CN103570051A - Method for preparing nano calcium carbonate quantum dot through microemulsion system - Google Patents
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- CN103570051A CN103570051A CN201310570949.0A CN201310570949A CN103570051A CN 103570051 A CN103570051 A CN 103570051A CN 201310570949 A CN201310570949 A CN 201310570949A CN 103570051 A CN103570051 A CN 103570051A
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Abstract
A method for a nano calcium carbonate quantum dot through a microemulsion system belongs to the technical field of nanometer materials. According to the method, a non-aqueous toluene/emulsifier/co-emulsifier microemulsion system is firstly prepared, then a calcium chloride microemulsion and a sodium carbonate microemulsion are respectively prepared in a microemulsion area, then the sodium carbonate microemulsion is slowly added into the calcium chloride microemulsion and reacts to finally obtain a nano calcium carbonate quantum dot microemulsion. The nano calcium carbonate prepared through the method provided by the invention has the characteristics such as small grain size and uniformity. The nano calcium carbonate quantum dot, as a modified intermediate, can be directly used in a special occasion with methylbenzene as a solvent, so as to reduce the dust pollution of the environment. According to the method, the reaction condition is mild, the equipment is simple and easy to operate, and meanwhile, the chosen main materials are rich in source and low in cost, 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 nano-calcium carbonate quantum dot under a kind of microemulsion system and this system, belong to technical field of nano material.
Background technology
Quantum dot refers to the nanoparticle of particle diameter between 1-10nm, in a plurality of fields such as medicine, microelectronic device, catalytic material and energy technologys, has potential broad prospect of application.Current domestic and foreign literature report, has successfully prepared tellurium every the quantum dot of the materials such as, zinc oxide, titanium dioxide, but up to this point, has not yet found that there is the report of calcium carbonate quantum point.Therefore be necessary calcium carbonate quantum point preparation method to further investigate.
The preparation method of current Nano-Calcium Carbonate is numerous, but most methods can cause material partial concn too high, easily reunite or to type of reactor, the reaction conditions shortcoming such as have relatively high expectations; There is in building-up process the dispersed common drawback such as undesirable grade of nano-calcium carbonate and develop limited simultaneously.The microemulsion method occurring in recent years, advantages such as, size controlled, particle good dispersity simple to operate with it and receiving much attention.Microemulsion method is to utilize the chemical reaction of in the drop of microemulsion (being microreactor) to generate solid to make required nanoparticle, can control volume of water and various reactant concn in the drop of microemulsion and be controlled to nucleus growth, to obtain the monodisperse nanoparticle of various particle diameters.In many published micro-emulsion method for preparing nano calcium carbonate schemes, preparation be all the calcium carbonate that particle diameter is not less than 10nm, the rare report that has the nano-calcium carbonate quantum dot preparation method who is less than 10nm.Therefore need to improve to obtain the nano-calcium carbonate quantum dot that particle diameter is less than 10nm to existing preparation scheme.
Summary of the invention
In order to solve the microemulsion method existing in prior art, can only prepare the problem that particle diameter is not less than the nano-calcium carbonate of 10nm, the object of the present invention is to provide a kind of microemulsion system to prepare the method that particle diameter is less than the nano-calcium carbonate quantum dot of 10nm.
For realizing the object of the invention, it is main raw material that water-soluble salt calcium chloride and sodium carbonate are take in the present invention, prepares nano-calcium carbonate quantum dot in microemulsion system.Specifically comprise the following steps:
(1) preparation microemulsion nonaqueous component system
In temperature, be at 10 ℃～30 ℃, each nonaqueous component in system is in emulsifying agent: assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of toluene oil phase is 2:2.5～3.5:1.5～8.3;
(2) prepare calcium chloride microemulsion
During Calcium Chloride Powder Anhydrous is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.0M～2.5M;
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: toluene oil phase: calcium chloride is 2:2.5～3.5:1.5～8.3:0.2～0.7;
(3) prepare sodium carbonate microemulsion
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M～2.0M;
By step (3)--
the aqueous sodium carbonate of preparation mixes with the microemulsion nonaqueous component system of (1) step preparation, stir, after mixing, the mass ratio of each component is emulsifying agent: assistant for emulsifying agent: toluene oil phase: sodium carbonate is 2:2.5～3.5:1.5～8.3:0.2～0.7;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion 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 ℃～30 ℃ again, and the reaction times is 1.0h～10 h.
