CN114671449B - Synthesis method of hollow calcium hydroxide microspheres - Google Patents
Synthesis method of hollow calcium hydroxide microspheres Download PDFInfo
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- CN114671449B CN114671449B CN202210442955.7A CN202210442955A CN114671449B CN 114671449 B CN114671449 B CN 114671449B CN 202210442955 A CN202210442955 A CN 202210442955A CN 114671449 B CN114671449 B CN 114671449B
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- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 title claims abstract description 36
- 239000000920 calcium hydroxide Substances 0.000 title claims abstract description 36
- 229910001861 calcium hydroxide Inorganic materials 0.000 title claims abstract description 36
- 239000004005 microsphere Substances 0.000 title claims abstract description 18
- 238000001308 synthesis method Methods 0.000 title claims abstract description 7
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 claims abstract description 52
- 239000011724 folic acid Substances 0.000 claims abstract description 27
- 235000019152 folic acid Nutrition 0.000 claims abstract description 27
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229960000304 folic acid Drugs 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000010431 corundum Substances 0.000 claims abstract description 6
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229940079593 drug Drugs 0.000 claims description 4
- 239000003814 drug Substances 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 239000000706 filtrate Substances 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 3
- 239000011363 dried mixture Substances 0.000 abstract 2
- 239000000126 substance Substances 0.000 abstract 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 abstract 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 1
- 239000000969 carrier Substances 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000012847 fine chemical Substances 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000011575 calcium Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 229940014144 folate Drugs 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 208000032005 Spinocerebellar ataxia with axonal neuropathy type 2 Diseases 0.000 description 1
- 208000033361 autosomal recessive with axonal neuropathy 2 spinocerebellar ataxia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- 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
- C01F11/04—Oxides or hydroxides by thermal decomposition
- C01F11/06—Oxides or hydroxides by thermal decomposition of carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2004/34—Spheres hollow
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for synthesizing hollow calcium hydroxide microspheres, which comprises the steps of firstly weighing corresponding anhydrous calcium chloride, anhydrous sodium carbonate and folic acid, mixing the weighed substances, respectively and uniformly mixing the substances in a beaker with water, placing the mixture in a polytetrafluoroethylene reaction kettle, placing the mixture in an oven, heating the mixture under the air condition for reaction for 12 hours at 200 ℃, cooling the mixture to room temperature, taking out the mixture, filtering the mixture for washing, drying the mixture, placing the dried mixture in a corundum crucible, roasting the dried mixture for 2 hours at the temperature of 800 ℃ in the air atmosphere, naturally cooling the mixture to room temperature, taking out the mixture, and uniformly grinding the mixture to obtain white powder. The hollow calcium hydroxide microsphere prepared by the method overcomes the defect of single structure of the traditional calcium hydroxide product, and utilizes folic acid as a template and CO 3 2‑ The hollow structure calcium hydroxide microsphere is prepared by a temperature treatment method, the synthesis method is simple and easy to implement, and the product has potential application value in the aspect of high-end application of powder, particularly fine chemical engineering and medical particle carriers.
Description
Technical Field
The invention belongs to the field of powder material synthesis, and particularly relates to a method for synthesizing a functional powder material by inducing precipitation reaction.
Background
Calcium hydroxide is used as an inorganic filler with the highest cost performance, and plays an important role in the preparation of materials such as plastics, papermaking, pharmacy, metallurgy, cement, putty powder, composite boards and the like. In addition, in some filling material application occasions with higher added values, such as health care products, tires, medicines and the like, the general calcined calcium hydroxide is difficult to meet the application requirements, and the structure and the morphology of the calcined calcium hydroxide are required to be modified to adapt to the application field with higher end, so that the added value is improved.
Therefore, by combining the factors, the hollow-structure calcium hydroxide microsphere is synthesized through the induced precipitation reaction, and the transition of calcium hydroxide from solid to hollow structure is realized through the adjustment of the folic acid template.
Disclosure of Invention
The invention aims to overcome the defect of single morphology and structure of the existing calcium hydroxide, and provides a method for preparing hollow-structure calcium hydroxide microspheres by using an induced precipitation method.
