CN103570052B - Method for preparing single-crystal-form ball aragonite nano calcium carbonate through microemulsion system - Google Patents
Method for preparing single-crystal-form ball aragonite nano calcium carbonate through microemulsion system Download PDFInfo
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Abstract
The invention discloses a method for preparing single-crystal-form ball aragonite nano calcium carbonate through a microemulsion system, and belongs to the technical field of nanometer materials. According to the method, a non-aqueous xylene/emulsifier/co-emulsifier microemulsion system is firstly prepared, then a calcium chloride microemulsion is prepared in a microemulsion area, then a sodium carbonate aqueous solution at certain concentration is slowly added into the calcium chloride microemulsion and reacts to finally obtain a ball aragonite nano calcium carbonate emulsion; or demulsification, precipitation, washing and drying are conducted to obtain the ball aragonite nano calcium carbonate powder. The ball aragonite nano calcium carbonate prepared according to the method provided by the invention has the characteristics such as small particle size, single crystal form, and good stability of crystal form. The reaction condition is mild, the equipment is simple and easy to operate, meanwhile, the chosen materials are low in cost and are easy to get, so that the method is easy in promotion and application.
Description
Technical field
The present invention relates to a kind of preparation method of nano material, particularly relate to the preparation method of single crystal form vaterite-type nano-calcium carbonate under a kind of microemulsion system and this system, belong to technical field of nano material.
Background technology
Nano-calcium carbonate can be used as the properties-correcting agent of plastics, rubber, macromolecule resin, coating, ink etc., improves product performance, improves the quality of products.Conventionally calcium carbonate has three kinds of anhydrous crystal forms, i.e. calcite, vaterite and aragonite.Research finds that the calcium carbonate of different-shape, size and crystal formation has unique character and feature, and shows excellent functionalization character.The calcium carbonate common name multiform calcium carbonate of this different crystal forms and pattern, is extended to multiple fields such as medicine, microelectronic device, catalytic material and energy technology.
Vaterite belongs to hexagonal system, there is unique spherical morphology, particle monodispersity is good, difficult assembles, and there is larger specific surface area, higher dispersing property and less proportion, improving Tu cloth, filling properties, the aspect such as physicals, glossiness, whiteness, mobility and printing performance of improving product has huge application potential.Therefore, how controllably preparing monodispersed vaterite-type Nano particles of calcium carbonate receives publicity.
The at present preparation method of Nano-Calcium Carbonate, mainly contains intermittently carborization, multilevel spray carbonization and gravity Method continuously, but three kinds of methods all exist in nano-calcium carbonate building-up process crystal formation not single, common drawback such as dispersed undesirable grade.And the microemulsion method occurring in recent years, advantages such as, size controlled, particle good dispersity simple to operate with it and receiving much concern.Prepare in scheme at many published microemulsion method vaterite-type calcium carbonates, preparation be all micron-sized vaterite-type calcium carbonate, the rare report that has single crystal form vaterite-type nano-calcium carbonate.Therefore need the existing preparation scheme to improve to obtain the calcium carbonate of vaterite-type Nano grade.
Summary of the invention
Can only prepare the problem of micron order vaterite-type calcium carbonate in order to solve the microemulsion method existing in prior art, the object of the present invention is to provide a kind of microemulsion system to prepare the method for single crystal form vaterite-type nano-calcium carbonate.
For realizing the object of the invention, the present invention, taking water-soluble salt calcium chloride and sodium carbonate as main raw material, prepares vaterite-type nano-calcium carbonate in a kind of microemulsion system.Specifically prepare by following steps method:
(1) preparation microemulsion nonaqueous component system
Be at 10 DEG C～30 DEG C in temperature, the each nonaqueous component in system is according to twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:3～8:1.3～10;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.5M～2.5M;
prepare calcium chloride microemulsion
First will walk (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stir, after mixing, the mass ratio of each component is twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:3～8:1.3～10:0.23～0.7;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M～2.0M;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, and after adding, then continues magnetic agitation reaction, temperature of reaction is 10 DEG C～30 DEG C;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
In the nano-calcium carbonate microemulsion of preparing in (4) step, adding the water that is equivalent to microemulsion total mass 100%～300%, is to stir at 10 DEG C～30 DEG C in temperature, carries out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation.
washing, dry
To walk (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 10 times of throw outs～30 times of volumes, washs and precipitates, collect the solid precipitation after cleaning, at 40 DEG C～60 DEG C, vacuum-drying is to constant weight, obtain white nano-calcium carbonate calcium powder, be placed in vacuum drier for subsequent use.
