CN108163879A - A kind of preparation method of the calcium carbonate of different-shape and phase structure - Google Patents
A kind of preparation method of the calcium carbonate of different-shape and phase structure Download PDFInfo
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- CN108163879A CN108163879A CN201810156052.6A CN201810156052A CN108163879A CN 108163879 A CN108163879 A CN 108163879A CN 201810156052 A CN201810156052 A CN 201810156052A CN 108163879 A CN108163879 A CN 108163879A
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- sodium bicarbonate
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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
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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
Abstract
The invention discloses the preparation methods of a kind of different-shape and the calcium carbonate of phase structure, using additive-free method, utilize calcium acetate and the simple precipitation reaction of sodium bicarbonate, under the system of water and ethylene glycol mixed solvent, it is prepared for spherical, ellipsoid, petal-shaped, it is rodlike, fusiform, it is cubic, the calcium carbonate microparticle of the different-shapes such as sheet, and have studied the concentration of calcium acetate and sodium bicarbonate, influence of the volume ratio and reaction temperature of water and ethylene glycol to product phase structure and pattern, the result shows that the concentration of calcium acetate and sodium bicarbonate, the volume ratio and reaction temperature of water and ethylene glycol can influence the phase structure and pattern of calcium carbonate.
Description
Technical field
The invention belongs to calcium carbonate preparing technical field, the calcium carbonate of more particularly to a kind of different-shape and phase structure
Preparation method.
Background technology
Calcium carbonate has the different morphologies such as chain, cube, spherical shape, spindle, sheet, needle-shaped, amorphous.Different-shape
Calcium carbonate is as Additive difference.It is easier to disperse for example, cubic calcium carbonate is added in paint；Chainlike calcium carbonate adds
Into rubber, plastics, there is strengthening action；Needle-like calcium carbonate particle is added to the products such as plastics, rubber, paper as additive
In, the mechanical performance of its orientation and the mobility and processing performance of system are can effectively improve, improves mechanical property, assigns modeling
Material products high surface finish and wear-resisting property.
At present, since the calcium carbonate of different-shape has the function of different, difference as additive in various fields
The preparation of the calcium carbonate of pattern is widely paid close attention to by people, in the reaction process for preparing calcium carbonate, by control starting from
The carbon of different-shape can be made in the reaction conditions such as sub- concentration, mixing speed, solution ph, additive types and additive amount
Sour calcium.People have utilized different inorganic ions (Mg2+、Fe2+、Ni2+And Zn2+Deng) and organic additive be made various
The calcium carbonate particle of pattern.
But majority prepare carried out all under conditions of additive is used, have costly, experimentation, it is cumbersome,
The shortcomings of time-consuming.For this purpose, we are explored under conditions of additive-free, provide a kind of economic and environment-friendly, easy to operate, time-consuming short
Preparation method synthesize the calcium carbonate with different phase structures and pattern.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of different-shapes and the calcium carbonate of phase structure
Preparation method.
To achieve the above object, the technical solution that the present invention takes is as follows：
A kind of preparation method of the calcium carbonate of different-shape and phase structure, includes the following steps：
S1, calcium acetate aqueous solution is added in Glycol Mixture, obtains calcium acetate-Glycol Mixture；
S2, sodium bicarbonate aqueous solution is added in Glycol Mixture, obtains sodium bicarbonate-Glycol Mixture；
S3, the sodium bicarbonate-Glycol Mixture obtained in S2 is added to the calcium acetate-ethylene glycol-water obtained in S1
In solution, 4~6h is stirred to react at 20~80 DEG C, after reaction, still aging 12~15h obtains reactant；Wherein,
The molar ratio of calcium acetate and sodium bicarbonate is 1:1；
S4, by the reactant obtained in S3 is filtered, after washing, dry 18 at 80~100 DEG C~for 24 hours to get to institute
State calcium carbonate.
Preferably, in S1, the volume ratio of ethylene glycol and distilled water is 1~3 in Glycol Mixture:1.
Preferably, in S1, a concentration of 0.3~0.75mol/L of calcium acetate in calcium acetate aqueous solution.
Preferably, in S2, the volume ratio of ethylene glycol and distilled water is 1~3 in Glycol Mixture:1.
In S2, a concentration of 0.3~0.75mol/L of sodium bicarbonate in sodium bicarbonate aqueous solution.