The invention provides a synthesis method of hollow calcium hydroxide microspheres, which is characterized by comprising the following steps:
1. the synthesis method of the hollow calcium hydroxide microsphere is characterized by comprising the following steps of:
a. weighing a certain amount of analytically pure CaCl 2 And Na (Na) 2 CO 3 Placing the medicines into beakers respectively, weighing analytically pure folic acid powder with the same mass respectively, placing into the two beakers respectively, adding deionized water with the same volume respectively, performing ultrasonic dispersion for 10 minutes, and then adding Na into the beakers respectively 2 CO 3 And folic acid in water are rapidly poured into CaCl 2 And folic acid water solution in a beaker, shaking and mixing uniformly, and standing and reacting for 30 minutes. Then mixTransferring the mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 12 hours at 200 ℃, naturally cooling, taking out, filtering at normal pressure, washing filter residues with deionized water for three times, washing with ethanol for three times, and drying at 80 ℃ for 12 hours to obtain a precursor mixture.
b. And mixing the precursors, taking out, and putting the mixture into an agate mortar for grinding uniformly for 5 minutes. And (3) placing the ground precursor in a corundum crucible, placing in a muffle furnace, reacting for 2 hours at 800 ℃ in an air atmosphere, cooling to room temperature, and taking out and grinding uniformly to obtain the hollow-structure calcium hydroxide microspheres.
Preferably, the amount of analytically pure Ca as described in step a 2 Cl 2 、Na 2 CO 3 And folic acid in the mass ratio of: (0.1110-0.6660): (0.106-0.6360): (0.0025 to 0.3).
Preferably, the precursor treatment is performed by hydrothermal treatment at 200 ℃ for 12 hours in the step a, wherein the heating system is 100 ℃ to 1h to 200 ℃ to 12h to finish.
Preferably, the atmosphere air atmosphere described in step b.
c. And mixing the precursors, taking out, and putting the mixture into an agate mortar for grinding uniformly for 5 minutes. And (3) placing the ground precursor into a corundum crucible, placing into a muffle furnace, reacting for 2 hours at 800 ℃ in an air atmosphere, cooling to room temperature, and taking out and grinding uniformly to obtain white powder.
A synthesis method of hollow calcium hydroxide microspheres is characterized in that the hollow calcium hydroxide microspheres are white powder.
The beneficial effects of the invention are as follows: the hollow structure calcium hydroxide microsphere prepared by the method overcomes the defect of single structure of the traditional calcium hydroxide product, and takes folic acid as a template and CO 3 2- The method for inducing precipitation is characterized in that hollow-structure calcium hydroxide microspheres are prepared by a temperature treatment method, and the crystal structure of the prepared white powder is the same as the crystal configuration of hexagonal biological calcium hydroxide by X-ray diffraction (XRD) detection. In the folic acid added sample, caCl is maintained 2 The mass of the catalyst is 0.1110g (0.001 mol) and Na 2 CO 3 Mass of 0.1060 (0.001 mol)Under the condition that the addition amount of folic acid is increased, the hollow structure of the obtained calcium hydroxide is gradually obvious, when the addition amount reaches 0.1000g, the hollow structure of the obtained calcium hydroxide is most obvious, the distribution of the calcium hydroxide presenting the hollow structure is the most, and when the addition amount exceeds 0.1000g, the hollow structure is gradually not obvious. When CaCl was changed while folic acid was added to maintain 0.1000g 2 And Na (Na) 2 CO 3 When the mass of the calcium hydroxide powder is respectively from 0.1110g and 0.1060g to 0.6660g and 0.6360g, the morphology of the obtained product is gradually approaching to a cube, and the spherical structure gradually collapses to form non-hollow calcium hydroxide particles with larger particles. The added folic acid can prevent and relieve the decomposition of calcium hydroxide, and the folic acid template is gradually burnt out after the heating time exceeds 2 hours, ca (OH) 2 Is calcined to calcium oxide.
Drawings
FIG. 1 is a different CaCl 2 、Na 2 CO 3 And a sample XRD pattern of folic acid feed ratio.
FIG. 2 is an XRD pattern for a sample after calcination at 800℃for 6 hours.
FIG. 3 is a different CaCl 2 、Na 2 CO 3 And SEM images of samples of folic acid feed ratio.
Detailed Description
The following examples are only some, but not all, of the examples of the invention. The embodiments of the invention generally described and illustrated herein may be arranged and designed in a wide variety of different configurations, and thus the detailed description of the embodiments of the invention provided below is not intended to limit the scope of the invention as claimed, but merely represent selected embodiments of the invention, based on which all other embodiments that a person skilled in the art would attain without inventive effort are within the scope of the invention.