Described emulsifying agent be OP-10, Tween-60, tween-80, Arlacel-80, AEO-3 at least one;
Described assistant for emulsifying agent be propyl carbinol, Pentyl alcohol, n-Octanol, primary isoamyl alcohol, isohexyl alcohol, Virahol at least one;
The principle of the invention and innovative point are: experiment discussion has been carried out in the preparation to microemulsion nonaqueous component system, select emulsifying agent, assistant for emulsifying agent, toluene oil phase to be mixed and made into Nonaqueous microemulsion liquid system, then water-soluble Ca salt and non-aqueous microemulsion are mixed and made into transparent emulsion A, again another kind of water soluble carbonate and non-aqueous microemulsion are mixed and made into transparent emulsion B, then microemulsion B is added dropwise in front a kind of microemulsion A, prepares the controlled nano-calcium carbonate quantum dot of particle diameter.Its median size 1nm～3nm.Have that granularity is tiny, homogeneous, stable performance, the features such as good dispersity, can be used as modification intermediate and directly use take the special occasions that toluene is solvent, reduce environment dust pollution.Be expected to bring into play its unique function in a plurality of fields such as biological medicine, microelectronic device, catalytic material and energy technologys.
The advantage of the inventive method is, reaction conditions is gentle, and equipment is simple, easy handling, and selected main raw material(s) source is abundant, and relative low price, is easy to industrial application.
Accompanying drawing explanation
Fig. 1 is according to the transmission electron microscope photo of the synthetic nano-calcium carbonate quantum dot of embodiments of the invention 1 (TEM figure).
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but with this, do not limit practical range of the present invention.
Embodiment 1.
(1) preparation microemulsion nonaqueous component system
In temperature, be at 10 ℃, 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 toluene oil phase is 2:3:5;
(2) prepare calcium chloride microemulsion
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.5M;
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: toluene oil phase: calcium chloride is 2:3:5:0.4;
(3) prepare sodium carbonate microemulsion
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M;
By step (3)--
the aqueous sodium carbonate 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: toluene oil phase: sodium carbonate is that 2:3:5:0.45 prepares sodium carbonate microemulsion;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion 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 ℃ again, and the reaction times is 10 h.
Characterize:
Nano-calcium carbonate microemulsion prepared by step (4) scans through TEM, analyzes and finds that particle diameter is that 1～3nm(is referring to accompanying drawing 1).
Embodiment 2.
(1) preparation microemulsion nonaqueous component system
In temperature, be at 20 ℃, each nonaqueous component in system is in twen-80 emulsifying agent: propyl carbinol and n-Octanol (propyl carbinol/n-Octanol mass ratio is 8/2) assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of toluene oil phase is 2:3:1.5;
(2) prepare calcium chloride microemulsion
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.0M;
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: toluene oil phase: calcium chloride is 2:3:1.5:0.2;
(3) prepare sodium carbonate microemulsion
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 2.0M;
By step (3)--
the aqueous sodium carbonate 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: toluene oil phase: sodium carbonate is that 2:3:1.5:0.25 prepares sodium carbonate microemulsion;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion 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 ℃ again, and the reaction times is 4 h.
Characterize:
Nano-calcium carbonate prepared by step (4) scans through TEM, analyzes and finds that particle diameter is 1～3nm.
Embodiment 3.
