CN111592026A - Preparation method of discus-shaped micron calcium carbonate - Google Patents
Preparation method of discus-shaped micron calcium carbonate Download PDFInfo
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- CN111592026A CN111592026A CN202010394156.8A CN202010394156A CN111592026A CN 111592026 A CN111592026 A CN 111592026A CN 202010394156 A CN202010394156 A CN 202010394156A CN 111592026 A CN111592026 A CN 111592026A
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- calcium carbonate
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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 92
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 12
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 12
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000004064 cosurfactant Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 14
- 239000001110 calcium chloride Substances 0.000 claims description 9
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 9
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000008346 aqueous phase Substances 0.000 claims description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000003973 paint Substances 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000000945 filler Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 241000950638 Symphysodon discus Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- HOQADATXFBOEGG-UHFFFAOYSA-N isofenphos Chemical compound CCOP(=S)(NC(C)C)OC1=CC=CC=C1C(=O)OC(C)C HOQADATXFBOEGG-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/184—Preparation of calcium carbonate by carbonation of solutions based on non-aqueous solvents
-
- 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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- 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)
Abstract
The invention belongs to the field of calcium carbonate preparation, and particularly relates to a preparation method of discus-shaped micron calcium carbonate. The method comprises the following steps: 1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant according to a volume ratio to prepare clear reverse microemulsion; 2) preparation of discus-shaped micron calcium carbonate: and (2) introducing carbon dioxide into the reversed-phase microemulsion obtained in the step 1) under the stirring state for reacting for a certain time until no precipitate is generated, stopping introducing carbon dioxide gas, ending stirring, standing at room temperature, aging, performing centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate. The method has the advantages of high safety performance, simplicity, reasonableness, low energy consumption, easily obtained raw materials and low price, and the discus-shaped micron calcium carbonate belongs to light calcium carbonate, has good particle size distribution and stability and good dispersity and can be used as a filler for rubber, plastics, papermaking, paint, ink and the like.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of calcium carbonate preparation, and particularly relates to a preparation method of discus-shaped micron calcium carbonate.
[ background of the invention ]
Calcium carbonate is an important inorganic chemical product and is widely used in the industries of rubber, plastics, printing ink, coating, paper making and the like. In particular to micro-nano calcium carbonate which is used for rubber, paper making, plastics and the like and can ensure that products have bright surface, large tensile strength, high tensile strength, good bending resistance, good cracking resistance and the like. The ink has the characteristics of good gloss, transparency, stability, quick drying and the like in high-grade ink. In the paint industry, the paint is mainly used for synthetic resin paint, automobile paint and the like, improves the thixotropy of a system, can obviously improve the adhesive force, the washing resistance and the stain resistance of the paint, and has good anti-settling effect; the paint has many excellent functions such as strong adhesion, impact resistance, scratch resistance, firmness and durability when added into the automobile chassis paint. In the industry of sealing and bonding materials, the cross-linking reaction of the glue can be accelerated, the stability of the glue is enhanced, the mechanical property of the glue is improved, the dual functions of filling and reinforcing are achieved, and the surface of the glue material is bright and fine. In the production of micro-nano calcium carbonate, the size, the crystal shape, the particle size distribution and the dispersion performance of calcium carbonate crystal particles are important performance indexes. The product with small granularity, uniform distribution and good dispersion performance has higher economic utilization value and wider market prospect.
The reverse microemulsion method is a water-in-oil type dispersion system composed of an oil phase, a water phase, a surfactant and the like. As a novel preparation method, the method has simple equipment and process, can provide a nano-scale microreactor, can accurately control the size and the shape of particles, well avoids the phenomena of agglomeration, oxidation and the like of micro-nano particles possibly caused in the processes of other preparation methods, and the prepared nanoparticles have the advantages of small particle size, good dispersibility, no impurities and the like. Therefore, the microemulsion method is an effective method for preparing micro-nano particles developed in recent years. Is a very good chemical reaction medium, and the particle size and other properties of the product can be controlled by artificially controlling the size of the 'micro water pool'.
