CN108101092A - A kind of preparation method of calcium carbonate rod-like nano particle package assembly - Google Patents

A kind of preparation method of calcium carbonate rod-like nano particle package assembly Download PDF

Info

Publication number
CN108101092A
CN108101092A CN201810115558.2A CN201810115558A CN108101092A CN 108101092 A CN108101092 A CN 108101092A CN 201810115558 A CN201810115558 A CN 201810115558A CN 108101092 A CN108101092 A CN 108101092A
Authority
CN
China
Prior art keywords
feed liquid
deionized water
calcium oxide
method described
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810115558.2A
Other languages
Chinese (zh)
Other versions
CN108101092B (en
Inventor
唐洁净
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Enping Huicheng New Material Co ltd
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201810115558.2A priority Critical patent/CN108101092B/en
Publication of CN108101092A publication Critical patent/CN108101092A/en
Application granted granted Critical
Publication of CN108101092B publication Critical patent/CN108101092B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/18Carbonates
    • C01F11/181Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/50Agglomerated particles
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A kind of preparation method of calcium carbonate rod-like nano particle package assembly, includes the following steps:Calcium oxide particle is scattered in deionized water, complexed surfactant is added in, stirs evenly, feed liquid is handled under microwave, and feed liquid introduces the liquid feeding end of atomizer, and carbon dioxide is introduced to the inlet end of atomizer, it under ultrasound condition, sprays, centrifuges to feed liquid, take clear liquid, high speed centrifugation, deionized water washing, again disperse in deionized water, strength combination of ultrasound centrifuge washing, is repeated 3 times, and obtains calcium carbonate rod-like nano particle package assembly.

