CN108358227B - Preparation method of calcium carbonate bone-rod-shaped nanoparticle assembly structure - Google Patents
Preparation method of calcium carbonate bone-rod-shaped nanoparticle assembly structure Download PDFInfo
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Abstract
A preparation method of a calcium carbonate bone-rod-shaped nanoparticle assembly structure comprises the following steps: dispersing calcium oxide particles in deionized water, adding a composite surfactant, uniformly stirring, treating feed liquid under microwave, introducing the feed liquid into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, spraying the feed liquid under an ultrasonic condition, performing centrifugal separation, taking clear liquid, performing high-speed centrifugation, washing with deionized water, re-dispersing in the deionized water, performing centrifugal washing by combining powerful ultrasound, and repeating for 3 times to obtain the calcium carbonate bone-rod-shaped nanoparticle assembly structure.
Description
Technical Field
The invention belongs to the field of calcium carbonate material preparation, and particularly relates to a method for preparing a calcium carbonate bone-shaped nanoparticle assembly structure.
Background
The calcium carbonate is widely used in the industries of rubber, plastics, coating, papermaking, printing ink, sizing agent DIAN, sealant and the like, and can also be applied to the industries of toothpaste, food, medicine, word materials, building materials, chemical fibers and the like. The crystal form of calcium carbonate includes three types of calcite, aragonite and vaterite, wherein the calcite structure is the most stable, and the aragonite and the vaterite are both unstable.
Calcium carbonate is an important plastic filler, the affinity of the calcium carbonate with a matrix macromolecule and the properties of the mechanical properties of filling modified materials are influenced by the particle size, the particle uniformity, the specific surface area and the surface state of the calcium carbonate, and how to obtain nano calcium carbonate which is easy to disperse, uniform in particle size and high in surface activity and an assembly structure of the nano calcium carbonate are still targets pursued in the industry.
Disclosure of Invention
The technical scheme of the invention is to overcome the defects of the prior art and provide a method for preparing a calcium carbonate bone-shaped nano particle assembly structure.
The invention provides a preparation method of a calcium carbonate bone-rod-shaped nano particle assembly structure, which comprises the following steps:
1) dispersing calcium oxide particles with the particle size of 1-1.5 mu m in deionized water, adding a composite surfactant, and uniformly stirring;
2) treating the feed liquid obtained in the step 1) for 40-50min under microwave;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) re-dispersing in deionized water, performing centrifugal washing in combination with powerful ultrasound, and repeating for 3 times to obtain the calcium carbonate bone-rod-shaped nanoparticle assembly structure.
Wherein the composite surfactant consists of dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl aminoacetic acid.
Wherein, the power of the microwave is 500-600W.
Wherein the mol ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3-0.5: 0.1-0.3.
Wherein, in the step 1), the mass ratio of the calcium oxide to the deionized water is 1: 250-400.
Wherein, in the step 3), the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200-400 mL.
Wherein, in the step 4), the centrifugal rotation speed is controlled to be 4000-6000 rpm.
Wherein, in the step 3), the ultrasonic power is 150-200W.
Wherein, in the step 4), the high-speed centrifugation rotation number is 8000-.
Wherein, in the step 5), the power of the powerful ultrasonic wave is 450-700W.
The invention adopts microwave condition to control the hydration of calcium oxide particles, so that calcium hydroxide is continuously formed on the surface layer of calcium oxide and is dissolved in aqueous solution, the composite surfactant reacts with calcium ions, and the calcium ions are induced to form bone-rod-shaped nano particles in carbonization reaction. By regulating and controlling the microwave power and time, the hydration speed of calcium oxide particles in the solution can be regulated, and further the concentration of calcium ions in the solution can be regulated. Calcium hydroxide in the solution reacts with carbon dioxide under the condition of ultrasonic spraying, feed liquid is impacted and wrapped by a large amount of carbon dioxide gas under the condition of turbulent flow and is dispersed into tiny liquid drops by the carbon dioxide under the action of ultrasonic, and the ultrasonic promotes the gas-liquid phase material to react at the moment of contact, and is favorable for avoiding the agglomeration of particles in the reaction process. The composite surfactant is combined on the surface of the particles, so that the particles are stabilized, agglomeration is avoided, and calcium carbonate is induced to form bone-shaped bars. Under the action of powerful ultrasound, energy generated by sound energy passes through a liquid medium to become dense small bubbles, the small bubbles are rapidly burst, partial surfactant is separated from the surface of particles, the surface energy of the particles is raised, and the particles are assembled into porous microspheres. Because the primary particles are uniform in size, the secondary assembly structure formed is also relatively uniform in size.
