CN106698494B - A kind of preparation method of spherical shape micro/nano level calcium carbonate - Google Patents
A kind of preparation method of spherical shape micro/nano level calcium carbonate Download PDFInfo
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- CN106698494B CN106698494B CN201710113014.8A CN201710113014A CN106698494B CN 106698494 B CN106698494 B CN 106698494B CN 201710113014 A CN201710113014 A CN 201710113014A CN 106698494 B CN106698494 B CN 106698494B
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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
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
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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
- 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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Abstract
The invention discloses a kind of preparation method of spherical micro/nano level calcium carbonate, steps are as follows: 1) prepare NH4 +Ammonium carbonate-the additive solution or ammonium hydrogen carbonate-additive solution that concentration is 0.5~4mol/L, additive concentration is 1~2mg/L；Additive is selected from Hexacyanoferrate potassium, Pidolidone, polyvinylpyrrolidone, beta-cyclodextrin, sodium polyphosphate, pentaerythrite, sodium pyrophosphate, sodium dihydrogen phosphate, sodium phosphate, calgon, sodium trimetaphosphate or sodium tetraborate；2) Ca is prepared2+Concentration is the calcium salt soln of 1~3mol/L；3) 1) solution is added drop-wise in calcium salt soln with 2000~4000ul/min, then in 20~50 DEG C of 1~4h of reaction, is added dropwise and all accompanies by when reacting the stirring of 200~400r/min；4) it washs, filters, it is dry；5) filter cake is taken out, is uniformly crushed.This is simple for process, and materials are environmentally friendly, pollution-free.
Description
Technical field
The present invention relates to a kind of preparation methods of spherical micro/nano level calcium carbonate.
Background technique
Calcium carbonate is widely used in various chemical industries as filler.And nanometer grade calcium carbonate is because of the ultra-fine of its particle
Change, crystal structure and Electronic Structure change, and produces quantum size effect that ordinary calcium carbonate do not have, small
Dimensional effect, skin effect and macroscopic quantum effect, magnetism, catalyst, photo-thermal resistance and in terms of with conventional material phase
Than showing superior performance.Its application is also relatively broad, and stability, the hardness of plastic products size can be improved in the plastic
And rigidity, the rheological property of plastics can be improved, improve the heat resistance of plastic products, be added to the ink and biography of nanometer calcium carbonate
System ink filler is compared, and excellent dispersibility, the transparency, excellent ink absorption, fabulous glossiness and high level cadre are embodied
Dry property applies the reinforcing property, tensile property and anti-aging property that material can be improved in rubber, and applying in coating can be with
Its flexibility, hardness, levelability and glossiness are greatly improved, and applies the opacity that paper can be improved in papermaking, increase
The ink absorption of paper, to make into paper softness more glossy.
According to the difference of additive types and additive amount, the crystal form of nanometer calcium carbonate is broadly divided into calcite type, vaterite
Type, aragonitic and the types such as unformed, wherein spherical nanometer calcium carbonate is mainly used in because its shape characteristic is using relatively broad
The industrial circles such as ink, papermaking, printing.
The existing forms of stable nanometer calcium carbonate are calcite type and unformed, and spherical nanometer calcium carbonate is as nano-sized carbon
Present in a kind of metastable state state of sour calcium, the smooth no corner angle in surface make it have other form nanometer calcium carbonate institutes not
The performance having, therefore prepare the hair that the higher nanometer calcium carbonate of sphericity is conducive to the chemical industries such as ink, papermaking, printing
Exhibition.
The preparation of existing spherical nanometer calcium carbonate generally uses more than one additive, and often organic addition
Agent, and method is complicated, and sphericity is not high, therefore, develops a kind of preparation side of new simple and easy spherical nanometer calcium carbonate
Method is extremely urgent to meet the application in terms of ink and papermaking.
Summary of the invention
Present invention seek to address that the technical issues of be to overcome lack in the prior art it is a kind of it is simple and easy, without using organic
The defect of the preparation method of additive and the high spherical nanometer calcium carbonate of product sphericity, and provide a kind of spherical micro/nano level
The preparation method of calcium carbonate.