(1) preparation microemulsion nonaqueous component system
In temperature, be at 30 ℃, each nonaqueous component in system is in emulsifying agent (Arlacel-80/soil temperature-60/OP-10/AEO-3 mass ratio is 1/2/2/1): assistant for emulsifying agent (isohexyl alcohol/propyl carbinol mass ratio is 1/9): the ratio mixing and stirring that the mass ratio of toluene oil phase is 2:2.5:4;
(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;
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: toluene oil phase: calcium chloride is 2:2.5:4:0.35;
(3) prepare sodium carbonate microemulsion
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.5M;
By step (3)--
the aqueous sodium carbonate 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: toluene oil phase: sodium carbonate is that 2:2.5:4:0.4 prepares sodium carbonate microemulsion;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion 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 ℃ again, and the reaction times is 1 h.
Characterize:
Nano-calcium carbonate prepared by step (4) scans through TEM, analyzes and finds that particle diameter is 1～3nm.
Embodiment 4.
(1) preparation microemulsion nonaqueous component system
In temperature, be at 15 ℃, each nonaqueous component in system is in emulsifying agent (OP-10/ Arlacel-80 mass ratio is 8/2): primary isoamyl alcohol assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of toluene oil phase is 2:3.5:8.3;
(2) prepare calcium chloride microemulsion
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 2.5M;
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: toluene oil phase: calcium chloride is 2:3.5:8.3:0.7;
(3) prepare sodium carbonate microemulsion
preparation aqueous sodium carbonate
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M;
By step (3)--
the aqueous sodium carbonate 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: toluene oil phase: sodium carbonate is that 2:3.5:8.3:0.6 prepares sodium carbonate microemulsion;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion 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 ℃ again, and the reaction times is 8 h.
Characterize:
Nano-calcium carbonate prepared by step (4) scans through TEM, analyzes and finds that particle diameter is 1～3nm.
Embodiment 5.
(1) preparation microemulsion nonaqueous component system
In temperature, be at 25 ℃, each nonaqueous component in system is in POLYSORBATE 80 emulsifying agent: assistant for emulsifying agent (Pentyl alcohol/Virahol mass ratio is 7/3): the ratio mixing and stirring that the mass ratio of toluene oil phase is 2:3:6;
(2) prepare calcium chloride microemulsion
During calcium chloride is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 2.0M;
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: toluene oil phase: calcium chloride is 2:3:6:0.5;
(3) prepare sodium carbonate microemulsion
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.5M;
By step (3)--
the aqueous sodium carbonate 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: toluene oil phase: sodium carbonate is that 2:3:6:0.5 prepares sodium carbonate microemulsion;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion 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 ℃ again, and the reaction times is 2 h.
Characterize:
Nano-calcium carbonate prepared by step (4) scans through TEM, analyzes and finds that particle diameter is 1～3nm.
Claims (4)
1. a method of preparing microemulsion system nano-calcium carbonate quantum dot, is characterized in that, step is prepared from by the following method:
(1) preparation microemulsion nonaqueous component system
In temperature, be at 10 ℃～30 ℃, each nonaqueous component in system is in emulsifying agent: assistant for emulsifying agent: the ratio mixing and stirring that the mass ratio of toluene oil phase is 2:2.5～3.5:1.5～8.3;
(2) prepare calcium chloride microemulsion
During Calcium Chloride Powder Anhydrous is soluble in the aqueous phase, stir, prepare the calcium chloride water that concentration is 1.0M～2.5M;
To suddenly walk (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: toluene oil phase: calcium chloride is 2:2.5～3.5:1.5～8.3:0.2～0.7;
(3) prepare sodium carbonate microemulsion
During powdered sodium carbonate is soluble in the aqueous phase, stir, prepare the aqueous sodium carbonate that concentration is 1.0M～2.0M;
By step (3)--
the aqueous sodium carbonate 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: toluene oil phase: sodium carbonate is 2:2.5～3.5:1.5～8.3:0.2～0.7;
(4) prepare nano-calcium carbonate microemulsion
According to Ca
2+with CO
3 2-the mol ratio ratio that is 1:1, sodium carbonate microemulsion prepared by (3) step slowly adds in sodium carbonate microemulsion prepared by (2) step, stirs while adding, after adding, continue magnetic agitation reaction, temperature of reaction is 10 ℃～30 ℃ again, and the reaction times is 1.0h～10 h;
Described emulsifying agent be OP-10, Tween-60, tween-80, Arlacel-80, AEO-3 at least one;
Described assistant for emulsifying agent be propyl carbinol, Pentyl alcohol, n-Octanol, primary isoamyl alcohol, isohexyl alcohol, Virahol at least one.