Description

A kind of preparation method of calcium carbonate rod-like nano particle package assembly
Technical field
The invention belongs to calcium carbonate material preparation fields, and in particular to a kind of to prepare calcium carbonate rod-like nano particle assembling knot The method of structure.
Background technology
Calcium carbonate is widely used in the industries such as rubber, plastics, coating, papermaking, ink, crafty dose of glue, 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.
Calcium carbonate all will as a kind of important plastic filler, grain size, particle homogeneity, specific surface area and surface state The property of its compatibility high molecular with matrix and the mechanical property of filling-modified material is influenced, how easily to be disperseed, grain It is still the target pursued in industry to spend homogeneous, high surface activity nano-calcium carbonate and its package assembly.
The content of the invention
The technical scheme is that in order to overcome the shortcoming of prior art, propose a kind of to prepare that calcium carbonate is rodlike to be received The method of rice grain package assembly.
The present invention proposes a kind of preparation method of calcium carbonate rod-like nano particle package assembly, includes the following steps:
1) calcium oxide particle that grain size is 1-1.5 μm is scattered in deionized water, adds in complexed surfactant, stirring Uniformly;
2) feed liquid that step 1) obtains is handled into 40-50min under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary, obtain calcium carbonate rod-like nano particle;
5) disperse in deionized water again, strength combination of ultrasound centrifuge washing is repeated 3 times, obtains calcium carbonate rod-like nano Particle package assembly.
Wherein, the complexed surfactant is by dodecyl benzyl dimethyl ammonium chloride and dodecyl polyoxyethylene groups Amion acetic acid into.
Wherein, the power of microwave is 500-600W.
Wherein, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl polyoxyethylene groups amion acetic acid rub You are than being 1: 0.3-0.5: 0.2-0.5.
Wherein, in step 1), the mass ratio of calcium oxide and deionized water is 1: 250-400.
Wherein, in step 3), the charge ratio of feed liquid and carbon dioxide is 1g: 200-400mL.
Wherein, in step 4), it is 3000-5000rpm to control centrifuge RPMs.
Wherein, in step 3), ultrasonic power 150-200W.
Wherein, in step 4), high speed centrifugation revolution is 6000-8000rpm.
Wherein, in step 5), strength ultrasonic power is 450-650W.
The present invention makes calcium oxide surface layer constantly form calcium hydroxide simultaneously using the aquation of microwave condition control calcium oxide particle It is dissolved into aqueous solution, complexed surfactant is had an effect with calcium ion, and it is rodlike that it is induced to be formed in carburizing reagent Nano particle.By regulating and controlling microwave power and time, the speed of calcium oxide particle aquation in solution can be adjusted, and then is adjusted molten The concentration of calcium ion in liquid.Calcium hydroxide in solution is with carbon dioxide reaction under conditions of ullrasonic spraying, and feed liquid is in turbulent flow Under the conditions of by great amount of carbon dioxide gas impact, sweep along, minimum drop is separated by carbon dioxide under ultrasonication, ultrasound The moment that gas-liquid phase materials are promoted in contact reacts, and is conducive to avoid the reunion of particle during the reaction.Using Complexed surfactant is incorporated into particle surface, stable particle, avoid reunite while, induction calcium carbonate formed it is rodlike. Under the action of strength ultrasound, the energy that acoustic energy generates becomes minute bubbles intensive one by one by liquid medium, these are stingy Bubble is burst rapidly, and part surface activating agent is caused to come off from particle surface, particle surface energy is caused to rise, and then is assembled into porous Micron sphere.Due to primary granule size uniform, the two level package assembly size of formation is also more uniform.
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, obtained product particle size is more homogeneous.Microwave method activation combines instantaneous under ullrasonic spraying Reaction so that granule surface activity point is more, and reaction is fast, causes particle surface rough and uneven in surface, more identical size, the particle ratio of pattern Surface area significantly increases.The rodlike calcium carbonate that length is about 300-600nm is obtained, after assembled, forms about 6-11 microns more Hole chondritic.
Specific embodiment
With reference to embodiment, further illustrate the present invention.
Embodiment 1
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary, calcium carbonate rod-like nano particle is obtained, length is about 510nm, and particle is more homogeneous;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times, it is rodlike to obtain calcium carbonate The package assembly of nano particle.
Embodiment 2
1) calcium oxide particle that grain size is 1.5 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 400, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.5: 0.5;
2) feed liquid that step 1) obtains is handled into 50min, microwave power 600W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 400mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary, calcium carbonate rod-like nano particle is obtained, length is about 450nm, and particle is more homogeneous;
5) again in scattered and deionized water, 650W strength combination of ultrasound centrifuge washings are repeated 3 times, it is rodlike to obtain calcium carbonate The package assembly of nano particle.
Embodiment 3
1) calcium oxide particle that grain size is 2 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary, obtain calcium oxide/calcium carbonate core shell nanoparticles;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 4
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 150, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 5
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 500, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 6
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 400W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 7
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 700W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 8
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 30min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 9
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 100mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 10
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 500mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 11
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.1: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 12
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.7: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 13
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.1;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 14
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.7;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary;
5) again in scattered and deionized water, 450W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 15
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary, calcium carbonate rod-like nano particle is obtained, length is about 510nm, and particle is more homogeneous;
5) again in scattered and deionized water, 300W strength combination of ultrasound centrifuge washings are repeated 3 times.
Embodiment 16
1) calcium oxide particle that grain size is 1 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;Calcium oxide and the mass ratio of deionized water are 1: 250, calcium oxide and dodecyl benzyl dimethyl ammonium chloride, dodecyl The molar ratio of polyoxyethylene groups amion acetic acid is 1: 0.3: 0.2;
2) feed liquid that step 1) obtains is handled into 40min, microwave power 500W under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced atomizer Inlet end under ultrasound condition, sprays to feed liquid;The charge ratio of feed liquid and carbon dioxide is 1g: 200mL;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water washing 2-3 It is secondary, calcium carbonate rod-like nano particle is obtained, length is about 510nm, and particle is more homogeneous;
5) again in scattered and deionized water, 750W strength combination of ultrasound centrifuge washings.
The pattern for the product that embodiment 1-16 is obtained is shown in Table 1.
Table 1
Embodiment 17
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 counter current contacting.Product is obtained as the inhomogenous particle of size, it is assembled, only randomly reunited Body.

Claims (10)

1. a kind of preparation method of calcium carbonate rod-like nano particle package assembly, which is characterized in that include the following steps:
1) calcium oxide particle that grain size is 1-1.5 μm is scattered in deionized water, adds in complexed surfactant, stirring is equal It is even;
2) feed liquid that step 1) obtains is handled into 40-50min under microwave;
3) feed liquid for obtaining step 2) introduces the liquid feeding end of atomizer, and carbon dioxide is introduced to the air inlet of atomizer End, under ultrasound condition, sprays to feed liquid;
4) feed liquid after spraying is collected, controls the revolution of centrifugation, takes clear liquid, high speed centrifugation, deionized water is washed 2-3 times;
5) disperse in deionized water again, strength combination of ultrasound centrifuge washing is repeated 3 times, and obtains calcium carbonate rod-like nano particle Package assembly.
2. according to the method described in claim 1, it is characterized in that:The complexed surfactant is by dodecyl dimethyl benzyl Ammonium chloride and dodecyl polyoxyethylene groups amion acetic acid composition.
3. according to the method described in claim 1, it is characterized in that:The power of microwave is 500-600W.
4. according to the method described in claim 2, it is characterized in that:Calcium oxide and dodecyl benzyl dimethyl ammonium chloride, ten The molar ratio of dialkyl group polyoxyethylene groups amion acetic acid is 1: 0.3-0.5: 0.2-0.5.
5. 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 ∶250-400。
6. 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。
7. according to the method described in claim 1, it is characterized in that:In step 4), it is 3000-5000rpm to control centrifuge RPMs.
8. according to the method described in claim 1, it is characterized in that:In step 3), ultrasonic power 150-200W.
9. according to the method described in claim 1, it is characterized in that:In step 4), high speed centrifugation revolution is 6000-8000rpm.
10. according to the method described in claim 1, it is characterized in that:In step 5), strength ultrasonic power is 450-650W.
CN201810115558.2A 2018-01-28 2018-01-28 Preparation method of calcium carbonate rod-shaped nanoparticle assembly structure Active CN108101092B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810115558.2A CN108101092B (en) 2018-01-28 2018-01-28 Preparation method of calcium carbonate rod-shaped nanoparticle assembly structure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810115558.2A CN108101092B (en) 2018-01-28 2018-01-28 Preparation method of calcium carbonate rod-shaped nanoparticle assembly structure