The principle of the invention and innovative point are: adopt microemulsion system, experiment discussion has been carried out in preparation to microemulsion nonaqueous component system, adopt emulsifying agent, assistant for emulsifying agent, oil phase to be mixed and made into transparent micro emulsion, prepare on this basis calcium chloride microemulsion, then the aqueous solution of water soluble carbonate is added dropwise to and in calcium chloride microemulsion, prepares pattern and the controlled vaterite-type single crystal form Nano particles of calcium carbonate of particle diameter.Its median size 2nm～3nm.Wherein the vaterite-type nano-calcium carbonate emulsion of preparation can be used as the direct use of modification intermediate at the special occasions taking dimethylbenzene as solvent; And vaterite-type nano-calcium carbonate calcium powder can add to and improves product performance in the system such as coating, ink, the nano-calcium carbonate emulsion of prepared vaterite-type single crystal form or powder property are stable, good dispersity, there is unique spherical morphology, larger specific surface area, less proportion have bright application prospect in multiple fields such as medicine, microelectronic device, catalytic material and energy technology.
The advantage of the inventive method is, reaction conditions gentleness, and equipment is simple, easy handling, selected starting material source is abundant, cheap, is easy to industrial application.
Brief description of the drawings
Fig. 1 is the x-ray diffraction pattern (XRD figure) of the single crystal form vaterite-type nano-calcium carbonate synthetic according to the embodiment of the present invention 1.
Fig. 2 be according to the synthetic vaterite-type nano-calcium carbonate of the embodiment of the present invention 1 in secondary deionized water, under air tight condition, in physical environment, place 9 months the x-ray diffraction pattern (XRD figure) recording.Can clearly see, except the characteristic peak of vaterite crystal formation, also occur the characteristic peak of calcite type (calcite).
Fig. 3 is the transmission electron microscope photo (TEM figure) of the vaterite-type nano-calcium carbonate synthetic according to the embodiment of the present invention 1.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but do not limit practical range of the present invention with this.
Embodiment 1.
(1) preparation microemulsion nonaqueous component system
Be at 10 DEG C in temperature, the each nonaqueous component in system is according to twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:3:5;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 2.0M;
prepare calcium chloride microemulsion
First by step (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stirs, and after mixing, the mass ratio of each component is twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:3:5:0.35;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, after adding, continue magnetic agitation reaction, temperature of reaction is 10 DEG C again, and the reaction times is 10 h;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
In the nano-calcium carbonate microemulsion of preparing in (4) step, adding the water that is equivalent to microemulsion total mass 200%, is to stir at 10 DEG C in temperature, carries out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation;
? washing, dry
To walk (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 15 times of volumes of throw out, washs 2 times and precipitation, collects the solid precipitation after washing, and at 40 DEG C, vacuum-drying, to constant weight, obtains white nano-calcium carbonate calcium powder, is placed in vacuum drier for subsequent use.
Characterize:
Nano-calcium carbonate prepared by step (4) and (5) adopts the scanning of XRD spectrum instrument, is found to be single crystal form vaterite-type nano-calcium carbonate (referring to accompanying drawing 1); Tem observation, finds that monodispersed average particle size 2nm～3nm(is referring to accompanying drawing 3).
Stable crystal form test:
Sample a: microemulsion prepared by step (4) is placed in encloses container places 9 months under physical environment, adopts the scanning of XRD spectrum instrument, finds that vaterite-type nano-calcium carbonate calcium contents is 100%, and crystal conversion does not occur.
