CN115744958A - Method for preparing calcium carbonate microspheres from artificial granite waste residues - Google Patents
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- CN115744958A CN115744958A CN202211567861.9A CN202211567861A CN115744958A CN 115744958 A CN115744958 A CN 115744958A CN 202211567861 A CN202211567861 A CN 202211567861A CN 115744958 A CN115744958 A CN 115744958A
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- calcium carbonate
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- granite waste
- carbonate microspheres
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 114
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 57
- 239000004005 microsphere Substances 0.000 title claims abstract description 45
- 239000002699 waste material Substances 0.000 title claims abstract description 42
- 239000010438 granite Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 25
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 20
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims abstract description 20
- 238000004945 emulsification Methods 0.000 claims abstract description 10
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims description 23
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000000839 emulsion Substances 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 229960002796 polystyrene sulfonate Drugs 0.000 claims description 12
- 239000011970 polystyrene sulfonate Substances 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 238000000967 suction filtration Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000000047 product Substances 0.000 abstract description 5
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 abstract description 2
- 239000011575 calcium Substances 0.000 abstract description 2
- 229910052791 calcium Inorganic materials 0.000 abstract description 2
- 229910001424 calcium ion Inorganic materials 0.000 abstract description 2
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 229920000620 organic polymer Polymers 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004579 marble Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000002969 artificial stone Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000009418 renovation Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for preparing calcium carbonate microspheres from artificial granite waste residues, which comprises the steps of removing a high-molecular organic polymer which does not react with dilute acid by acid dissolution and filtration, taking the artificial granite waste residues as a calcium source, taking calcium ions and carbonate ions to react to generate calcium carbonate precipitates as a main reaction, taking sodium polystyrene sulfonate as a template agent and sodium dodecyl sulfate as a surfactant, and regulating the shape and crystal form of calcium carbonate to obtain the calcium carbonate microspheres. The method combines the characteristics of a template method, an emulsion method and a double decomposition method, and has the advantages of low raw material cost, mild reaction conditions, simple equipment operation, good product regulation and control performance and the like.
Description
Technical Field
The invention relates to the technical field of inorganic functional materials and chemical materials, in particular to a method for preparing calcium carbonate microspheres by using waste residues of artificial granite.
Background
The artificial granite is also called synthetic stone, reconstructed stone and engineering stone. It is made up by using natural marble and stone powder as raw material, adding organic resin as cementing agent, vacuum stirring, high-pressure shaking and room-temp. solidifying and forming. More than 92 percent of the natural stone is marble, so that the natural stone has the characteristics of noble and elegant properties, bright color, uniform color, accurate size, high finish, compression resistance, wear resistance, good air permeability, environmental protection, multiple renovations and the like, and is an internationally popular green environment-friendly decorative material. Waste slurry can appear in the polishing process of the artificial granite, the waste slurry can be subjected to natural air drying to obtain artificial granite waste residue, the artificial granite waste residue is generally simply buried and stored in the open air by many large-scale enterprises, the artificial granite waste residue is not only polluted by the environment, but also wasted by resources, the surface area is occupied, a large amount of volatile organic matters are generated at the same time, secondary pollution is caused to the environment, the sustainable development of the enterprises is reduced, how to change waste into valuable is realized, a plurality of effective utilization methods of the artificial granite waste residue are provided through continuous exploration of a plurality of scientific research workers, and the reports about preparation of calcium carbonate microspheres by using the artificial granite waste residue as a raw material are rare.
The calcium carbonate microspheres have the following unique properties: small volume, large specific surface area, large porosity and the like, and is widely applied to the high-end field. As for the drug carrier, the sustained release property of the calcium carbonate can be utilized to achieve high-efficiency utilization of the drug, which greatly contributes to the treatment of diseases, and the calcium carbonate is an indispensable effective source for supplementing calcium ions to human bodies. The calcium carbonate microspheres can also be used as an adsorbent, porous calcium carbonate microspheres can be prepared by using a special means, and the product is used as the adsorbent, so that the investment is low, and the value is high. Besides the fields, the preparation can also be used in biotechnology, cosmetic industry and the like.
