CN109911924A - The preparation method of calcium carbonate granule - Google Patents
The preparation method of calcium carbonate granule Download PDFInfo
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- CN109911924A CN109911924A CN201711362572.4A CN201711362572A CN109911924A CN 109911924 A CN109911924 A CN 109911924A CN 201711362572 A CN201711362572 A CN 201711362572A CN 109911924 A CN109911924 A CN 109911924A
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- Prior art keywords
- calcium carbonate
- calcium
- preparation
- rotating disk
- carbonate granule
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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 211
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 107
- 239000008187 granular material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000011575 calcium Substances 0.000 claims abstract description 41
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 46
- 239000002002 slurry Substances 0.000 claims description 25
- 239000001569 carbon dioxide Substances 0.000 claims description 23
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 23
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 20
- 239000000920 calcium hydroxide Substances 0.000 claims description 20
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 20
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 238000006703 hydration reaction Methods 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 description 10
- 239000004033 plastic Substances 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 9
- 229920001971 elastomer Polymers 0.000 description 8
- 239000005060 rubber Substances 0.000 description 8
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 5
- 230000010412 perfusion Effects 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000123 paper Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- -1 papermaking Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Abstract
A kind of preparation method of calcium carbonate granule, it include: to have concentration in the hypergravity rotating disk reactor of rotating disk for the calcium source of 0.00015 mol/L to 0.1 mol/L and carbon source feed-in, in 1,000rpm to 5, the revolving speed of 000rpm mixes the calcium source and the carbon source, to form calcium carbonate serosity；And liquid and calcium carbonate granule are separated from the calcium carbonate serosity, wherein the brilliant looks of the calcium carbonate granule include petal-shaped, chain or cubic.
Description
Technical field
This disclosure relates to a kind of preparation method of calcium carbonate granule, espespecially a kind of preparation side of not isomorphous looks calcium carbonate granule
Method.
Background technique
The calcium carbonate of isomorphous looks does not have different purposes, and is applied to different industries.For example, brilliant looks are rose
Petal-shaped calcium carbonate can be used in paper-making industry and rubber, plastics and paint industry, wherein in paper-making industry, have provide whiteness,
The purposes such as brightness, opacity, fluffy degree and ink absorption；It is applied in rubber, plastics and paint industry, having to provide to improve
Expect the purposes such as porosity, oil suction hydrophily, water-retaining property and comprehensive physical mechanical performance；Prismatic calcium carbonate can be used in papermaking
Industry, and have and the purposes such as opacity, intensity and volume are provided；Needle-like calcium carbonate can be used in magazine paper and rubber and plastics
Industry, wherein in magazine paper application, have and promote the purposes such as sheet gloss and fiber coverage rate；In rubber and plastics
In industry, has and promote the purposes such as reinforcing rubber effect and the shock resistance and the flexural strength that promote plastics；Ultra-fine chain carbonic acid
Calcium can be used in industries such as rubber, plastics, paper and coating, has the dispersibility for promoting rubber, plastics, paper and coating, mentions
The activity for rising natural rubber breaking point makes it have the reinforcing effect of more preferably binding ability, promotion synthetic rubber between matrix,
Using as reinforcing filler, and part replaces carbon black or White Carbon black, and then reduces the purposes such as production cost；Spherical calcium carbonate can be used
In industries such as rubber, papermaking, ink and plastics, has and promote dispersibility, specific surface area, coating and filling capacity, to improve light
The purposes such as damp degree, whiteness, mobility and printing；And flaky calcium carbonate can be used in the industries such as papermaking and coating, has and mentions
Rise the purposes such as ink absorption ability, whiteness, printing, flatness, smoothness, glossiness, resistivity and coefficient of elasticity.