The present invention provides a kind of preparation methods of spherical micro/nano level calcium carbonate comprising following steps:
(1) ammonium carbonate-additive solution or ammonium hydrogen carbonate-additive solution are prepared；The additive is Hexacyanoferrate
Potassium, Pidolidone, polyvinylpyrrolidone, beta-cyclodextrin, sodium polyphosphate, pentaerythrite, sodium pyrophosphate, sodium dihydrogen phosphate,
Any one of sodium phosphate, calgon, sodium trimetaphosphate and sodium tetraborate；Ammonium carbonate-the additive solution or described
In ammonium hydrogen carbonate-additive solution, NH4 +Concentration be 0.5~4mol/L, the concentration of the additive is 1~2mg/L；
(2) calcium salt soln, Ca in the calcium salt soln are prepared2+Concentration is 1~3mol/L；
(3) ammonium carbonate-additive solution or ammonium hydrogen carbonate-additive solution are added drop-wise in calcium salt soln, drop rate
For 2000~4000ul/min, 1~4h is reacted after being added dropwise again, be added dropwise and all accompanies by stirring, the temperature of the reaction when reacting
Degree is 20~50 DEG C, and the rate of the stirring is 200~400r/min；
(4) it washs, filters, it is dry；
(5) filter cake after drying is taken out, is uniformly crushed.
It is described to be formulated as this field routine operation in step (1), generally sodium carbonate or sodium bicarbonate are mixed with additive
It closes uniform.It is described it is uniformly mixed preferably realized in a manner of magnetic agitation, the revolving speed of the magnetic agitation is preferably
For 300~500r/min.
In step (1), in the ammonium carbonate-additive solution or the ammonium hydrogen carbonate-additive solution, NH4 +Concentration
Preferably 1~2mol/L.
It is described to be formulated as this field routine operation in step (2), generally calcium salt is uniformly mixed with deionized water, i.e.,
It can.
In step (2), the calcium salt soln is the calcium salt soln of this field routine, preferably calcium chloride solution, fluorination
One of calcium solution and calcium nitrate solution are a variety of.
In step (2), Ca in the calcium salt soln2+Concentration is preferably 1.5~2.5mol/L.
In step (3), the dropwise addition is preferably carried out using peristaltic pump.Wherein, the drop rate of the peristaltic pump is preferable
Ground is 2600ul/min~3600ul/min.Drop rate has been largely fixed the granular size of finished product.
In step (3), the rate of the stirring is preferably 250r/min~350r/min.
In step (3), the time of the reaction is preferably 1.5~3.5h.The time of reaction and the time of stirring are very big
Determined in degree product whether balling-up.The temperature of the reaction is preferably 25 DEG C~35 DEG C.The temperature of reaction is to balling-up
There is very big influence.
In step (4), the washing is preferably washed with deionized water.
In step (4), the temperature of the drying is preferably 100~150 DEG C, is more preferably 110 DEG C~140 DEG C.It is described
Time of drying be preferably 20~50h, be more preferably 30~48h.After through a long time is dry, product structure is more stable,
Be conducive to improve humidity resistance, product is firmer.
In step (5), the crushing is preferably realized in a manner of grinding.
In the present invention, average grain diameter (the average grain of spherical shape micro/nano level calcium carbonate made from the preparation method
Diameter is partial size corresponding to cumulative particle sizes percentile reaches 50%) be 150nm~2 μm, within the scope of this product dispersibility compared with
Good, excessive or too small partial size can all impact the dispersibility of product, this particle size range is also more suitable in ink.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that: the present invention passes through the controllable adjustment to micro-nano calcium carbonate crystal form, preparation
Going out spherical micro/nano level calcium carbonate, the average grain diameter of final products is 150nm~2 μm, conducive to the additive as ink,
And preparation method is simple, materials are environmentally friendly, pollution-free；Particulate component is more evenly, higher at sphericity, and institute is at spherical micro-nano
Calcium carbonate is fuller, and particle diameter distribution is more concentrated, and low energy consumption, conducive to cost is reduced；Equipment used in the present invention is simple, easily grasps
Make, additive used is environment friendly and pollution-free, for preparing green material, creation friendly environment society advantageously.
Detailed description of the invention
Fig. 1 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 1；
Fig. 2 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 2；
Fig. 3 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 3；
Fig. 4 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 4；
Fig. 5 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 5；
Fig. 6 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 6；
Fig. 7 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 7；
Fig. 8 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 8；
Fig. 9 is the SEM figure of spherical shape micro/nano level calcium carbonate made from embodiment 9.
Specific embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
The selection of product specification.
Embodiment 1
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is configured to NH4 +Concentration be 1.2mol/L, be added additive Hexacyanoferrate
Potassium 0.1g stirs to form solution A with 300r/min with magnetic agitation, and additive concentration is 1mg/L in solution A；
(2) calcium chloride is dissolved in deionized water and is configured to the solution that concentration is 1mol/L, form solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2661ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 2 hours.During reaction, reaction temperature is controlled with low temperature thermostat bath
Degree is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 110 DEG C after fully reacting.