Compared with prior art, preparation method of the invention has the advantages that：
(1) present invention uses additive-free method, using calcium acetate and the simple precipitation reaction of sodium bicarbonate, in water and second two
Under the system of alcohol mixed solvent, the calcium carbonate microparticle of different phase structures and pattern is prepared for, and has studied calcium acetate and carbonic acid
The influence of the concentration of hydrogen sodium, the volume ratio and reaction temperature of water and ethylene glycol to product morphology, result of study show calcium acetate with
The concentration of sodium bicarbonate, the volume ratio of water and ethylene glycol and reaction temperature have an impact the pattern of product；The method of the present invention
It is not used additive, at low cost, easy to operate, energy conservation and environmental protection takes short, and method of the invention be synthesis with different-shape
Calcium carbonate particle provides new approach, has certain reference value.
(2) improvement in terms of phase structure：The body of the concentration of calcium acetate and sodium bicarbonate, water and ethylene glycol is had studied herein
The influence that product ratio and reaction temperature synthesize calcium carbonate, the results showed that：The concentration of calcium acetate and sodium bicarbonate is to the object of calcium carbonate
Phase structure has large effect, when the solution concentration of calcium acetate and sodium bicarbonate is relatively low, advantageously forms pure vaterite-type
Calcium carbonate；When the concentration of calcium acetate and sodium bicarbonate is higher, then the calcium carbonate of the mixture phase of vaterite and calcite is generated；
And the volume ratio of ethylene glycol and water does not have much influences to the phase structure of calcium carbonate；Reaction temperature is to the phase structure of calcium carbonate
There is larger impact, reaction temperature height advantageously forms pure aragonite calcium carbonate.
(3) improvement in terms of pattern：The volume ratio of the concentration of calcium acetate and sodium bicarbonate, water and ethylene glycol is had studied herein
The influence synthesized with reaction temperature to calcium carbonate, the results showed that：By adjusting calcium acetate and sodium bicarbonate concentration, water and ethylene glycol
Volume ratio and reaction temperature can synthesize spherical, ellipsoid, petal-shaped is rodlike, and fusiform is cubic, the differences such as sheet
The calcium carbonate of pattern.
Description of the drawings
Fig. 1 is the XRD diagram that various concentration calcium acetate and sodium bicarbonate prepare calcium carbonate；
Wherein Fig. 1 a, Fig. 1 b, Fig. 1 c be respectively calcium acetate and a concentration of 0.3mol/L, 0.5mol/L of sodium bicarbonate,
The XRD diagram of 0.75mol/L；
Fig. 2 is the scanning electron microscope (SEM) photograph that various concentration calcium acetate and sodium bicarbonate prepare calcium carbonate；
Wherein Fig. 2 a, Fig. 2 b, Fig. 2 c be respectively calcium acetate and a concentration of 0.3mol/L, 0.5mol/L of sodium bicarbonate,
The scanning electron microscope (SEM) photograph of 0.75mol/L；
Fig. 3 be different volumes than ethylene glycol prepare with water the XRD diagram of calcium carbonate；
Wherein Fig. 3 a, Fig. 3 b, Fig. 3 c are that the volume ratio of ethylene glycol and water is 3 respectively:1、1:1、1:3 XRD diagram；
Fig. 4 be different volumes than ethylene glycol prepare with water the scanning electron microscope (SEM) photograph of calcium carbonate；
Wherein Fig. 4 a, Fig. 4 b, Fig. 4 c are that the volume ratio of ethylene glycol and water is 3 respectively:1、1:1、1:3 scanning electron microscope (SEM) photograph；
Fig. 5 is the XRD diagram that differential responses temperature prepares calcium carbonate；
Wherein Fig. 5 a, Fig. 5 b, Fig. 5 c, Fig. 5 d are reaction temperature respectively for 20 DEG C, 40 DEG C, 60 DEG C, 80 DEG C of XRD diagram；
Fig. 6 is the scanning electron microscope (SEM) photograph that differential responses temperature prepares calcium carbonate；
Wherein Fig. 6 a, Fig. 6 b, Fig. 6 c, Fig. 6 d are reaction temperature respectively for 20 DEG C, 40 DEG C, 60 DEG C, 80 DEG C of scanning electron microscope
Figure.
Specific embodiment
The specific embodiment of invention is described in detail below, it is to be understood that protection scope of the present invention not by
The limitation of specific embodiment.The test method of actual conditions is not specified in the following example, usually according to normal condition or
According to the condition proposed by each manufacturer.