As described above, the calcium carbonate based on not isomorphous looks can should in different industries, therefore, industrially, calcium carbonate
Demand is very big.For example, the demand of the plastics calcium carbonate of China is annual greater than 1,000,000 tons, and in papermaking industry, carbon
The demand of sour calcium is annual greater than 3,000,000 tons；The Tai Su company in Taiwan is about 250,000 tons annual in the production capacity of calcium carbonate；And beauty
The calcium carbonate production capacity of the Speciality Minerals company of state is annual 40000000 tons.
It can be seen from the above, isomorphous looks calcium carbonate is not very important industrially for preparation.The prior art uses different
Method controls the brilliant looks of calcium carbonate, for example, improve the reaction temperature of production calcium carbonate, be added in reaction solution additive,
Nonaqueous solvents using methanol or the inverse microemulsion method etc. using surfactant；However, these methods are lacked there are a little
Point, for example, heating can improve the manufacturing cost of calcium carbonate；The residual of additive will affect the purity and mechanicalness of calcium carbonate product
Energy；And the manufacturing cost of calcium carbonate can be improved using nonaqueous solvents and surfactant, reduces reaction speed, and causes environment
Pollution etc..
Therefore, it develops under conditions of without using the additive of such as brilliant looks controlling agent, improves prepared calcium carbonate
The preparation method of the low cost of particle purity, is this field urgent problem to be solved.
Summary of the invention
A kind of preparation method of calcium carbonate granule, comprising: be the calcium of 0.00015 mol/L to 0.1 mol/L by concentration
Source and carbon source feed-in have in the hypergravity rotating disk reactor of rotating disk, make the calcium in the revolving speed of 1,000rpm to 5,000rpm
Source and carbon source mixing, to form calcium carbonate serosity；And liquid and calcium carbonate granule are separated from the calcium carbonate serosity,
In, the brilliant looks of the calcium carbonate granule include petal-shaped, chain or cubic.
Detailed description of the invention
Fig. 1 is the schematic cross-sectional view of hypergravity rotating disk reactor；
Fig. 2 is petal-shaped calcium carbonate granule obtained by the embodiment of the present invention；
Fig. 3 is chainlike calcium carbonate particle obtained by the embodiment of the present invention；
Fig. 4 is cubic calcium carbonate granule obtained by the embodiment of the present invention；And
Fig. 5 is nano-calcium carbonate particles obtained by comparative example of the invention.
Wherein, appended drawing reference:
1 hypergravity rotating disk reactor
10 shells
11 rotating disks
12 shafts
13 perfusion tubes
13a, 13b pipe
14 gas accesses
15 gas vents
16 fluid outlets.
Specific embodiment
Illustrate embodiments of the present invention below by way of particular specific embodiment, those skilled in the art can be by this explanation
The revealed content of book understands other advantages and effect of the invention.The present invention can also be added by other different specific embodiments
To implement or apply, details in this specification can also be based on different perspectives and applications, without departing from the spirit
It is lower to carry out various modifications and change.
Unless otherwise indicated herein, otherwise specification and singular used in the attached claims " one " and
"the" includes plural number individual.
Unless otherwise indicated herein, otherwise specification and term "or" used in the attached claims include " and/
Or " meaning.
Term " brilliant looks " used herein refers to the appearance of particle alignment；Brilliant looks are that chain refers to that major diameter is about 30 to receive
The nano particle of rice (nm) to 99 nanometers is interconnected to form chain pattern；Brilliant looks are that petal-shaped refers to that length is about 0.5 micron
To 5 microns of petal-shaped pattern；And brilliant looks are that cubic refers to the cubic shape that side length is about 0.5 micron to 5 microns
Looks.
Term " nano particle " used herein refers to size between 1nm to the particle between 100nm.
The present invention provides a kind of preparation method of calcium carbonate granule, comprising: concentration is rubbed for 0.00015 mol/L to 0.1
You/liter calcium source and carbon source feed-in have rotating disk hypergravity rotating disk reactor in, in 1,000rpm to 5,000rpm's
Revolving speed mixes the calcium source and the carbon source, to form calcium carbonate serosity；And liquid and carbonic acid are separated from the calcium carbonate serosity
Calcium particle, wherein the brilliant looks of the calcium carbonate granule include petal-shaped, chain or cubic.