Publications (2)

Publication Number Publication Date
CN108101092A true CN108101092A (en) 2018-06-01
CN108101092B CN108101092B (en) 2020-03-13

Family

ID=62221844

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810115558.2A Active CN108101092B (en) 2018-01-28 2018-01-28 Preparation method of calcium carbonate rod-shaped nanoparticle assembly structure

Country Status (1)

Country Link
CN (1) CN108101092B (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130164206A1 (en) * 2011-12-27 2013-06-27 Hankuk Paper Mfg, Co, Ltd. Calcium carbonate having a surface charge, the preparing process thereof and filler for producing a paper using the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130164206A1 (en) * 2011-12-27 2013-06-27 Hankuk Paper Mfg, Co, Ltd. Calcium carbonate having a surface charge, the preparing process thereof and filler for producing a paper using the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
聂颖等: ""纳米碳酸钙的生产工艺及改性技术进展"", 《化工文摘》 *
蒋惠亮等: ""表面活性剂对纳米碳酸钙结晶过程的影响"", 《日用化学工业》 *

Also Published As

Publication number Publication date
CN108101092B (en) 2020-03-13

Similar Documents

Publication Publication Date Title
CN104289161B (en) A kind of aluminium hydroxide microcapsule of melamine formaldehyde resin cladding and preparation method thereof
CN108299811A (en) A kind of preparation method of calcium carbonate rod-like nano particulate composite
CN105579478B (en) Prepare the method for toner and the integrated coagulator for this method
JP2980231B2 (en) Organic polymer-calcium carbonate composite particles, hollow calcium carbonate particles, methods for their preparation, their use as fillers or additives in plastics and elastomers
CN108689411A (en) A kind of preparation method of waterproof high tenacity porous silica
CN108101092A (en) A kind of preparation method of calcium carbonate rod-like nano particle package assembly
CN108358227A (en) A kind of preparation method of calcium carbonate bone rod-like nano particle package assembly
CN108190934A (en) A kind of preparation method of calcium carbonate rod-like nano particle
CN111017973B (en) Method for preparing hollow nano calcium carbonate by using ultrasonic aerosol
CN108101094A (en) A kind of preparation method of calcium oxide-calcium carbonate core shell nanoparticles package assembly
CN108328639A (en) A kind of preparation method of calcium carbonate bone rod-like nano particle
CN108264077A (en) A kind of preparation method of the core shell nanoparticles package assembly with calcium carbonate shell
CN108455643B (en) Preparation method of calcium carbonate dumbbell-shaped nanoparticle assembly structure
CN108455646A (en) A kind of preparation method of calcium carbonate bone rod-like nano particulate composite
CN108249466A (en) A kind of preparation method of calcium oxide-calcium carbonate core shell nanoparticles
CN108314072A (en) A kind of preparation method of the core shell nanoparticles with calcium carbonate shell
CN107117639B (en) A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nanometer package assembly
CN102910663A (en) Device for continuously preparing nano calcium carbonate
CN107188998A (en) A kind of preparation method of calcium carbonate/polymer core-shell structure
CN110862498A (en) Preparation method of asymmetric aminated silicon dioxide/phenolic resin composite particles
CN102963918B (en) Carbonation reaction method of nano calcium carbonate
CN205495554U (en) Receive particle ultrasonic atomization reaction unit a little
CN106268810A (en) A kind of surface recombination modifies particle aggregate carrier material and preparation method and application
CN110773079B (en) Method for preparing superfine powder balls by ultrasonic spraying method
CN107162033B (en) A kind of preparation method of vaterite-type calcium carbonate nano-particles self assemble film

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20230721

Address after: 529400 Workshop in Zone B, Dongjiao Industrial Zone, Hengpi Town, Enping City, Jiangmen City, Guangdong Province (information declaration system)

Patentee after: Enping Huicheng New Material Co.,Ltd.

Address before: 315400 room 315, 1 International Business Center, China Plastics City, Yuyao, Ningbo, Zhejiang

Patentee before: NINGBO PLASTIC METAL PRODUCT Co.,Ltd.