The dry time is 48h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 1 μm, and appearance is spherical in shape, as shown in Figure 1.
Embodiment 2
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is configured to NH4 +Concentration be 2mol/L, be added additive sodium pyrophosphate
0.15g is stirred with magnetic agitation with 30r/min, forms solution A, and additive concentration is 1.5mg/L in solution A.
(2) calcium chloride is dissolved in deionized water and is configured to Ca2+Concentration is the solution of 1mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2664ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 1.5 hours.During reaction, it is controlled and is reacted with low temperature thermostat bath
Temperature is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 112 DEG C after fully reacting.
The dry time is 48h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 0.9 μm, and appearance is spherical in shape, as shown in Figure 2.
Embodiment 3
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is configured to NH4 +Concentration be 1.5mol/L, be added additive sodium trimetaphosphate
0.15g is stirred to form solution A with magnetic agitation with 300r/min.Additive concentration is 1.5mg/L in solution A.
(2) calcium chloride is dissolved in deionized water and is configured to Ca2+Concentration is the solution of 1.5mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2668ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 2 hours.During reaction, reaction temperature is controlled with low temperature thermostat bath
Degree is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 110 DEG C after fully reacting.
The dry time is 48h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 0.8 μm, and appearance is spherical in shape, as shown in Figure 3.
Embodiment 4
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is configured to NH4 +Concentration be 1mol/L, be added additive polyvinylpyrrolidine
Ketone 0.11g is stirred to form solution A with magnetic agitation with 300r/min.Additive concentration is 1.1mg/L in solution A.
(2) calcium chloride is dissolved in deionized water and is configured to Ca2+Concentration is the solution of 1mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2672ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 1.5 hours.During reaction, it is controlled and is reacted with low temperature thermostat bath
Temperature is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 110 DEG C after fully reacting.
The dry time is 42h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 1.1 μm, and appearance is spherical in shape, as shown in Figure 4.
Embodiment 5
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is made into NH4 +Concentration be 1mol/L, be added additive glutamic acid 0.12g, add
The concentration for adding agent is 1.2mg/L, is stirred to form solution A with 300r/min with magnetic agitation.
(2) calcium chloride is dissolved in water and is configured to Ca2+Concentration is the solution of 1mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2669ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 2 hours.During reaction, reaction temperature is controlled with low temperature thermostat bath
Degree is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 113 DEG C after fully reacting.
The dry time is 44h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 0.85 μm, and appearance is spherical in shape, as shown in Figure 5.
Embodiment 6
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is made into NH4 +Concentration be 1mol/L, be added additive beta-cyclodextrin 0.13g,
The concentration of additive is 1.3mg/L, is stirred to form solution A with 300r/min with magnetic agitation.
(2) calcium chloride is dissolved in water and is configured to Ca2+Concentration is the solution of 1mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2672ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 1.5 hours.During reaction, it is controlled and is reacted with low temperature thermostat bath
Temperature is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 111 DEG C after fully reacting.
The dry time is 43h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 0.8 μm, and appearance is spherical in shape, as shown in Figure 6.
Embodiment 7
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is made into NH4 +Concentration be 1mol/L, be added additive sodium polyphosphate
0.15g, additive concentration 1.5mg/L are stirred to form solution A with magnetic agitation with 300r/min.
(2) calcium chloride is dissolved in water and is configured to Ca2+Concentration is the solution of 1.5mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2671ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 2 hours.During reaction, reaction temperature is controlled with low temperature thermostat bath
Degree is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 113 DEG C after fully reacting.
The dry time is 43h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 0.9 μm, and appearance is spherical in shape, as shown in Figure 7.
Embodiment 8
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is made into NH4 +Concentration be 1mol/L, be added additive pentaerythrite 0.15g,
The concentration of additive is 1.5mg/L, is stirred to form solution A with 300r/min with magnetic agitation.
(2) calcium chloride is dissolved in water and is configured to Ca2+Concentration is the solution of 1mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2670ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 2 hours.During reaction, reaction temperature is controlled with low temperature thermostat bath
Degree is 30 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 112 DEG C after fully reacting.
The dry time is 48h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 0.7 μm, and appearance is spherical in shape, as shown in Figure 8.
Embodiment 9
A kind of preparation method of the micro-nano calcium carbonate of spherical shape, comprising the following steps:
(1) ammonium carbonate is dissolved in deionized water and is made into NH4 +Concentration be 0.5mol/L, be added additive sodium dihydrogen phosphate
The concentration of 0.14g, additive are 1.4mg/L, are stirred to form solution A with 300r/min with magnetic agitation.