Fig. 1 is please referred to, the schematic cross-sectional view of the figure one hypergravity rotating disk reactor of illustrative display is non-to limit
The hypergravity rotating disk reactor types or structure that the present invention uses.
The hypergravity rotating disk reactor 1 has shell 10；Rotating disk 11 in the shell 10, wherein the rotation
The radius of disk 11 is 5 centimetres to 80 centimetres；Connect the shaft 12 of the rotating disk 11；It is connected to the perfusion tube 13 of the rotating disk 11；
Set on the gas access of the shell 10 14, gas vent 15 and fluid outlet 16, wherein the perfusion tube 13 may include two son pipes
13a,13b.It is 0.00015 mol/L to 0.1 mol/L that the preparation method of calcium carbonate granule provided by the invention, which is by concentration,
Calcium source via in 13 feed-in rotating disk 11 of perfusion tube, by the shaft 12 of hypergravity rotating disk reactor 1, extremely with 1,000rpm
5, the 000rpm rotational speed rotating disk 11 makes the calcium source in 0.005 centimetre to 0.1 of average thickness of formation in rotating disk 11
Centimetre liquid film；In addition, carbon source keeps the calcium source and the carbon source mixed via 14 feed-in rotating disk 11 of perfusion tube 13 or gas access
It closes, to form calcium carbonate serosity.
In a specific embodiment, the example of the calcium source includes calcium hydroxide slurry or calcium chloride water, and the calcium source
The flow velocity of the feed-in hypergravity rotating disk reactor 1 is 0.1 liter/min to 1.0 liters/min.More specifically, specific real in one
It applies in example, the preparation method of the calcium carbonate granule further includes by the calcium source and the carbon source feed-in, this has the overweight of rotating disk 11
Before power rotating disk reactor 1, so that calcium oxide and water is carried out hydration reaction, have to obtain the calcium hydroxide slurry as feed-in
The calcium source of the hypergravity rotating disk reactor of rotating disk.It, will be dense in the specific embodiment that the calcium source is calcium hydroxide slurry
Degree is 0.00015 mol/L to 0.1 mol/L and the feedback of calcium hydroxide slurry that flow velocity is 0.1 liter/min to 0.35 liter/min
Enter in the hypergravity rotating disk reactor 1 with rotating disk 11, and it is 0.005 to rub that the carbon source of the feed-in rotating disk 11, which is concentration,
You/rise to 0.05 mol/L, the carbonate aqueous solution that pH value is 3 to 5 and the carbonate aqueous solution feed-in hypergravity rotating disk
The flow velocity of reactor 1 is 0.5 liter/min to 1.2 liters/min, makes the calcium hydroxide in the revolving speed of 1,000rpm to 5,000rpm
Slurries and carbonate aqueous solution mixing, to form calcium carbonate serosity, finally can be obtained cubic calcium carbonate granule, implement herein
In example, the calcium source and the carbon source can begin to be mixed with each other, to be formed respectively via after in sub- pipe 13a, 13b feed-in rotating disk 11
The liquid film of calcium carbonate serosity.
In addition, the preparation method of calcium carbonate granule of the invention may additionally include the calcium source to obtain carbonate aqueous solution
And before the carbon source feed-in hypergravity rotating disk reactor 1 with rotating disk 11, by carbon dioxide gas in a manner of being bubbled
It is soluble in water, to obtain the carbonate aqueous solution.
In the preparation method of calcium carbonate granule of the invention, in addition to use carbonate aqueous solution as carbon source other than, the carbon source is also
It can be carbon dioxide, carbonated mixed gas or carbonate aqueous solution.In addition, passing through the phase of control supply carbon source
Or flow velocity, the brilliant looks of resulting calcium carbonate granule can be changed.