Embodiment 1
A kind of preparation method of the calcium carbonate of different-shape and phase structure, is as follows：
S1, the Glycol Mixture (ethylene glycol that the calcium acetate aqueous solution of a concentration of 0.3mol/L of 1ml is added to 20ml
Volume ratio with distilled water is 3:1) in, calcium acetate-Glycol Mixture is obtained；
S2, the Glycol Mixture (second two that the sodium bicarbonate aqueous solution of a concentration of 0.3mol/L of 1ml is added to 20ml
The volume ratio of alcohol and distilled water is 3:1) in, sodium bicarbonate-Glycol Mixture is obtained；
S3, the sodium bicarbonate-Glycol Mixture obtained in S2 is added to the calcium acetate-ethylene glycol-water obtained in S1
In solution, 4h is stirred to react at 20 DEG C, after reaction, still aging 12h obtains reactant；
S4, by the reactant obtained in S3 is filtered, after washing, it is dry for 24 hours to get to the calcium carbonate at 80 DEG C.
Embodiment 2
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is, a concentration of 0.5mol/L of sodium bicarbonate aqueous solution in a concentration of 0.5mol/L of calcium acetate aqueous solution in S1, S2.
Embodiment 3
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is, a concentration of 0.75mol/L of sodium bicarbonate aqueous solution in a concentration of 0.75mol/L of calcium acetate aqueous solution in S1, S2.
Embodiment 4
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is, the volume ratio of ethylene glycol and distilled water is 1 in Glycol Mixture in S1:Ethylene glycol in Glycol Mixture in 1, S2
Volume ratio with distilled water is 1:1.
Embodiment 5
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is, the volume ratio of ethylene glycol and distilled water is 1 in Glycol Mixture in S1:Ethylene glycol in Glycol Mixture in 1, S2
Volume ratio with distilled water is 1:3.
Embodiment 6
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is 40 DEG C to be the reaction temperature in S3.
Embodiment 7
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is 60 DEG C to be the reaction temperature in S3.
Embodiment 8
A kind of preparation method of the calcium carbonate of different-shape and phase structure, specific steps are same as Example 1, and difference is only
It is 80 DEG C to be the reaction temperature in S3.
First, we illustrate different calcium acetates with sodium bicarbonate concentration to carbon by taking calcium carbonate prepared by Examples 1 to 3 as an example
The influence of sour calcium phase structure and pattern
Fig. 1 is the XRD diagram that various concentration calcium acetate and sodium bicarbonate prepare calcium carbonate.Wherein Fig. 1 a, Fig. 1 b, Fig. 1 c difference
It is the XRD diagram of calcium acetate and sodium bicarbonate a concentration of 0.3mol/L, 0.5mol/L, 0.75mol/L.Work as vinegar as seen from Figure 1
During a concentration of 0.3mol/L of sour calcium and sodium bicarbonate, product is calcium carbonate, and object is mutually pure vaterite crystal phase structure；Work as acetic acid
During a concentration of 0.5mol/L of calcium and sodium bicarbonate, product is still calcium carbonate, and object is mutually vaterite and the mix-crystal of calcite
Phase structure；As a concentration of 0.75mol/L of calcium acetate and sodium bicarbonate, product is calcium carbonate, and object is mutually solved for vaterite and side
The multiphase structure of stone；These results suggest that, the concentration of calcium acetate and sodium bicarbonate have to the phase structure of calcium carbonate compared with
Big influence when the solution concentration of calcium acetate and sodium bicarbonate is relatively low, advantageously forms pure vaterite-type calcium carbonate；Work as acetic acid
When the concentration of calcium and sodium bicarbonate is higher, then the calcium carbonate of the mixture phase of vaterite and calcite is generated.
Fig. 2 is the scanning electron microscope (SEM) photograph that various concentration calcium acetate and sodium bicarbonate prepare calcium carbonate.Wherein Fig. 2 a, Fig. 2 b, figure
2c is the scanning electron microscope (SEM) photograph of calcium acetate and sodium bicarbonate a concentration of 0.3mol/L, 0.5mol/L, 0.75mol/L respectively.It can by Fig. 2
During finding out a concentration of 0.3mol/L when calcium acetate and sodium bicarbonate, the calcium carbonate of preparation is shaggy sphere pattern,
About 1 μm of grain diameter；As a concentration of 0.5mol/L of calcium acetate and sodium bicarbonate, calcium carbonate granule is ellipsoid pattern；When
During a concentration of 0.75mol/L of calcium acetate and sodium bicarbonate, the pattern of calcium carbonate product is fusiform, illustrates calcium acetate and bicarbonate
Na concn has a certain impact to the pattern tool of calcium carbonate.
