/l2Solution,
The vaterite of 100% purity can be prepared.
Embodiment 2
The present embodiment is directed to the nahco of low concentration3Reaction solution, changes magnetic treatment condition, carries out the preparation of vaterite.
In reactor, magnetic stirring paddle is installed, and magnetic stirring paddle is connected with controller, to control the rotation of magnetic stirring paddle
Speed, makes reaction solution mix homogeneously using the stirring of magnetic stirring paddle.On magnetic stirring paddle, permanent magnet magnetic induction is 3000 height
This.
Opening controller, under the conditions of stir speed (S.S.) is 500 revs/min, by the nahco of 150ml concentration 0.005mol/l3
Solution, with the speed of 7.5ml/min, at the uniform velocity introduces the 75ml cacl that the concentration in reactor is 0.005mol/l2In solution.Instead
Solution is answered to cut the high-intensity magnetic field being made up of permanent magnet on stirring paddle under the stirring action of magnetic stirring paddle, the stirring magnetic field of rotation promotees
Enter the one-tenth nuclear reaction of Calcium Carbonate, and provide vaterite stable required energy.
After reaction solution stirring 1h, closing control device, solution through sucking filtration, deionized water wash, 105 DEG C be dried after 2h
To vaterite-type calcium carbonate powder.Through x-ray diffraction (xrd) instrument and electronic scanner microscope (sem) analysis, result shows this ball
Aragonite purity is that 100%, sem image particle size range is 1-5 μm.
This example demonstrates that, using the nahco of low concentration 0.005mol/l3Solution and the cacl of 0.005mol/l2Solution,
Change magnetic treatment condition, the vaterite of 100% purity can be prepared.
Embodiment 3
The present embodiment is directed to the na of high concentration2co3Reaction solution, carries out the preparation of vaterite.
In reactor, magnetic stirring paddle is installed, and magnetic stirring paddle is connected with controller, to control the rotation of magnetic stirring paddle
Speed, makes reaction solution mix homogeneously using the stirring of magnetic stirring paddle.On magnetic stirring paddle, permanent magnet magnetic induction is 4000 height
This.
Opening controller, under the conditions of stir speed (S.S.) is 800 revs/min, by the na of 150ml concentration 0.1mol/l2co3Molten
Liquid, with the speed of 7.5ml/min, at the uniform velocity introduces the 150ml cacl that the concentration in reactor is 0.1mol/l2In solution.Reaction
Solution cuts the high-intensity magnetic field being made up of permanent magnet on stirring paddle under the stirring action of magnetic stirring paddle, and the stirring magnetic field of rotation promotes
The one-tenth nuclear reaction of Calcium Carbonate, and provide vaterite stable required energy.
Reaction solution stirring 1.5h after, closing control device, solution through sucking filtration, deionized water wash, 105 DEG C be dried after 2h
Obtain vaterite-type calcium carbonate powder.Through x-ray diffraction (xrd) instrument and electronic scanner microscope (sem) analysis, result shows this
Vaterite purity is that 100%, sem image particle size range is 1-5 μm.
This example demonstrates that, using the na of high concentration 0.1mol/l2co3Solution and the cacl of 0.1mol/l2Solution, changes
Magnetic treatment condition, can prepare the vaterite of 100% purity.
Embodiment 4
The present embodiment is directed to the nahco of high concentration3Reaction solution, changes magnetic treatment condition, carries out the preparation of vaterite.
In reactor, magnetic stirring paddle is installed, and magnetic stirring paddle is connected with controller, to control the rotation of magnetic stirring paddle
Speed, makes reaction solution mix homogeneously using the stirring of magnetic stirring paddle.On magnetic stirring paddle, permanent magnet magnetic induction is 6000 height
This.
Opening controller, under the conditions of stir speed (S.S.) is 1000 revs/min, by the nahco of 150ml concentration 0.1mol/l3
Solution, with the speed of 7.5ml/min, at the uniform velocity introduces the 75ml cacl that the concentration in reactor is 0.1mol/l2In solution.Reaction
Solution cuts the high-intensity magnetic field being made up of permanent magnet on stirring paddle under the stirring action of magnetic stirring paddle, and the stirring magnetic field of rotation promotes
The one-tenth nuclear reaction of Calcium Carbonate, and provide vaterite stable required energy.
After reaction solution stirring 2h, closing control device, solution through sucking filtration, deionized water wash, 105 DEG C be dried after 2h
To vaterite-type calcium carbonate powder.Through x-ray diffraction (xrd) instrument and electronic scanner microscope (sem) analysis, result shows this ball
Aragonite purity is that 100%, sem image particle size range is 1-5 μm.
This example demonstrates that, using the nahco of high concentration 0.1mol/l3Solution and the cacl of 0.1mol/l2Solution, changes
Magnetic treatment condition, can prepare the vaterite of 100% purity.
Above are only the preferred embodiments of the present invention, the present invention is not limited in the content of embodiment.For in this area
Technical staff for, can have various change and change in the range of technical scheme, any change made and
Change, all within the scope of the present invention.