In a specific embodiment, which is carbon dioxide, and the carbon dioxide is somebody's turn to do via 14 feed-in of gas access
Hypergravity rotating disk reactor 1, reaction residual gas are then discharged by gas vent 15, wherein the carbon dioxide flow rate is 0.2
Liter/min to 3.0 liters/min.If the carbon source is carbonated mixed gas, with the intracorporal total volume meter of the gaseous mixture
It calculates, the concentration of the carbon dioxide is 10% to less than 100%, and the mixed gas feed-in hypergravity rotating disk reactor 1
Flow velocity is 0.2 liter/min to 50 liters/min.
In using the specific embodiment of carbon dioxide or carbonated mixed gas as carbon source, the carbon dioxide
Flow velocity can be 0.2 liter/min to 1.2 liters/min, being 30 nanometers to 99 nanometers as major diameter to obtain the calcium carbonate granule receives
Rice grain, the nano particle simultaneously arrange chaining shape.If the flow velocity for adjusting the carbon dioxide is 1.3 liters/min to 3.0 liters/min,
Petal-shaped calcium carbonate granule then can be obtained.
The preparation method of calcium carbonate granule according to the present invention is to make aforementioned calcium source and carbon source at such as 15 DEG C to 35 DEG C of room temperature
It is mixed with various concentration and flow velocity, to form calcium carbonate serosity, later, which flows through fluid outlet 16, then with mistake
The mode of filter or centrifugation separates liquid and calcium carbonate granule from the calcium carbonate serosity, to obtain the calcium carbonate of not isomorphous looks
Grain, and brilliant looks controlling agent is not used in the present invention, therefore without brilliant looks controlling agent in the calcium carbonate serosity.Therefore, the calcium carbonate granule
Preparation method can save energy cost, avoid because additive remain, influence calcium carbonate granule purity and its mechanical performance.Again
Person, the preparation method of calcium carbonate granule according to the present invention can avoid nucleation rate mistake caused by hypergravity rotating disk reactor
Fastly, the problem of being unable to control crystal shape.
Embodiment 1: preparation petal-shaped calcium carbonate granule
0.0446 moles calcium is placed in 1 liter of deionized water, is stirred to form calcium hydroxide slurry；By hydroxide
Respectively with 0.25 liter/min and 2 liters/min of flow velocity, feed-in revolving speed is 2,000rpm's for calcium slurries and carbon dioxide gas
In hypergravity rotating disk reactor with rotating disk, make calcium hydroxide slurry in 0.03 li of average thickness of formation in rotating disk
The liquid film of rice after carbon dioxide gas is mixed with the calcium hydroxide slurry in rotating disk, forms calcium carbonate serosity.Calcium carbonate is starched
Liquid is filtered, and makes to be separated by solid-liquid separation, to obtain petal-shaped calcium carbonate granule as shown in Figure 2.Petal-shaped calcium carbonate obtained
The purity of particle measures about 95.3% with thermogravimetric analyzer, and micro- with about 0.5 micron to 5 of length with electron microscope observation
The size of rice.
Embodiment 2: preparation arranges catenulate calcium carbonate granule
0.0446 moles calcium is placed in 1 liter of deionized water, is stirred to form calcium hydroxide slurry；By hydroxide
Respectively with 0.25 liter/min and 1 liter/min of flow velocity, feed-in revolving speed is 2,000rpm's for calcium slurries and carbon dioxide gas
In hypergravity rotating disk reactor with rotating disk, make calcium hydroxide slurry in 0.03 li of average thickness of formation in rotating disk
The liquid film of rice after carbon dioxide gas is mixed with the calcium hydroxide slurry in rotating disk, forms calcium carbonate serosity.Calcium carbonate is starched
Liquid is filtered, and makes to be separated by solid-liquid separation, to obtain the calcium carbonate granule of catenation as shown in Figure 3.Catenation obtained
The purity of calcium carbonate granule be about 96.7%, and the nano particle for being about 30 nanometers to 99 nanometers with major diameter.