Examples 1 to 16
Weighing medicines according to the raw material ratio of the table 1, adding water into beakers with the marks of A and B respectively, mixing uniformly for 10 minutes by ultrasonic treatment, pouring the liquid in the beaker B into the beaker A, standing for 30 minutes, transferring into a polytetrafluoroethylene reaction kettle, reacting for 12 hours at 200 ℃, wherein the heating system is 100 ℃ to 1h to 200 ℃ to 12h, finishing, naturally cooling, filtering at normal pressure, washing with deionized water for three times, washing with ethanol for three times, and drying filter residues at 80 ℃ for 12 hours to obtain a tan precursor mixture; the precursor mixture was taken out and put into an agate mortar for grinding uniformly for 5 minutes. And (3) placing the ground precursor into a corundum crucible, placing the corundum crucible into a muffle furnace, reacting for 2 hours and 6 hours at 800 ℃ in an air atmosphere, cooling to room temperature, and taking out and grinding uniformly to obtain white powder.
TABLE 1 raw material proportions
XRD tests were performed on the samples of examples 1 to 16, respectively, with a scan 2 theta angle set in the range of 5 DEG to 80 DEG and a scan step size of 20 DEG/min. The data from the test were compared to a standard spectrum using MDI Jade 5.0 software. The effect of different feed qualities on the crystal structure was tested, the XRD patterns of samples prepared with different feed qualities are shown in FIG. 1, and the XRD patterns of samples with calcination time of 6 hours are shown in FIG. 2.
FIG. 1 shows XRD patterns of samples of examples 1 to 15, and it is understood from FIG. 1 that, when the synthesis of the samples is carried out according to the charged mass of Table 1, the sample No. 1, except for the sample to which folic acid was not added, is CaCO due to the shorter heating schedule 3 The white powder sample prepared according to the feeding of the numbers 2-15 is completely matched with the standard calcium hydroxide spectrogram, and the card number of the standard spectrogram is marked as PDF 44-1481. The prepared samples of examples No. 2-15 belong to hexagonal systems and the XRD spectrum and Ca (OH) of the samples are analyzed by Jade 5.0 crystal analysis software 2 Is in conformity with the standard spectrogram of (c). The XRD pattern in fig. 2 shows that after 6 hours of calcination, the template formed by folic acid in the sample is burned out and the sample becomes calcium oxide.
SEM tests were carried out on the samples of examples 1 to 15, respectively, with a scanning voltage of 5kV. Testing the effect of different feeding quality on the morphology and structure of calcium carbonateSEM images of samples prepared with different dosing quality are shown in fig. 3. As can be seen from SEM images of samples No. 1-8 in the scanning electron microscope image, in the process of adding folic acid from 0g to 0.1000g, the hollow spherical structure of the sample is gradually obvious, the particle size distribution is about 15 μm, and the combined Ca is formed along with the increase of the adding amount 2+ The bonding effect between the folic acid templates is gradually enhanced, the distribution of the induced calcium hydroxide interlayer is gradually obvious, and the hollow structure formed during the temperature treatment is gradually obvious. As the folate template increases, as in samples No. 9 and No. 10 of FIG. 3, the more the folate template increases, the more pronounced the globular structure that forms. Comparing the scanning electron microscope images of 8,11,12,13,14,15 samples, the result shows that under the condition that the addition amount of the fixed folic acid is 0.1000g, the CaCl is added 2 And Na (Na) 2 CO 3 The hollow structure of the sample gradually decreases, exhibiting a relatively fine lamellar distribution, because with CaCl 2 And Na (Na) 2 CO 3 Increase in Ca 2+ The template formed by folic acid is far smaller than CaCl 2 With Na and Na 2 CO 3 The cubic calcium carbonate structure is dominant at this time, and at the time of calcination, the calcium carbonate without interlayer distribution is calcined into calcium hydroxide without hollow structure, and the sample No. 14 in fig. 3 is particularly excellent.
Claims (3)
1. The synthesis method of the hollow calcium hydroxide microsphere is characterized by comprising the following steps of:
a. weighing a certain amount of analytically pure CaCl 2 、Na 2 CO 3 Folic acid, said amount of analytically pure CaCl 2 、Na 2 CO 3 The mass ratio of folic acid is as follows: (0.1110-0.6660): (0.1060-0.6360): (0.0025-0.3000) CaCl 2 And Na (Na) 2 CO 3 Respectively placing into two different beakers, respectively adding folic acid powder with the same mass, respectively injecting water with the same volume, respectively dispersing with ultrasound for the same time to uniformly mix the medicines in the beakers, mixing Na 2 CO 3 Rapidly pouring aqueous solution of folic acid into CaCl 2 In aqueous solution of leaf acid, stand for 30 minThen placing the mixed solution into a hydrothermal reaction kettle for reaction for 12 hours at 200 ℃, naturally cooling, filtering at normal pressure, washing with water for three times, washing with alcohol for three times, and keeping the obtained filtrate at constant temperature in an oven at 80 ℃ for 12 hours to obtain a calcium hydroxide precursor mixture;
b. and taking out the precursor mixture, putting the precursor mixture into an agate mortar for grinding uniformly for 10 minutes, putting the ground precursor into a corundum crucible, reacting for 2 hours at 800-810 ℃ in air atmosphere, cooling to room temperature, taking out and grinding uniformly to obtain the white powder of the hollow calcium hydroxide microspheres.
