CN108314072A - A kind of preparation method of the core shell nanoparticles with calcium carbonate shell - Google Patents
A kind of preparation method of the core shell nanoparticles with calcium carbonate shell Download PDFInfo
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- CN108314072A CN108314072A CN201810116573.9A CN201810116573A CN108314072A CN 108314072 A CN108314072 A CN 108314072A CN 201810116573 A CN201810116573 A CN 201810116573A CN 108314072 A CN108314072 A CN 108314072A
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- deionized water
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
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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
- C01F11/02—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- 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
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- Life Sciences & Earth Sciences (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
A kind of preparation method of the core shell nanoparticles with calcium carbonate shell, calcium oxide particle is scattered in deionized water, and the complexed surfactant being made of dodecyl benzyl dimethyl ammonium chloride and lauric acid thiocarbamide imidazoline surfactant is added, stirs evenly；Feed liquid is handled under microwave, and feed liquid introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced to the inlet end of atomizer, it under ultrasound condition, sprays, centrifuges to feed liquid, deionized water is washed, dry, obtains the core shell nanoparticles with calcium carbonate shell.
Description
Technical field
The invention belongs to calcium carbonate material preparation fields, and in particular to a kind of to prepare calcium oxide-calcium carbonate core-shell nano
The method of grain.
Background technology
Calcium carbonate is widely used in the industries such as rubber, plastics, coating, papermaking, ink, Jiao Dot agent, fluid sealant, can also apply
In industries such as toothpaste, food, medicine, word material, building materials, chemical fibres.The crystal form of calcium carbonate includes calcite, aragonite, three kinds of vaterite
Type, wherein calcite structure is most stable, and aragonite and vaterite belong to unstable state.
Core-shell particle is usually by a kind of nano material is coated on another nanometer by chemical bond or other active forces
The nanostructure that the surface of material is formed.For example, being surface modified on nuclear structure, then pass through coating material and nuclear material
Interaction, complete the cladding of shell material.However, cladding process usually requires to overcome the cladding between coating material and core
Not exclusively and coating material is combined upper difficulty with shell material, each link occurs coating not comprehensive enough situation, all
The cladding of core-shell material will be caused imperfect.Currently, the method for preparing calcium carbonate is more, but how to prepare with nucleocapsid
Calcium oxide-calcium carbonate core shell nanoparticles simultaneously realize that complete cladding has not been reported, and the present invention is abandoned through surface modification synthetic kernel
Calcium oxide-calcium carbonate core shell nanoparticles of complete cladding have been prepared by growth in situ for the thinking of shell material.
Invention content
The technical scheme is that in order to overcome the shortcoming of prior art, propose a kind of with calcium carbonate shell
The preparation method of core shell nanoparticles.
The present invention proposes a kind of preparation method of the core shell nanoparticles with calcium carbonate shell, includes the following steps：
1) calcium oxide particle that grain size is 2-3 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl
The complexed surfactant of ammonium chloride and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；
2) feed liquid that step 1) obtains is handled into 25-35min under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
Inlet end sprays to feed liquid under ultrasound condition；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Wherein, the power of microwave is 500-600W.
Wherein, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant rub
You are than being 1: 0.7-0.9: 0.05-0.2.
Wherein, in step 1), the mass ratio of calcium oxide and deionized water is 1: 100-200.
Wherein, in step 3), the charge ratio of feed liquid and carbon dioxide is 1g: 200-400mL.
Wherein, in step 4), control centrifuge RPMs are 4000-6000rpm.
Wherein, in step 3), ultrasonic power 150-200W.
The present invention makes calcium oxide surface layer form hydroxide calcium layer using the aquation of microwave condition control calcium oxide particle, leads to
Regulation and control microwave power and time are spent, the thickness of hydroxide calcium layer can be adjusted, and then control the thickness of calcium carbonate shell.Particle table
The calcium hydroxide of layer is with carbon dioxide reaction under conditions of ullrasonic spraying, and feed liquid is under turbulent-flow conditions by great amount of carbon dioxide gas
Body impact is swept along, and is separated into minimum drop by carbon dioxide under ultrasonication, ultrasound promotes gas-liquid phase materials and contacting
Moment react, and be conducive to avoid the reunion of particle during the reaction.It is incorporated into using complexed surfactant
Grain surface, stable particle, avoid reunite while, induction calcium carbonate formed aragonite phase.