Embodiment 3: cubic calcium carbonate granule is prepared
0.0446 moles calcium is placed in 1 liter of deionized water, is stirred to form calcium hydroxide slurry；It is another to utilize exposure
Device of air injects carbon dioxide into water, to form the carbonate aqueous solution of pH 3.8.Calcium hydroxide slurry and carbonic acid is water-soluble
For liquid respectively with 0.25 liter/min and 0.75 liter/min of flow velocity, feed-in revolving speed is the hypergravity with rotating disk of 2,000rpm
In rotating disk reactor, make calcium hydroxide slurry with carbonate aqueous solution after mixing in rotating disk, forms calcium carbonate serosity.By carbon
Sour calcium slurries are filtered, to obtain cubic calcium carbonate granule as shown in Figure 4.Cubic calcium carbonate obtained
The purity of grain is about 97.7%, and with about 0.5 micron to 5 microns of side length of size.
Comparative example 1: nano-calcium carbonate particles are prepared
0.178 moles calcium is placed in 1 liter of deionized water, is stirred to form calcium hydroxide slurry；By hydroxide
Respectively with 1.1 liters/min and 2 liters/min of flow velocity, feed-in revolving speed is the tool of 2,000rpm for calcium slurries and carbon dioxide gas
Have in the hypergravity rotating disk reactor of rotating disk, makes calcium hydroxide slurry in 0.055 li of average thickness of formation in rotating disk
The liquid film of rice to 0.067 centimetre after carbon dioxide gas is mixed with the calcium hydroxide slurry in rotating disk, forms calcium carbonate slurry
Liquid.Calcium carbonate serosity is filtered, makes to be separated by solid-liquid separation, to obtain nano-calcium carbonate particles as shown in Figure 5.
Compared above-described embodiment 1 to 3 and comparative example 1, the preparation method of not isomorphous looks calcium carbonate granule of the invention is
At such as 15 DEG C to 35 DEG C of room temperature, the obtained calcium hydroxide slurry of hydration reaction is carried out using the calcium source of low concentration, by overweight
Power rotating disk reactor is mixed with carbon source, and the revolving speed of the flow velocity and rotating disk by adjusting calcium source and carbon source, is not being added
Under conditions of adding the additives such as any brilliant looks controlling agent, unsaturated fatty acid or dispersing agent, obtained in a manner of continuous production
The calcium carbonate granule of the not isomorphous looks such as petal-shaped, chain or cubic of high-purity.In addition, not isomorphous looks carbonic acid of the invention
Calcium oxide used in calcium source may be derived from the obtained product after limestone calcination, and carbon source institute in the preparation method of calcium particle
The carbon dioxide used is recyclable from air, and therefore, the present invention provides not only the preparation method of low cost, and passes through waste
Recycling and reusing and achieving the effect that preserve our planet resource with reduce environmental pollution.In addition, the present invention avoids remaining because of additive,
Influence calcium carbonate granule purity and its mechanical performance.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
Various corresponding changes and modifications, but these corresponding changes and modifications can be made according to the present invention by knowing those skilled in the art
It all should belong to the protection scope of the claims in the present invention.
Claims (16)
1. a kind of preparation method of calcium carbonate granule, comprising:
By the hypergravity rotation of calcium source and carbon source feed-in with rotating disk that concentration is 0.00015 mol/L to 0.1 mol/L
In disk reactor, mix the calcium source and the carbon source in the revolving speed of 1,000rpm to 5,000rpm, to form calcium carbonate serosity；With
And
Liquid and calcium carbonate granule are separated from the calcium carbonate serosity, which is characterized in that the brilliant looks of the calcium carbonate granule include flower
Petaloid, chain or cubic.
2. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that the calcium source is to be fed to the rotating disk
On, and being formed by average thickness of liquid film is 0.005 centimetre to 0.1 centimetre.
3. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that the calcium source includes calcium hydroxide slurry
Or calcium chloride water, and the flow velocity of the calcium source feed-in hypergravity rotating disk reactor is 0.1 liter/min to 1.0 liters/min
Clock.
4. the preparation method of calcium carbonate granule as claimed in claim 3, which is characterized in that further include by the calcium source and the carbon
Before the source feed-in hypergravity rotating disk reactor with rotating disk, calcium oxide and water is set to carry out hydration reaction, to be somebody's turn to do
As feed-in, this has the calcium source of the hypergravity rotating disk reactor of rotating disk to calcium hydroxide slurry.
5. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that the carbon source includes carbon dioxide, contains
Mixed gas, carbonate aqueous solution or the carbonate aqueous solution of carbon dioxide.
6. the preparation method of calcium carbonate granule as claimed in claim 5, which is characterized in that the carbon source is carbon dioxide, and should
The flow velocity of the carbon dioxide feed-in hypergravity rotating disk reactor is 0.2 liter/min to 3.0 liters/min.
7. the preparation method of calcium carbonate granule as claimed in claim 5, which is characterized in that the carbon source is carbonated mixed
Gas is closed, and with the calculating of the total volume of the mixed gas, the concentration of the carbon dioxide is 10% to less than 100%, and the mixing
The flow velocity of the gas feed-in hypergravity rotating disk reactor is 0.2 liter/min to 50 liters/min.
8. the preparation method of calcium carbonate granule as claimed in claims 6 or 7, which is characterized in that the flow velocity is 0.2 liter/min
To 1.2 liters/min, and the obtained calcium carbonate granule is the nano particle that major diameter is 30 nanometers to 99 nanometers, the nanometer
Chips with side-by-side arranges into chain.
9. the preparation method of calcium carbonate granule as claimed in claims 6 or 7, which is characterized in that the flow velocity is 1.3 liters/min
To 3.0 liters/min, and the obtained calcium carbonate granule is in the petal-shaped.
10. the preparation method of calcium carbonate granule as claimed in claim 5, which is characterized in that the carbon source is that concentration is rubbed for 0.005
You/0.05 mol/L, the carbonate aqueous solution that pH value is 3 to 5 are risen to, and the carbonate aqueous solution feed-in hypergravity rotating disk is anti-
The flow velocity for answering device is 0.5 liter/min to 1.2 liters/min.
11. the preparation method of calcium carbonate granule as claimed in claim 10, which is characterized in that calcium source feed-in hypergravity rotation
The flow velocity of disk reactor is 0.1 liter/min to 0.35 liter/min, and the obtained calcium carbonate granule is in the cube
Shape.
12. the preparation method of calcium carbonate granule as described in claim 10 or 11, which is characterized in that further include by the calcium source
And before the carbon source feed-in hypergravity rotating disk reactor with rotating disk, carbon dioxide gas is dissolved in a manner of being bubbled
In water, to obtain the carbonate aqueous solution.
13. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that be to make the calcium at 15 DEG C to 35 DEG C
Source and carbon source mixing.
14. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that without crystalline substance in the calcium carbonate serosity
Looks controlling agent.
15. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that the radius of the rotating disk is 5 centimetres
To 80 centimetres.