Sample b: step (5)-
the solid precipitation leaching, with after being equivalent to the secondary deionized water of 20 times of volumes of throw out and throw out and mixing, be placed in encloses container, under physical environment, place 9 months, adopt the scanning of XRD spectrum instrument, can clearly see, except the characteristic peak of vaterite, also occur the characteristic peak of calcite (calcite/ brief note is: " C ").Find that vaterite-type nano-calcium carbonate calcium contents is 91.5.4%, all the other are converted into calcite crystal formation (referring to accompanying drawing 2).
Embodiment 2.
(1) preparation microemulsion nonaqueous component system
Be at 20 DEG C in temperature, the each nonaqueous component in system is in twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:8:10;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 2.0M;
prepare calcium chloride microemulsion
First by step (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stirs, and after mixing, the mass ratio of each component is twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:8:10:0.61;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M;
(4) prepare nano-calcium carbonate microemulsion
Complete (2), after (3) step, according to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, after adding, continue magnetic agitation reaction, temperature of reaction is 20 DEG C again, and the reaction times is 5 h;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
After (4) step completes, in the nano-calcium carbonate microemulsion of preparing in (4) step, add the water that is equivalent to microemulsion total mass 100%, be to stir at 20 DEG C in temperature, carry out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation;
washing, dry
To walk (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 10 times of volumes of throw out, washs 2 times and precipitation, collects the solid precipitation after washing, and at 50 DEG C, vacuum-drying, to constant weight, obtains white nano-calcium carbonate calcium powder, is placed in vacuum drier for subsequent use.
Characterize:
Vaterite-type nano-calcium carbonate prepared by step (4) and (5) is through tem observation, and adopts the scanning of XRD spectrum instrument, finds monodispersed average particle size 2nm～3nm, and result is similar to embodiment 1
Stable crystal form test:
Sample a: microemulsion prepared by step (4) is placed in encloses container places 9 months under physical environment, adopts the scanning of XRD spectrum instrument, finds that result is identical with embodiment 1, and crystal conversion does not occur.
Sample b: step (5)-
the solid precipitation leaching, with after being equivalent to the secondary deionized water of 20 times of volumes of throw out and throw out and mixing, be placed in encloses container, under physical environment, place 9 months, adopt the scanning of XRD spectrum instrument, find that vaterite-type nano-calcium carbonate calcium contents is 95.5%, all the other are converted into calcite crystal formation.
Embodiment 3.
(1) preparation microemulsion nonaqueous component system
Be at 30 DEG C in temperature, the each nonaqueous component in system is in twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:3.5:5;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 2.5M;
prepare calcium chloride microemulsion
First by step (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stirs, and after mixing, the mass ratio of each component is twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:3.5:5:0.7;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.5M;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, after adding, continue magnetic agitation reaction, temperature of reaction is 30 DEG C again, and the reaction times is 1h;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
In the nano-calcium carbonate microemulsion of preparing in (4) step, adding the water that is equivalent to microemulsion total mass 220%, is to stir at 30 DEG C in temperature, carries out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation;
washing, dry
To walk (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 20 times of volumes of throw out, washs 3 times and precipitation, collects the solid precipitation after washing, and at 60 DEG C, vacuum-drying, to constant weight, obtains white nano-calcium carbonate calcium powder, is placed in vacuum drier for subsequent use.
Characterize:
Vaterite-type nano-calcium carbonate prepared by step (4) and (5) is through tem observation, and adopts the scanning of XRD spectrum instrument, finds monodispersed average particle size 2nm～3nm, and result is similar to embodiment 1.
Stable crystal form test:
Sample a: microemulsion prepared by step (4) is placed in encloses container places 9 months under physical environment, adopts the scanning of XRD spectrum instrument, finds that result is identical with embodiment 1, and crystal conversion does not occur.