The invention has the beneficial effects that: the method adopts the carbon dioxide as the gas for feed liquid atomization, and compared with the method of contacting with the carbon dioxide after atomization, the particle size of the obtained product is more uniform. The microwave activation is combined with the instantaneous reaction under ultrasonic spraying, so that the active points on the surface of the particles are more, the reaction is fast, the surface of the particles is uneven, and the specific surface area of the particles with the same size and appearance is obviously increased. Obtaining bone-rod-shaped calcium carbonate with the length of about 80-120nm, and forming a porous spherical structure with the length of about 2-4 microns after assembling.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing with deionized water for 2-3 times to obtain calcium carbonate bone-rod-shaped nanoparticles with the length of about 115nm and uniform size;
5) re-dispersing in deionized water, performing 450W powerful ultrasonic combined centrifugal washing, and repeating for 3 times to obtain the calcium carbonate bone-rod-shaped nanoparticle assembly structure.
Example 2
1) Dispersing calcium oxide particles with the particle size of 1.5 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 400, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.5: 0.3;
2) treating the feed liquid obtained in the step 1) for 50min under microwave with the microwave power of 600W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 400 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing with deionized water for 2-3 times to obtain calcium carbonate bone-rod-shaped nanoparticles with the length of about 92nm and uniform size;
5) re-dispersing in deionized water, performing 700W powerful ultrasonic combined centrifugal washing, and repeating for 3 times to obtain the calcium carbonate bone-rod-shaped nanoparticle assembly structure.
Example 3
1) Dispersing calcium oxide particles with the particle size of 2 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at a high speed, and washing for 2-3 times by using deionized water to obtain calcium oxide/calcium carbonate core-shell nano particles;
5) re-dispersing in deionized water, carrying out centrifugal washing by combining 450W strong ultrasound, and repeating for 3 times to obtain the calcium oxide/calcium carbonate core-shell nanoparticle assembly structure.
Example 4
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 150, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 5
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 500, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 6
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave, wherein the microwave power is 400W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 7
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave, wherein the microwave power is 700W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 8
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 30min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 9
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 100 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 10
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 500 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 11
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 12
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.7: 0.1;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 13
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.05;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 14
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.5;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 450W strong ultrasonic combined centrifugal washing, repeat 3 times.
Example 15
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.5;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) redispersion in deionized water, 350W strong ultrasound combined with centrifugal washing, repeat 3 times.
Example 16
1) Dispersing calcium oxide particles with the particle size of 1 mu m in deionized water, adding a composite surfactant, and uniformly stirring; the mass ratio of the calcium oxide to the deionized water is 1: 250, and the molar ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3: 0.5;
2) treating the feed liquid obtained in the step 1) for 40min under microwave with the microwave power of 500W;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition; the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 mL;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) re-dispersing in deionized water, and performing 800W powerful ultrasonic combined centrifugal washing for 3 times.
The morphology of the products obtained in examples 1 to 16 is shown in Table 1.
TABLE 1
Example 17
The process and parameters of example 1 were used, and only the carrier gas for ultrasonic atomization in example 1 was replaced with nitrogen gas, and the atomized liquid was brought into countercurrent contact with carbon dioxide gas. The resulting product was spherical particles of non-uniform size, assembled to give only random agglomerates.
Claims (5)
1. The preparation method of the calcium carbonate bone-rod-shaped nanoparticle assembly structure is characterized by comprising the following steps of:
1) dispersing calcium oxide particles with the particle size of 1-1.5 mu m in deionized water, adding a composite surfactant, and uniformly stirring;
2) treating the feed liquid obtained in the step 1) for 40-50min under microwave;
3) introducing the feed liquid obtained in the step 2) into a liquid inlet end of an atomizing nozzle, introducing carbon dioxide gas into a gas inlet end of the atomizing nozzle, and spraying the feed liquid under an ultrasonic condition;
4) collecting the sprayed feed liquid, controlling the revolution of centrifugal separation, taking clear liquid, centrifuging at high speed, and washing for 2-3 times by using deionized water;
5) re-dispersing in deionized water, washing with powerful ultrasonic wave and centrifuging, and repeating for 3 times to obtain the calcium carbonate bone-rod-shaped nanoparticle assembly structure;
the composite surfactant consists of dodecyl dimethyl benzyl ammonium chloride and dodecyl dimethyl aminoacetic acid;
the mol ratio of the calcium oxide to the dodecyl dimethyl benzyl ammonium chloride and the dodecyl dimethyl aminoacetic acid is 1: 0.3-0.5: 0.1-0.3;
the power of the microwave is 500-600W;
in the step 3), the feeding ratio of the feed liquid to the carbon dioxide is 1 g: 200 and 400 mL;
in the step 3), the ultrasonic power is 150-.
2. The method of claim 1, wherein: in the step 1), the mass ratio of the calcium oxide to the deionized water is 1: 250-400.
3. The method of claim 1, wherein: in the step 4), the centrifugal rotation speed is controlled to be 4000-.
4. The method of claim 1, wherein: in step 4), the high-speed centrifugation rotation number is 8000- & lt12000 rpm.
5. The method of claim 1, wherein: in the step 5), the power of the powerful ultrasonic wave is 450-700W.
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