There are many main preparation methods of calcium carbonate microspheres, wherein the template method is a main method for preparing calcium carbonate microspheres commonly used by people; although the double decomposition method is simple, the product purity is low; the emulsion method has low energy consumption and good stability, but the molecular particles are large and the particle size is not easy to control; the sol-gel method has good molecular uniformity, good dispersibility and low reaction temperature, but the raw materials are expensive, long in time consumption and easy to deform; the hydrothermal method has rigorous reaction conditions, small preparation amount and difficult mass preparation; although the spray drying method contributes greatly in the field of preparing calcium carbonate microspheres, the equipment investment is large, and the cost is high. In addition, there are many methods such as carbonization, laser ablation, and the like.
Aiming at the defects that heavy calcium carbonate cannot be comprehensively utilized due to the fact that heavy calcium carbonate and an organic high molecular polymer in artificial granite waste residues are difficult to separate, and the organic high molecular polymer continuously emits volatile organic matters to pollute the environment and the like, the method utilizes the artificial granite waste residues as a calcium source, adds dilute nitric acid for reaction, filters and removes the high molecular polymer, enables filtrate to react with sodium carbonate to generate calcium carbonate precipitate as a main reaction, utilizes sodium polystyrene sulfonate as a template agent and sodium dodecyl sulfate as a surfactant, and regulates the morphology and the crystal form of the calcium carbonate, so that the calcium carbonate microspheres are obtained. Not only solves the problem of environmental pollution, but also makes a contribution to the calcium carbonate industrial chain. The method combines the characteristics of a template method, an emulsion method and a double decomposition method, and has the advantages of low raw material cost, mild reaction conditions, simple equipment operation, good product regulation and control performance and the like.
Disclosure of Invention
The invention aims to provide a method for preparing calcium carbonate microspheres by using artificial granite waste residues, which aims to overcome the defects of the prior art. The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a method for preparing calcium carbonate microspheres from waste residues of artificial granite is characterized by comprising the following steps:
a. weighing 5g of artificial granite waste residue, putting the artificial granite waste residue into a beaker, slowly adding the prepared nitric acid into the artificial granite waste residue, slightly stirring until no bubbles are generated, and performing suction filtration;
b. 0.5mL of n-hexane was measured and added to 99.5mL of deionized water to prepare 100mL of selective solvent, 0.3-0.7g of Sodium Dodecyl Sulfate (SDS) is weighed and dissolved in 100mL of selective solvent to obtain a mixed solution X; 3.18g of anhydrous sodium carbonate are weighed and prepared into 1mol/L Na in 30mL of deionized water 2 CO 3 Solution, 0.4-0.6g sodium polystyrene sulfonate (PSS) is weighed and added into Na 2 CO 3 And stirring the solution until the PSS is completely dissolved to obtain a mixed solution Y. Adding the mixed solution X into the mixed solution Y, and performing ultrasonic emulsification to obtain an emulsion;
c. pouring 50mL of the filtrate obtained in the step a into the emulsion obtained in the step b under the environment of a constant-temperature magnetic stirrer at the temperature of 60-80 ℃, and stirring and reacting for 20-40min to obtain a suspension; standing the suspension to room temperature, performing suction filtration, washing the filter cake with distilled water and hot ethanol for 3-5 times, and drying the filter cake in a drying oven at 60 ℃ for 6h to obtain white powder, namely the calcium carbonate microspheres.
The artificial granite waste residue is ball-milled and then sieved by a 200-mesh sieve;
the concentration of the nitric acid is 2-10%.
The invention has the beneficial effects that:
1. the waste artificial granite slag is comprehensively utilized, so that the environmental problem of the waste artificial granite slag can be solved;
2. the method combines the characteristics of a template method, an emulsion method and a double decomposition method, and has the advantages of low raw material cost, mild reaction conditions, simple equipment operation and the like;
3. the product has good regulation and control performance, and the prepared calcium carbonate microspheres have good appearance and round spheres.