16. the preparation method of calcium carbonate granule as described in claim 1, which is characterized in that be in a manner of filtering or be centrifuged
Liquid and calcium carbonate granule are separated from the calcium carbonate serosity.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW106143715 | 2017-12-13 | ||
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451544A (en) * | 2019-08-14 | 2019-11-15 | 青海民族大学 | A kind of preparation method of ball shaped nano strontium carbonate |
| CN114074950A (en) * | 2020-08-20 | 2022-02-22 | 财团法人工业技术研究院 | Hollow calcium carbonate micro-sphere and preparation method thereof |
| TWI791339B (en) * | 2021-11-26 | 2023-02-01 | 財團法人工業技術研究院 | Method for preparing rod-shaped calcium carbonate |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116185A (en) * | 1995-05-26 | 1996-02-07 | 北京化工大学 | Ultra-fine calcium carbonate preparation method |
| CN1305956A (en) * | 2000-01-18 | 2001-08-01 | 北京化工大学 | Process for preparing calcium carbonate deposit by continuous method |
| CN1429772A (en) * | 2001-12-31 | 2003-07-16 | 纳米材料科技有限公司 | Method for preparing calcium carbonate with actual forms |
| CN1461731A (en) * | 2002-05-31 | 2003-12-17 | 湘潭大学 | Preparation method of nanometer grade super fine calcium carbonate |
| US20040234443A1 (en) * | 2001-12-31 | 2004-11-25 | Jianfeng Chen | Calcium carbonate of different shapes and the preparation process thereof |
| CN103897434A (en) * | 2014-04-19 | 2014-07-02 | 芮城新泰纳米材料有限公司 | Method for preparing special nano calcium carbonate for plastic master batch |
| CN104229849A (en) * | 2013-06-24 | 2014-12-24 | 湖南宜化化工有限责任公司 | Method for preparing nano calcium carbonate |
| CN105060330A (en) * | 2015-09-14 | 2015-11-18 | 广西大学 | Preparation method of spherical calcium carbonate crystal |
| CN105417564A (en) * | 2015-09-14 | 2016-03-23 | 广西大学 | Preparation method for petal sheet-like calcium carbonate crystals |
-
2017
- 2017-12-13 TW TW106143715A patent/TWI636957B/en active
- 2017-12-18 CN CN201711362572.4A patent/CN109911924B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116185A (en) * | 1995-05-26 | 1996-02-07 | 北京化工大学 | Ultra-fine calcium carbonate preparation method |
| CN1305956A (en) * | 2000-01-18 | 2001-08-01 | 北京化工大学 | Process for preparing calcium carbonate deposit by continuous method |
| CN1429772A (en) * | 2001-12-31 | 2003-07-16 | 纳米材料科技有限公司 | Method for preparing calcium carbonate with actual forms |
| US20040234443A1 (en) * | 2001-12-31 | 2004-11-25 | Jianfeng Chen | Calcium carbonate of different shapes and the preparation process thereof |
| CN1461731A (en) * | 2002-05-31 | 2003-12-17 | 湘潭大学 | Preparation method of nanometer grade super fine calcium carbonate |
| CN104229849A (en) * | 2013-06-24 | 2014-12-24 | 湖南宜化化工有限责任公司 | Method for preparing nano calcium carbonate |
| CN103897434A (en) * | 2014-04-19 | 2014-07-02 | 芮城新泰纳米材料有限公司 | Method for preparing special nano calcium carbonate for plastic master batch |
| CN105060330A (en) * | 2015-09-14 | 2015-11-18 | 广西大学 | Preparation method of spherical calcium carbonate crystal |
| CN105417564A (en) * | 2015-09-14 | 2016-03-23 | 广西大学 | Preparation method for petal sheet-like calcium carbonate crystals |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451544A (en) * | 2019-08-14 | 2019-11-15 | 青海民族大学 | A kind of preparation method of ball shaped nano strontium carbonate |
| CN114074950A (en) * | 2020-08-20 | 2022-02-22 | 财团法人工业技术研究院 | Hollow calcium carbonate micro-sphere and preparation method thereof |
| CN114074950B (en) * | 2020-08-20 | 2024-01-05 | 财团法人工业技术研究院 | Hollow calcium carbonate microspheres and preparation method thereof |
| TWI791339B (en) * | 2021-11-26 | 2023-02-01 | 財團法人工業技術研究院 | Method for preparing rod-shaped calcium carbonate |
Also Published As
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| CN109911924B (en) | 2021-10-01 |
| TW201927696A (en) | 2019-07-16 |
| TWI636957B (en) | 2018-10-01 |
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