2. the preparation method who prepares microemulsion system nano-calcium carbonate quantum dot as claimed in claim 1, is characterized in that, each nonaqueous component of step (1) is in emulsifying agent: assistant for emulsifying agent: the mass ratio of toluene oil phase selects a kind of in following ratio:
2:3:5;
2:3:1.5;
2:2.5:4;
2:3.5:8.3;
2:3:6.
3. the preparation method who prepares microemulsion system nano-calcium carbonate quantum dot as claimed in claim 1, is characterized in that, step (2)-
prepare each component in calcium chloride microemulsion according to emulsifying agent: assistant for emulsifying agent: toluene oil phase: the mass ratio of calcium chloride selects a kind of in following ratio:
2:3:5:0.4;
2:3:1.5:0.2;
2:2.5:4:0.35;
2:3.5:8.3:0.7;
2:3:6:0. 5.
4. the preparation method who prepares microemulsion system nano-calcium carbonate quantum dot as claimed in claim 1, is characterized in that, step (3)-
prepare each component of sodium carbonate microemulsion system in emulsifying agent: assistant for emulsifying agent: toluene oil phase: a kind of in the preferred following ratio of mass ratio of aqueous sodium carbonate:
2:3:5:0.45;
2:3:1.5:0.25;
2:2.5:4:0.4;
2:3.5:8.3:0.6;
2:3:6:0.5.
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| CN109399682A (en) * | 2018-12-06 | 2019-03-01 | 河南省科学院高新技术研究中心 | A kind of food additives active nano-calcium carbonate and preparation method thereof |
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| CN114455621A (en) * | 2022-01-11 | 2022-05-10 | 兰州交通大学 | Preparation method of acicular calcium carbonate |
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| CN104961148A (en) * | 2015-06-26 | 2015-10-07 | 黑龙江大学 | Content-controllable mixed crystal form nano calcium carbonate synthesis method |
| CN105123990A (en) * | 2015-10-08 | 2015-12-09 | 河南工业大学 | Method for preparing stable type sesamol microemulsion |
| CN105123990B (en) * | 2015-10-08 | 2021-08-06 | 河南工业大学 | Method for preparing stable sesamol microemulsion |
| CN109399682A (en) * | 2018-12-06 | 2019-03-01 | 河南省科学院高新技术研究中心 | A kind of food additives active nano-calcium carbonate and preparation method thereof |
| CN109516485A (en) * | 2018-12-06 | 2019-03-26 | 河南省科学院高新技术研究中心 | A kind of method that self-emulsifying systems prepare rodlike modified calcium carbonate |
| CN109608582A (en) * | 2018-12-06 | 2019-04-12 | 河南省科学院高新技术研究中心 | A kind of calcium carbonate functional master batch |
| CN109608582B (en) * | 2018-12-06 | 2021-04-20 | 河南省科学院高新技术研究中心 | Calcium carbonate functional master batch |
| CN110902708A (en) * | 2019-12-13 | 2020-03-24 | 贺州学院 | Method for preparing nano calcium carbonate by using artificial granite waste residues |
| CN110902708B (en) * | 2019-12-13 | 2022-08-16 | 贺州学院 | Method for preparing nano calcium carbonate by using artificial granite waste residues |
| CN114455621A (en) * | 2022-01-11 | 2022-05-10 | 兰州交通大学 | Preparation method of acicular calcium carbonate |
| CN114455621B (en) * | 2022-01-11 | 2023-10-27 | 兰州交通大学 | Preparation method of needle-shaped calcium carbonate |
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