Sample b: step (5)-
the solid precipitation leaching, with after being equivalent to the secondary deionized water of 20 times of volumes of throw out and throw out and mixing, be placed in encloses container, under physical environment, place 9 months, adopt the scanning of XRD spectrum instrument, find that vaterite-type nano-calcium carbonate calcium contents is 93.5%, all the other are converted into calcite crystal formation.
Embodiment 4.
(1) preparation microemulsion nonaqueous component system
Be at 15 DEG C in temperature, the each nonaqueous component in system is in twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:4:6;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 2.0M;
prepare calcium chloride microemulsion
First by step (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stirs, and after mixing, the mass ratio of each component is twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:4:6:0.5;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 2.0M;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, after adding, continue magnetic agitation reaction, temperature of reaction is 15 DEG C again, and the reaction times is 8h;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
In the nano-calcium carbonate microemulsion of preparing in (4) step, adding the water that is equivalent to microemulsion total mass 150%, is to stir at 15 DEG C in temperature, carries out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation;
washing, dry
To walk (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 30 times of volumes of throw out, washs 3 times and precipitation, collects the solid precipitation after washing, and at 40 DEG C, vacuum-drying, to constant weight, obtains white nano-calcium carbonate calcium powder, is placed in vacuum drier for subsequent use.
Characterize:
Vaterite-type nano-calcium carbonate prepared by step (4) and (5) is through tem observation, and adopts the scanning of XRD spectrum instrument, finds monodispersed average particle size 2nm～3nm, and result is similar to embodiment 1.
Stable crystal form test:
Sample a: microemulsion prepared by step (4) is placed in encloses container places 9 months under physical environment, adopts the scanning of XRD spectrum instrument, finds that result is identical with embodiment 1, and crystal conversion does not occur.
Sample b: step (5)-
the solid precipitation leaching, with after being equivalent to the secondary deionized water of 20 times of volumes of throw out and throw out and mixing, be placed in encloses container, under physical environment, place 9 months, adopt the scanning of XRD spectrum instrument, find that vaterite-type nano-calcium carbonate calcium contents is 90.5%, all the other are converted into calcite crystal formation.
Embodiment 5.
(1) preparation microemulsion nonaqueous component system
Be at 25 DEG C in temperature, the each nonaqueous component in system is in twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:3:1.3;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.5M;
prepare calcium chloride microemulsion
First by step (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stirs, and after mixing, the mass ratio of each component is twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:3:1.3:0.23;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 2.0M;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, after adding, continue magnetic agitation reaction, temperature of reaction is 25 DEG C again, and the reaction times is 3h;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
In the nano-calcium carbonate microemulsion of preparing in (4) step, adding the water that is equivalent to microemulsion total mass 300%, is to stir at 25 DEG C in temperature, carries out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation;
washing, dry
By step (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 20 times of volumes of throw out, washs 3 times and precipitation, collects the solid precipitation after cleaning, and at 40 DEG C, vacuum-drying, to constant weight, obtains white nano-calcium carbonate calcium powder, is placed in vacuum drier for subsequent use.
Characterize:
Vaterite-type nano-calcium carbonate prepared by step (4) and (5) is through tem observation, and adopts the scanning of XRD spectrum instrument, finds monodispersed average particle size 2nm～3nm, and result is similar to embodiment 1.
Stable crystal form test:
Sample a: microemulsion prepared by step (4) is placed in encloses container places 9 months under physical environment, adopts the scanning of XRD spectrum instrument, finds that result is identical with embodiment 1, and crystal conversion does not occur.
Sample b: step (5)-
the solid precipitation leaching, with after being equivalent to the secondary deionized water of 20 times of volumes of throw out and throw out and mixing, be placed in encloses container, under physical environment, place 9 months, adopt the scanning of XRD spectrum instrument, find that vaterite-type nano-calcium carbonate calcium contents is 92.6%, all the other are converted into calcite crystal formation.