Beneficial effects of the present invention：This method uses the gas that is atomized as feed liquid of carbon dioxide, compared to after atomization again
It is contacted with carbon dioxide gas, obtained product particle size is more uniform.Since microwave method has activated the surface of particle, in conjunction with
Transient response under ullrasonic spraying, granule surface activity point is more, and reaction is fast, causes particle surface rough and uneven in surface, more identical size,
The specific grain surface product of pattern significantly increases.The calcium carbonate layer with stable aragonite phase is obtained, nucleocapsid particles size is about
450-720nm。
Specific implementation mode
With reference to embodiment, further illustrate the present invention.
Embodiment 1
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 2
1) calcium oxide particle that grain size is 3 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.9: 0.2；
2) feed liquid that step 1) obtains is handled into 35min, microwave power 600W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 400mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 3
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 4
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 400W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 5
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 700W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 6
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 10min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 7
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 50min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 8
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 100mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 9
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 500mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 10
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.6: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 11
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 1: 0.05；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 12
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.01；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
Embodiment 13
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, is added by dodecyl dimethyl benzyl chloride
The complexed surfactant for changing ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；Calcium oxide and dodecane
Base dimethyl benzyl ammonium chloride, lauric acid thiocarbamide imidazoline surfactant molar ratio be 1: 0.7: 0.3；
2) feed liquid that step 1) obtains is handled into 25min, microwave power 500W under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced atomizer
The charge ratio of inlet end, feed liquid and carbon dioxide is 1g: 200mL, under ultrasound condition, is sprayed to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with carbon
The core shell nanoparticles of sour calcium shell.
The pattern for the product that embodiment 1-13 is obtained is shown in Table 1.
Table 1
Embodiment 14
Using the technique of embodiment 1, parameter, the carrier gas of ultrasonic atomizatio in embodiment 1 is only replaced with into nitrogen, after making atomization
Liquid and carbon dioxide gas counter current contacting.Product is obtained as the inhomogenous particle of the size of 600-1300nm.
Claims (7)
1. a kind of preparation method of the core shell nanoparticles with calcium carbonate shell, which is characterized in that include the following steps：
1) calcium oxide particle that grain size is 2-3 μm is scattered in deionized water, is added by dodecyl dimethyl Benzylmagnesium chloride
The complexed surfactant of ammonium and lauric acid thiocarbamide imidazoline surfactant composition, stirs evenly；
2) feed liquid that step 1) obtains is handled into 25-35min under microwave；
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide gas is introduced to the air inlet of atomizer
End, under ultrasound condition, sprays to feed liquid；
4) feed liquid after spraying is collected, the revolution of centrifugation is controlled, deionized water is washed 2-3 times, dry, is obtained with calcium carbonate
The core shell nanoparticles of shell.
2. according to the method described in claim 1, it is characterized in that：The power of microwave is 500-600W.
3. according to the method described in claim 2, it is characterized in that：Calcium oxide and dodecyl benzyl dimethyl ammonium chloride, the moon
The molar ratio of cinnamic acid thiocarbamide imidazoline surfactant is 1: 0.7-0.9: 0.05-0.2.
4. according to the method described in claim 1, it is characterized in that：In step 1), the mass ratio of calcium oxide and deionized water is 1
∶100-200。
5. according to the method described in claim 1, it is characterized in that：In step 3), the charge ratio of feed liquid and carbon dioxide is 1g:
200-400mL。
6. according to the method described in claim 1, it is characterized in that：In step 4), control centrifuge RPMs are 4000-6000rpm.
7. according to the method described in claim 1, it is characterized in that：In step 3), ultrasonic power 150-200W.
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Cited By (1)
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| CN113603125A (en) * | 2021-03-08 | 2021-11-05 | 台湾塑胶工业股份有限公司 | Calcined shellfish shell powder and its preparation method |
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| EP2796412A1 (en) * | 2013-04-24 | 2014-10-29 | Università Del Salento - Dipartimento Di Ingegneria Dell'Innovazione | Synthesis of nano-sized CaCO3 particles by spray dryer |
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| CN113603125A (en) * | 2021-03-08 | 2021-11-05 | 台湾塑胶工业股份有限公司 | Calcined shellfish shell powder and its preparation method |
| CN113603125B (en) * | 2021-03-08 | 2023-02-28 | 台湾塑胶工业股份有限公司 | Calcined shellfish shell powder and its preparation method |
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