Drawings
FIG. 1 is a scanning electron micrograph of the calcium carbonate microspheres of example 1.
FIG. 2 is a scanning electron micrograph of the calcium carbonate microspheres of example 2.
FIG. 3 is a scanning electron micrograph of the calcium carbonate microspheres of example 3.
FIG. 4 is a scanning electron micrograph of the calcium carbonate microspheres of example 4.
FIG. 5 is a partially enlarged SEM image of the calcium carbonate microspheres of example 4.
FIG. 6 is an X-ray diffraction pattern of calcium carbonate microspheres from example 4.
Detailed Description
The following further details the embodiments of the invention: it should be emphasized that the embodiments described herein are illustrative rather than restrictive, and thus the present invention is not limited to the embodiments described in the detailed description, but other embodiments derived from the technical solutions of the present invention by those skilled in the art are also within the scope of the present invention.
Example 1
a. Weighing 5g of artificial granite waste residue which is ball-milled and sieved by a 200-mesh sieve, putting the artificial granite waste residue into a beaker, slowly adding the prepared 5% nitric acid into the artificial granite waste residue, slightly stirring until no bubbles are generated, and performing suction filtration;
b. weighing 0.5mL of n-hexane, adding the n-hexane into 99.5mL of deionized water to prepare 100mL of selective solvent, weighing 0.3g of Sodium Dodecyl Sulfate (SDS), and dissolving the Sodium Dodecyl Sulfate (SDS) in 100mL of selective solvent to obtain a mixed solution X; 3.18g of anhydrous sodium carbonate are weighed and prepared into 1mol/L Na in 30mL of deionized water 2 CO 3 Solution 0.5g of sodium polystyrene sulfonate (PSS) was weighed into Na 2 CO 3 And stirring the solution until the PSS is completely dissolved to obtain a mixed solution Y. Adding the mixed solution X into the mixed solution Y, and performing ultrasonic emulsification to obtain an emulsion;
c. pouring 50mL of the filtrate obtained in the step a into the emulsion obtained in the step b under the environment of a constant-temperature magnetic stirrer at the temperature of 60 ℃, and stirring and reacting for 20min to obtain a suspension; standing the suspension to room temperature, performing suction filtration, washing the filter cake with distilled water and hot ethanol for 3-5 times, and drying the filter cake in a drying oven at 60 ℃ for 6h to obtain white powder, namely the calcium carbonate microspheres. FIG. 1 is a scanning electron microscope image of the calcium carbonate microspheres of example 1, which are spherical in shape.
Example 2
a. Weighing 5g of artificial granite waste residue which is ball-milled and sieved by a 200-mesh sieve, putting the artificial granite waste residue into a beaker, slowly adding the prepared 5% nitric acid into the artificial granite waste residue, slightly stirring until no bubbles are generated, and performing suction filtration;
b. weighing 0.5mL of n-hexane, adding 99.5mL of deionized water to obtain 100mL of selective solvent, weighing 0.3g of Sodium Dodecyl Sulfate (SDS), and dissolving in 100mL of selective solvent to obtain a mixtureMixing the solution X; 3.18g of anhydrous sodium carbonate are weighed and prepared into 1mol/L Na in 30mL of deionized water 2 CO 3 Solution 0.5g of sodium polystyrene sulfonate (PSS) was weighed into Na 2 CO 3 And stirring the solution until the PSS is completely dissolved to obtain a mixed solution Y. Adding the mixed solution X into the mixed solution Y, and performing ultrasonic emulsification to obtain an emulsion;
c. pouring 50mL of the filtrate obtained in the step a into the emulsion obtained in the step b under the environment of a constant-temperature magnetic stirrer at 70 ℃, and reacting for 20min under stirring to obtain a suspension; standing the suspension to room temperature, performing suction filtration, washing the filter cake with distilled water and hot ethanol for 3-5 times, and drying the filter cake in a drying oven at 60 ℃ for 6h to obtain white powder, namely the calcium carbonate microspheres. FIG. 2 is a scanning electron micrograph of the calcium carbonate microspheres of example 2, which are spherical in shape.