Claims (4)
1. microemulsion system is prepared a method for vaterite nano-calcium carbonate, it is characterized in that, by the following method preparation:
(1) preparation microemulsion nonaqueous component system
Be at 10 DEG C～30 DEG C in temperature, the each nonaqueous component in system is according to emulsifying agent: assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of dimethylbenzene oil phase is 2:3～8:1.3～10;
(2) prepare calcium chloride microemulsion
preparation calcium chloride solution
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.5M～2.5M;
prepare calcium chloride microemulsion
By step (2)--
the calcium chloride water of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stirs, and after mixing, the mass ratio of each component is emulsifying agent: assistant for emulsifying agent: dimethylbenzene oil phase: calcium chloride is 2:3～8:1.3～10:0.23～0.7;
(3) prepare aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M～2.0M;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate solution prepared by (3) step slowly adds in calcium chloride microemulsion prepared by (2) step, stirs while adding, and after adding, then continues magnetic agitation reaction, temperature of reaction is 10 DEG C～30 DEG C;
(5) prepare nano-calcium carbonate calcium powder
breakdown of emulsion, precipitation
In the nano-calcium carbonate microemulsion of preparing in (4) step, adding the water that is equivalent to microemulsion total mass 100%～300%, is to stir at 10 DEG C～30 DEG C in temperature, carries out, after breakdown of emulsion precipitation, solid precipitation being leached to collecting precipitation;
washing, dry
By step (5)-
the solid precipitation leaching, by the secondary deionized water that is equivalent to 10 times of throw outs～30 times of volumes, washs and precipitates, and collects the solid precipitation after cleaning, and at 40 DEG C～60 DEG C, vacuum-drying, to constant weight, obtains nano-calcium carbonate calcium powder.
2. a kind of microemulsion system as claimed in claim 1 is prepared the method for vaterite nano-calcium carbonate, it is characterized in that, step (1) preparation microemulsion nonaqueous component system is selected respectively: twen-80 is as emulsifying agent, and propyl carbinol is as assistant for emulsifying agent, and dimethylbenzene is as oil phase.
3. a kind of microemulsion system as claimed in claim 1 is prepared the method for vaterite nano-calcium carbonate, it is characterized in that step (1) preparation microemulsion nonaqueous component system: twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: the mass ratio of dimethylbenzene oil phase selects the one in following ratio: 2:3:5; 2:8:10; 2:3.5:5; 2:4:6; 2:3:1.3.
4. a kind of microemulsion system as claimed in claim 1 is prepared the method for vaterite nano-calcium carbonate, it is characterized in that step (2)--
prepare calcium chloride microemulsion: twen-80 emulsifying agent: propyl carbinol assistant for emulsifying agent: dimethylbenzene oil phase: the mass ratio of calcium chloride selects the one in following ratio: 2:3:5:0.35; 2:8:10:0.61; 2:3.5:5:0.7; 2:4:6:0.5; 2:3:1.3:0.23.
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| CN110902708B (en) * | 2019-12-13 | 2022-08-16 | 贺州学院 | Method for preparing nano calcium carbonate by using artificial granite waste residues |
| CN111675235B (en) * | 2020-05-21 | 2023-05-16 | 贺州学院 | Preparation method of porous superfine calcium carbonate |
| CN113955788B (en) * | 2021-10-20 | 2023-03-21 | 兰州交通大学 | Method for preparing calcium carbonate particles with different morphologies by adjusting S/CoS ratio in reverse microemulsion system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59142834A (en) * | 1983-02-02 | 1984-08-16 | Ricoh Co Ltd | Manufacture of nonaqueous dispersion liquid of ultrafine carbonate particles |
| CN102583481A (en) * | 2012-01-18 | 2012-07-18 | 兰州交通大学 | Method for preparing spherical nanometer calcium carbonate particles of different grain diameters by reverse microemulsion method |
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59142834A (en) * | 1983-02-02 | 1984-08-16 | Ricoh Co Ltd | Manufacture of nonaqueous dispersion liquid of ultrafine carbonate particles |
| CN102583481A (en) * | 2012-01-18 | 2012-07-18 | 兰州交通大学 | Method for preparing spherical nanometer calcium carbonate particles of different grain diameters by reverse microemulsion method |
| 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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