2. The method of claim 1, wherein the precursor synthesis is performed by reacting at 200 ℃ for 12 hours in step a, and the heating schedule is 100 ℃ -1 h- →200 ℃ -12 h- →end.
3. The method of synthesizing hollow calcium hydroxide microspheres according to claim 1, wherein the hollow calcium hydroxide microspheres are white powder.
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| CN114671449B true CN114671449B (en) | 2023-08-25 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB713853A (en) * | 1950-11-30 | 1954-08-18 | Upjohn Co | Purification of synthetic folic acid |
| JP2005281034A (en) * | 2004-03-29 | 2005-10-13 | Nagoya Kogyo Univ | Hollow/spherical calcium carbonate particles and method for manufacturing the same |
| 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 |
| CN106604891A (en) * | 2014-07-31 | 2017-04-26 | 艾玛菲克有限公司 | Non-aqueous liquid and semi-solid formulations of amorphous calcium carbonate |
| CN108291096A (en) * | 2015-12-01 | 2018-07-17 | 欧米亚国际集团 | Method for producing the pellet for including the calcium carbonate reacted through surface |
| CN111453754A (en) * | 2020-04-28 | 2020-07-28 | 广西夏阳环保科技有限公司 | Preparation method of high-purity and high-activity nano calcium carbonate |
| CN113716594A (en) * | 2021-08-27 | 2021-11-30 | 杭州师范大学 | Preparation method of hollow calcium carbonate nanoparticles and double-additive mediated hollow calcium carbonate nanoparticles |
-
2022
- 2022-04-26 CN CN202210442955.7A patent/CN114671449B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB713853A (en) * | 1950-11-30 | 1954-08-18 | Upjohn Co | Purification of synthetic folic acid |
| JP2005281034A (en) * | 2004-03-29 | 2005-10-13 | Nagoya Kogyo Univ | Hollow/spherical calcium carbonate particles and method for manufacturing the same |
| CN106604891A (en) * | 2014-07-31 | 2017-04-26 | 艾玛菲克有限公司 | Non-aqueous liquid and semi-solid formulations of amorphous calcium carbonate |
| CN108291096A (en) * | 2015-12-01 | 2018-07-17 | 欧米亚国际集团 | Method for producing the pellet for including the calcium carbonate reacted through surface |
| 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 |
| CN111453754A (en) * | 2020-04-28 | 2020-07-28 | 广西夏阳环保科技有限公司 | Preparation method of high-purity and high-activity nano calcium carbonate |
| CN113716594A (en) * | 2021-08-27 | 2021-11-30 | 杭州师范大学 | Preparation method of hollow calcium carbonate nanoparticles and double-additive mediated hollow calcium carbonate nanoparticles |
Non-Patent Citations (1)
| Title |
|---|
| pH敏感性叶酸修饰羧甲基壳聚糖/CaCO_3混合纳米球作为药物载体的研究;刘举慧;赵峰;郭建峰;;现代化工(04);全文 * |
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Application publication date: 20220628 Assignee: Guangxi Hezhou Asia Pacific powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046438 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 Application publication date: 20220628 Assignee: Guangxi Hezhou Kewei New Material Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046408 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 Application publication date: 20220628 Assignee: Guangxi Hezhou Jinlong Powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046406 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 Application publication date: 20220628 Assignee: Hezhou Xinhua hair powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046344 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 Application publication date: 20220628 Assignee: Hezhou Guangli powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046341 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 Application publication date: 20220628 Assignee: Hezhou Fuyuan Powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046335 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 Application publication date: 20220628 Assignee: Hezhou Zhaojun Chemical Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046442 Denomination of invention: A Synthesis Method of Hollow Calcium Hydroxide Microspheres Granted publication date: 20230825 License type: Common License Record date: 20231108 |