Example 3
a. Weighing 5g of artificial granite waste residue which is ball-milled and then sieved by a 200-mesh sieve, putting the artificial granite waste residue into a beaker, slowly adding prepared 10% nitric acid into the artificial granite waste residue, slightly stirring until no bubbles are generated, and performing suction filtration;
b. weighing 0.5mL of n-hexane, adding the n-hexane into 99.5mL of deionized water to prepare 100mL of selective solvent, weighing 0.5g of Sodium Dodecyl Sulfate (SDS), and dissolving the SDS in 100mL of selective solvent to obtain a mixed solution X; 3.18g of anhydrous sodium carbonate are weighed into 30mL of deionized water to prepare 1mol/L Na 2 CO 3 Solution, 0.4-0.6g sodium polystyrene sulfonate (PSS) is weighed and added into Na 2 CO 3 And stirring the solution until the PSS is completely dissolved to obtain a mixed solution Y. Adding the mixed solution X into the mixed solution Y, and performing ultrasonic emulsification to obtain an emulsion;
c. pouring 50mL of the filtrate obtained in the step a into the emulsion obtained in the step b under the environment of a constant-temperature magnetic stirrer at 70 ℃, and reacting for 40min under stirring to obtain a suspension; standing the suspension to room temperature, performing suction filtration, washing the filter cake with distilled water and hot ethanol for 3-5 times, and drying the filter cake in a drying oven at 60 ℃ for 6h to obtain white powder, namely the calcium carbonate microspheres. FIG. 3 is a scanning electron micrograph of the calcium carbonate microspheres of example 3, which are spherical in shape.
Example 4
a. Weighing 5g of artificial granite waste residue which is ball-milled and then sieved by a 200-mesh sieve, putting the artificial granite waste residue into a beaker, slowly adding 10% nitric acid into the artificial granite waste residue, slightly stirring until no bubbles are generated, and performing suction filtration;
b. weighing 0.5mL of n-hexane, adding the n-hexane into 99.5mL of deionized water to prepare 100mL of selective solvent, weighing 0.5g of Sodium Dodecyl Sulfate (SDS), and dissolving the SDS in 100mL of selective solvent to obtain a mixed solution X; 3.18g of anhydrous sodium carbonate are weighed into 30mL of deionized water to prepare 1mol/L Na 2 CO 3 Solution 0.5g of sodium polystyrene sulfonate (PSS) was weighed into Na 2 CO 3 And stirring the solution until the PSS is completely dissolved to obtain a mixed solution Y. Adding the mixed solution X into the mixed solution Y, and performing ultrasonic emulsification to obtain an emulsion;
c. pouring 50mL of the filtrate obtained in the step a into the emulsion obtained in the step b under the environment of a constant-temperature magnetic stirrer at 70 ℃, and stirring and reacting for 30min to obtain a suspension; standing the suspension to room temperature, performing suction filtration, washing the filter cake with distilled water and hot ethanol for 3-5 times, and drying the filter cake in a drying oven at 60 ℃ for 6h to obtain white powder, namely the calcium carbonate microspheres. Fig. 4 is a scanning electron micrograph of the calcium carbonate microspheres of example 4, and fig. 5 is a partial enlarged view of the calcium carbonate microspheres of example 4. From fig. 4, it can be seen that the prepared calcium carbonate microspheres have a round surface, a good dispersion degree and a uniform size, and from the enlarged view of the calcium carbonate microspheres in fig. 5, the spherical surfaces of the calcium carbonate microspheres are formed by aggregation of nano calcium carbonate, the spherical surfaces are round, and the average particle size is about 5 μm. The calcium carbonate microspheres of example 4 were subjected to a particle size test, D of the calcium carbonate microspheres 50 Is 4.71 μm, D 90 The particle size of the calcium carbonate microspheres is 12.28 micrometers, namely the average particle size of the prepared calcium carbonate microspheres is 4.71 micrometers, which is consistent with the particle size analyzed by a scanning electron microscope.