Claims (10)
1. a kind of method preparing vaterite using dynamic magnetic stirring paddle, the method is: permanent magnet is arranged in order and makes magnetic
Stirring paddle, described magnetic stirring paddle is placed in reactor, under agitation, carbonate solution is at the uniform velocity introduced in reactor
In calcium salt soln, using the high-intensity magnetic field of permanent magnet composition on magnetic stirring paddle, the reaction solution in reactor is made to carry out cutting magnetic force
Line moves, and then reaction solution is obtained vaterite through sucking filtration, washing, dried.
2. as claimed in claim 1 using dynamic magnetic stirring paddle prepare vaterite method it is characterised in that: described magnetic stirring
The stir speed (S.S.) of oar is 300-1000 rev/min.
3. as claimed in claim 1 using dynamic magnetic stirring paddle prepare vaterite method it is characterised in that: described magnetic stirring
Oar by 2 to or 2 above permanent magnet is formed, the magnetic induction of described permanent magnet is 2000-6000 Gauss.
4. as claimed in claim 1 using dynamic magnetic stirring paddle prepare vaterite method it is characterised in that: described carbonate
Solution is the na of 0.005-1.0mol/l2co3Or nahco3Solution, described calcium salt soln is the cacl of 0.005-0.5mol/l2Molten
Liquid.
5. the utilization dynamic magnetic stirring paddle as described in claim 1 or 4 prepare vaterite method it is characterised in that: described carbon
The speed that acid salt solution at the uniform velocity introduces calcium salt soln is 1.0-7.5ml/min.
6. as claimed in claim 1 using dynamic magnetic stirring paddle prepare vaterite method it is characterised in that: described reaction is molten
Liquid adopts deionized water wash；Described baking temperature is 105 DEG C, and drying time is 2h.
7. as claimed in claim 1 using dynamic magnetic stirring paddle prepare vaterite method it is characterised in that: described reaction is molten
The time that liquid stirs cutting magnetic line movement is 0.5-2h.
8. a kind of device preparing vaterite using dynamic magnetic stirring paddle, this device includes: reactor, magnetic stirring paddle and control
Device；
Magnetic stirring paddle is installed in described reactor, magnetic stirring paddle is connected with controller, to control the rotary speed of magnetic stirring paddle, profit
Make the reaction solution mix homogeneously in reactor with the stirring of magnetic stirring paddle；
Described magnetic stirring paddle by 2 to or 2 above permanent magnet is rearranged from top to bottom, one piece of permanent magnet in each pair permanent magnet
N pole upward, the s pole of another piece of permanent magnet is upward.
9. as claimed in claim 8 using dynamic magnetic stirring paddle prepare vaterite device it is characterised in that: described magnetic stirring
N, s pole of each pair permanent magnet on oar is along stirring loom central axis direction and with setting substantially symmetrical about its central axis.
10. as claimed in claim 8 or 9 using dynamic magnetic stirring paddle prepare vaterite device it is characterised in that: described forever
The magnetic induction of magnet is 2000-6000 Gauss.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107117639A (en) * | 2017-06-12 | 2017-09-01 | 宁波普莱斯帝金属制品有限公司 | A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nanometer package assembly |
| CN107162032A (en) * | 2017-06-12 | 2017-09-15 | 宁波普莱斯帝金属制品有限公司 | A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle |
| CN107162033A (en) * | 2017-06-12 | 2017-09-15 | 宁波普莱斯帝金属制品有限公司 | A kind of preparation method of vaterite-type calcium carbonate nano-particles self assemble film |
| CN109867301A (en) * | 2017-12-05 | 2019-06-11 | 财团法人工业技术研究院 | The method for generating needle-like calcium carbonate particle |
| CN113351132A (en) * | 2021-05-13 | 2021-09-07 | 西北矿冶研究院 | Device for correspondingly degrading ziram through photo-magnetic cooperation and use method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107117639A (en) * | 2017-06-12 | 2017-09-01 | 宁波普莱斯帝金属制品有限公司 | A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nanometer package assembly |
| CN107162032A (en) * | 2017-06-12 | 2017-09-15 | 宁波普莱斯帝金属制品有限公司 | A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle |
| CN107162033A (en) * | 2017-06-12 | 2017-09-15 | 宁波普莱斯帝金属制品有限公司 | A kind of preparation method of vaterite-type calcium carbonate nano-particles self assemble film |
| CN107162033B (en) * | 2017-06-12 | 2018-07-10 | 宁波普莱斯帝金属制品有限公司 | A kind of preparation method of vaterite-type calcium carbonate nano-particles self assemble film |
| CN109867301A (en) * | 2017-12-05 | 2019-06-11 | 财团法人工业技术研究院 | The method for generating needle-like calcium carbonate particle |
| CN109867301B (en) * | 2017-12-05 | 2022-01-28 | 财团法人工业技术研究院 | Method for producing acicular calcium carbonate particles |
| CN113351132A (en) * | 2021-05-13 | 2021-09-07 | 西北矿冶研究院 | Device for correspondingly degrading ziram through photo-magnetic cooperation and use method |
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