2nd, we illustrate the volume ratio of ethylene glycol and water to calcium carbonate object by taking calcium carbonate prepared by embodiment 3~5 as an example
The influence of phase structure and pattern
Fig. 3 be different volumes than ethylene glycol prepare with water the XRD diagram of calcium carbonate.Wherein Fig. 3 a, Fig. 3 b, Fig. 3 c are respectively
The volume ratio of ethylene glycol and water is 3:1、1:1、1:3 XRD diagram.As seen from Figure 3, it is different from the volume ratio of water in ethylene glycol
When, pure calcium carbonate can be prepared, and when the volume ratio of ethylene glycol and water is 3:When 1, product is vaterite and calcite
Multiphase structure；When the volume ratio of ethylene glycol and water is 1:When 1, product is vaterite and the multiphase knot of calcite
Structure；When the volume ratio of ethylene glycol and water is 1:When 3, multiphase structure of the product still for vaterite and calcite；Therefore explanation
The volume ratio of ethylene glycol and water does not have much influences to the phase structure of calcium carbonate.
Fig. 4 be different volumes than ethylene glycol prepare with water the scanning electron microscope (SEM) photograph of calcium carbonate.Wherein Fig. 4 a, Fig. 4 b, Fig. 4 c
The volume ratio for being respectively ethylene glycol and water is 3:1、1:1、1:3 scanning electron microscope (SEM) photograph.As seen from Figure 4 when ethylene glycol and water
Volume ratio is 3:When 1, product morphology is fusiform；When the volume ratio of ethylene glycol and water is 1:When 1, the calcium carbonate granule shape seen
Looks are petal-shaped；When the volume ratio of ethylene glycol and water is 1:When 3, calcium carbonate granule is by irregular blocky and cyclic annular (arrow in Fig. 4 c
The direction of head) particle composition.The result shows that：When the volume of ethylene glycol and water is bigger, product morphology is fusiform, works as ethylene glycol
With the volume of water it is smaller when, reach 1:When 3, product morphology is made of irregular blocky and annular granule, illustrate ethylene glycol with
The volume ratio of water is affected to product morphology.
3rd, we illustrate influence of the reaction temperature to shape and appearance of calcium carbonate by taking calcium carbonate prepared by embodiment 3,6~8 as an example
Fig. 5 is the XRD diagram that differential responses temperature prepares calcium carbonate.Wherein Fig. 5 a, Fig. 5 b, Fig. 5 c, Fig. 5 d are reaction respectively
Temperature is 20 DEG C, 40 DEG C, 60 DEG C, 80 DEG C of XRD diagram.It can be prepared at different temperatures it can be seen from Fig. 5 pure
Calcium carbonate.When reaction temperature is 20 DEG C, multiphase structure of the product for vaterite and calcite；When reaction temperature is 40 DEG C
When, product is pure calcite phase structure；When reaction temperature is 60 DEG C, mixture phase of the product for vaterite and calcite
Structure；When reaction temperature is 80 DEG C, product is pure aragonite phase structure；Thus illustrate, reaction temperature is to the object of calcium carbonate
Phase structure has larger impact, and reaction temperature height advantageously forms pure aragonite calcium carbonate.
Fig. 6 is the scanning electron microscope (SEM) photograph that differential responses temperature prepares calcium carbonate.Wherein Fig. 6 a, Fig. 6 b, Fig. 6 c, Fig. 6 d are respectively
Reaction temperature is 20 DEG C, 40 DEG C, 60 DEG C, 80 DEG C of scanning electron microscope (SEM) photograph.It can be seen from Fig. 6 when reaction temperature is 20 DEG C,
Calcium carbonate granule is made of irregular blocky and annular granule, and when reaction temperature is 40 DEG C, the calcium carbonate granule seen is
Cube bulk；When reaction temperature is 60 DEG C, calcium carbonate granule is stratiform；When reaction temperature is 80 DEG C, the pattern of product is
It is rodlike；Illustrate that reaction temperature is affected for the pattern of product.
In conclusion the present invention uses additive-free method, using calcium acetate and the simple precipitation reaction of sodium bicarbonate, in water
Under the system of ethylene glycol mixed solvent, spherical, ellipsoid is prepared for, petal-shaped is rodlike, and fusiform is cubic, and sheet etc. is no
With the calcium carbonate microparticle of pattern, and have studied the concentration of calcium acetate and sodium bicarbonate, the volume ratio of water and ethylene glycol and react temperature
Spend the influence to product phase structure and pattern, the results showed that the volume of the concentration of calcium acetate and sodium bicarbonate, water and ethylene glycol
Than the pattern that calcium carbonate can be influenced with reaction temperature.