(2) calcium chloride is dissolved in water and is configured to Ca2+Concentration is the solution of 1mol/L, forms solution B.
(3) solution A is added dropwise in solution B with peristaltic pump with the drop rate of 2665ul/min, is continued at this time in B solution
In be stirred with 300r/min, wait be added dropwise completely after react 2 hours.During reaction, reaction temperature is controlled with low temperature thermostat bath
Degree is 50 DEG C.
(4) to which, by gains washing, suction filtration, drying in step (3), wherein drying temperature is 113 DEG C after fully reacting.
The dry time is 48h.
(5) product after will be dry obtained by step (4) takes out, and grinds, obtains final products.
By measurement, the average grain diameter of final products is 1.2 μm, and appearance is spherical in shape, as shown in Figure 9.
Claims (10)
1. a kind of preparation method of spherical shape micro/nano level calcium carbonate, which is characterized in that it includes the following steps:
(1) ammonium carbonate-additive solution or ammonium hydrogen carbonate-additive solution are prepared；The additive is Hexacyanoferrate potassium, L-
Glutamic acid, polyvinylpyrrolidone, beta-cyclodextrin, sodium polyphosphate, pentaerythrite, sodium pyrophosphate, sodium dihydrogen phosphate, phosphoric acid
Any one of sodium, calgon, sodium trimetaphosphate and sodium tetraborate；Ammonium carbonate-the additive solution or the carbonic acid
In hydrogen ammonium-additive solution, NH4 +Concentration be 0.5~4mol/L, the concentration of the additive is 1~2mg/L；
(2) calcium salt soln, Ca in the calcium salt soln are prepared2+Concentration is 1~3mol/L；
(3) ammonium carbonate-additive solution or ammonium hydrogen carbonate-additive solution are added drop-wise in calcium salt soln, drop rate is
2000~4000ul/min reacts 1~4h again after being added dropwise, be added dropwise and all accompany by stirring, the temperature of the reaction when reacting
It is 20~50 DEG C, the rate of the stirring is 250r/min~350r/min；
(4) it washs, filters, it is dry；
(5) filter cake after drying is taken out, is uniformly crushed；
Wherein, the average grain diameter of the spherical micro/nano level calcium carbonate is 150nm~2 μm.
2. preparation method as described in claim 1, which is characterized in that described to be formulated as sodium carbonate or carbonic acid in step (1)
Hydrogen sodium is uniformly mixed with additive；In the ammonium carbonate-additive solution or the ammonium hydrogen carbonate-additive solution,
NH4 +Concentration be 1~2mol/L.
3. preparation method as claimed in claim 2, which is characterized in that in step (1), described is uniformly mixed to be stirred with magnetic force
The mode of mixing is realized.
4. preparation method as claimed in claim 3, which is characterized in that in step (1), the revolving speed of the magnetic agitation is
300~500r/min.
5. preparation method as described in claim 1, which is characterized in that described to be formulated as calcium salt and deionization in step (2)
Water is uniformly mixed；
In step (2), the calcium salt soln is one of calcium chloride solution, calcium fluoride melt solution and calcium nitrate solution or a variety of；
In step (2), Ca in the calcium salt soln2+Concentration is 1.5~2.5mol/L.
6. preparation method as described in claim 1, which is characterized in that in step (3), described be added dropwise is carried out using peristaltic pump.
7. preparation method as claimed in claim 6, which is characterized in that the drop rate of the peristaltic pump is 2600uL/min
~3600uL/min.
8. preparation method as described in claim 1, which is characterized in that in step (3), time of the reaction is 1.5~
3.5h；The temperature of the reaction is 25 DEG C~35 DEG C.
9. preparation method as described in claim 1, which is characterized in that in step (4), the washing be with deionized water into
Row washing；
In step (4), the temperature of the drying is 100~150 DEG C；The time of the drying is 20~50h.
10. preparation method as claimed in claim 9, which is characterized in that in step (4), the temperature of the drying is 110 DEG C~
140℃；The time of the drying is 30~48h；
In step (5), the crushing is realized in a manner of grinding.
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| JP2011051834A (en) * | 2009-09-02 | 2011-03-17 | Taiheiyo Cement Corp | Method of producing high purity vaterite-type spherical calcium carbonate |
| CN102557100A (en) * | 2012-01-06 | 2012-07-11 | 兰州交通大学 | Preparation method of spherical nano calcium carbonate |
| CN103232051A (en) * | 2013-04-24 | 2013-08-07 | 陕西科技大学 | Preparation method of ultrafine porous calcium carbonate microsphere |
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