FIG. 6 is an X-ray diffraction pattern of the calcium carbonate microspheres of example 4. As can be seen from fig. 6, 20.8 °, 24.76 °, 26.96 °, 32.6 °, 43.76 °, 49.84 ° and 55.6 ° are the characteristic peaks of the vaterite-type calcium carbonate, and the peaks have sharp shapes, indicating good crystallinity, indicating that the prepared calcium carbonate microspheres are the vaterite-type calcium carbonate.
Claims (3)
1. A method for preparing calcium carbonate microspheres from waste residues of artificial granite is characterized by comprising the following steps:
a. weighing 5g of artificial granite waste residue, putting the artificial granite waste residue into a beaker, slowly adding the prepared nitric acid into the artificial granite waste residue, slightly stirring until no bubbles are generated, and performing suction filtration;
b. weighing 0.5mL of n-hexane, adding the n-hexane into 99.5mL of deionized water to prepare 100mL of selective solvent, weighing 0.3-0.7g of Sodium Dodecyl Sulfate (SDS), and dissolving the Sodium Dodecyl Sulfate (SDS) in 100mL of selective solvent to obtain a mixed solution X; 3.18g of anhydrous sodium carbonate are weighed and prepared into 1mol/L Na in 30mL of deionized water 2 CO 3 Solution, 0.4-0.6g sodium polystyrene sulfonate (PSS) is weighed and added into Na 2 CO 3 And stirring the solution until the PSS is completely dissolved to obtain a mixed solution Y. Adding the mixed solution X into the mixed solution Y, and performing ultrasonic emulsification to obtain an emulsion;
c. pouring 50mL of the filtrate obtained in the step a into the emulsion obtained in the step b under the environment of a constant-temperature magnetic stirrer at the temperature of 60-80 ℃, and stirring and reacting for 20-40min to obtain a suspension; standing the suspension to room temperature, performing suction filtration, washing the filter cake with distilled water and hot ethanol for 3-5 times, and drying the filter cake in a drying oven at 60 ℃ for 6h to obtain white powder, namely the calcium carbonate microspheres.
2. The method for preparing calcium carbonate microspheres from artificial granite waste residues as claimed in claim 1, wherein the artificial granite waste residues in step a are ball-milled and sieved with a 200-mesh sieve.
3. The method for preparing calcium carbonate microspheres from artificial granite waste residues as claimed in claim 1, wherein the nitric acid concentration in step a is 2-10%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992374A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Preparation method of calcium carbonate micro-spheres |
| CN103232051A (en) * | 2013-04-24 | 2013-08-07 | 陕西科技大学 | Preparation method of ultrafine porous calcium carbonate microsphere |
| CN105329929A (en) * | 2015-12-15 | 2016-02-17 | 浙江理工大学 | Spherical calcium carbonate particles and preparation method thereof |
| CN105502463A (en) * | 2015-12-28 | 2016-04-20 | 中南大学 | Preparation method of hollow calcium carbonate microspheres of micro-scale and nano-scale pore structures |
| CN110902708A (en) * | 2019-12-13 | 2020-03-24 | 贺州学院 | Method for preparing nano calcium carbonate by using artificial granite waste residues |
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2022
- 2022-12-07 CN CN202211567861.9A patent/CN115744958A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992374A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Preparation method of calcium carbonate micro-spheres |
| CN103232051A (en) * | 2013-04-24 | 2013-08-07 | 陕西科技大学 | Preparation method of ultrafine porous calcium carbonate microsphere |
| CN105329929A (en) * | 2015-12-15 | 2016-02-17 | 浙江理工大学 | Spherical calcium carbonate particles and preparation method thereof |
| CN105502463A (en) * | 2015-12-28 | 2016-04-20 | 中南大学 | Preparation method of hollow calcium carbonate microspheres of micro-scale and nano-scale pore structures |
| CN110902708A (en) * | 2019-12-13 | 2020-03-24 | 贺州学院 | Method for preparing nano calcium carbonate by using artificial granite waste residues |
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