It should be noted that involved in claims of the present invention during numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, since the step method of use is identical with embodiment,
It repeats in order to prevent, the present invention describes preferred embodiment and its effect, but those skilled in the art once know base
This creative concept, then additional changes and modifications may be made to these embodiments.So appended claims are intended to be construed to
Including preferred embodiment and fall into all change and modification of the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
God and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (5)
1. the preparation method of the calcium carbonate of a kind of different-shape and phase structure, which is characterized in that include the following steps：
S1, calcium acetate aqueous solution is added in Glycol Mixture, obtains calcium acetate-Glycol Mixture；
S2, sodium bicarbonate aqueous solution is added in Glycol Mixture, obtains sodium bicarbonate-Glycol Mixture；
S3, the sodium bicarbonate-Glycol Mixture obtained in S2 is added to the calcium acetate-Glycol Mixture obtained in S1
In, 4~6h is stirred to react at 20~80 DEG C, after reaction, still aging 12~15h obtains reactant；Wherein, acetic acid
The molar ratio of calcium and sodium bicarbonate is 1:1；
S4, by the reactant obtained in S3 is filtered, after washing, dry 18 at 80~100 DEG C~for 24 hours to get to the carbon
Sour calcium.
2. the preparation method of the calcium carbonate of a kind of different-shape according to claim 1 and phase structure, which is characterized in that
In S1, the volume ratio of ethylene glycol and distilled water is 1~3 in Glycol Mixture:1.
3. the preparation method of the calcium carbonate of a kind of different-shape according to claim 1 and phase structure, which is characterized in that
In S1, a concentration of 0.3~0.75mol/L of calcium acetate in calcium acetate aqueous solution.
4. the preparation method of the calcium carbonate of a kind of different-shape according to claim 1 and phase structure, which is characterized in that
In S2, the volume ratio of ethylene glycol and distilled water is 1~3 in Glycol Mixture:1.
5. the preparation method of the calcium carbonate of a kind of different-shape according to claim 1 and phase structure, which is characterized in that
In S2, a concentration of 0.3~0.75mol/L of sodium bicarbonate in sodium bicarbonate aqueous solution.
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| CN109133137A (en) * | 2018-11-14 | 2019-01-04 | 上海应用技术大学 | A kind of micro-nano calcium carbonate of ellipsoid and preparation method thereof |
| CN109574058A (en) * | 2019-01-18 | 2019-04-05 | 天水师范学院 | A kind of homogeneous precipitation preparation method of calcium carbonate |
| CN109809458A (en) * | 2019-03-21 | 2019-05-28 | 广西大学 | Rugby shape calcium carbonate and its preparation process |
| CN112591780A (en) * | 2020-12-02 | 2021-04-02 | 成都理工大学 | Preparation method of braided calcium carbonate |
| CN113666406A (en) * | 2021-09-17 | 2021-11-19 | 湖北工业大学 | Method for preparing pure calcite phase calcium carbonate in anhydrous system |
| CN117682544A (en) * | 2024-02-04 | 2024-03-12 | 山东宇信纳米科技有限公司 | Preparation method and application of composite crystal form nano calcium carbonate |
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| CN109133137A (en) * | 2018-11-14 | 2019-01-04 | 上海应用技术大学 | A kind of micro-nano calcium carbonate of ellipsoid and preparation method thereof |
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| CN109809458A (en) * | 2019-03-21 | 2019-05-28 | 广西大学 | Rugby shape calcium carbonate and its preparation process |
| CN112591780A (en) * | 2020-12-02 | 2021-04-02 | 成都理工大学 | Preparation method of braided calcium carbonate |
| CN112591780B (en) * | 2020-12-02 | 2023-07-14 | 成都理工大学 | Preparation method of braided calcium carbonate |
| CN113666406A (en) * | 2021-09-17 | 2021-11-19 | 湖北工业大学 | Method for preparing pure calcite phase calcium carbonate in anhydrous system |
| CN113666406B (en) * | 2021-09-17 | 2023-09-22 | 湖北工业大学 | Method for preparing pure calcite phase calcium carbonate in anhydrous system |
| CN117682544A (en) * | 2024-02-04 | 2024-03-12 | 山东宇信纳米科技有限公司 | Preparation method and application of composite crystal form nano calcium carbonate |
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