[ summary of the invention ]
The invention aims to provide a preparation method of discus-shaped micron calcium carbonate. The method has the advantages of high safety performance, simplicity, reasonableness, low energy consumption, easily obtained raw materials, low price, good particle size distribution and stability of the discus-shaped micron calcium carbonate, good dispersion degree and wide application prospect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of discus-shaped micron calcium carbonate comprises the following steps:
1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant according to a volume ratio to prepare clear reverse microemulsion; said aqueous phase is an aqueous calcium chloride solution, said oil phase is cyclohexane, said co-surfactant is n-octanol, said surfactant is OP-10;
2) preparation of discus-shaped micron calcium carbonate: and (2) introducing carbon dioxide into the reversed-phase microemulsion obtained in the step 1) under the stirring state for reacting for a certain time until no precipitate is generated, stopping introducing carbon dioxide gas, ending stirring, standing at room temperature, aging, performing centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate.
Further, the volume ratio of the water, the oil, the cosurfactant and the surfactant is 4:50:15: 15.
Further, in the step 2), carbon dioxide is introduced into the reversed-phase microemulsion of the step 1) to react for 30 min.
Further, in the step 2), the aging time is 24 hours.
Further, in the step 2), the drying treatment is drying in an oven at 80 ℃ for 24 hours.
In the invention, the calcium chloride aqueous solution is prepared by the following method: weighing calcium chloride, dissolving with 25% ammonia water and a small amount of water, and adding water to obtain 0.5mol/L solution after completely dissolving.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
the preparation method of the discus-shaped micron calcium carbonate has the advantages of high safety performance, simplicity, reasonability, low energy consumption, easily available raw materials and low price, and the discus-shaped micron calcium carbonate has good particle size distribution and stability, good dispersity and wide application prospect.
[ description of the drawings ]
FIG. 1: scanning electron micrographs of the discus-like micron calcium carbonate prepared in the examples;
FIG. 2: x-ray diffraction patterns of the discus-like micrometer calcium carbonate prepared in the examples;
FIG. 3: scanning electron micrographs of the micron calcium carbonate prepared in the comparative example;
FIG. 4: the X-ray diffraction pattern of the micron calcium carbonate prepared in the comparative example;
FIG. 5: the main characteristic peaks in the standard X-ray diffraction patterns of vaterite and calcite.
[ detailed description ] embodiments
The specific embodiments and effects of the present invention will be illustrated by the following examples, but the scope of the present invention is not limited thereto.
Examples
A preparation method of discus-shaped micron calcium carbonate comprises the following steps:
1) preparation of an aqueous calcium chloride solution: 5.5278g of calcium chloride is weighed by an electronic balance, 7ml of 25% ammonia water with small amount of water is weighed by a pipette and dissolved in a beaker, and the beaker is transferred to a 100ml volumetric flask after being completely dissolved to achieve constant volume to obtain 0.5mol/L calcium chloride aqueous solution for later use;
2) preparing reverse microemulsion: respectively measuring 15ml of OP-10, 15ml of n-octanol, 50ml of cyclohexane and 4ml of calcium chloride aqueous solution obtained in the step 1) to prepare reverse microemulsion;
3) preparation of discus-shaped micron calcium carbonate: placing the beaker containing the reverse microemulsion prepared in the step 2) on a magnetic stirrer for stirring, and then introducing carbon dioxide into the reverse microemulsion for reaction for 30min without generating precipitates; and then ending the introduction of carbon dioxide, ending the stirring, standing at room temperature, aging for 24 hours, then carrying out centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate.
The obtained sample is shown in fig. 1 and fig. 2, and it can be observed from fig. 1 that the micron calcium carbonate prepared by the invention is similar to discus shape, and has uniform appearance and good dispersity; from fig. 2, it can be seen that diffraction peaks exist at diffraction angles 2 θ around 20.81 °, 24.81 °, 26.92 °, 32.60 °, 43.75 °, 49.87 °, and 55.70 °, which are consistent with the vaterite standard pattern (as in fig. 5), indicating that the prepared micron calcium carbonate crystalline form is substantially a vaterite form.
In addition, the inventor finds in experiments that during the preparation of the reverse microemulsion, if n-octanol is replaced by n-butanol, a discus-shaped micron calcium carbonate crystal form cannot be obtained, and particularly the following comparative example is shown below.
Comparative example
A method for preparing micron calcium carbonate comprises the following steps:
1) preparation of an aqueous calcium chloride solution: 5.5278g of calcium chloride is weighed by an electronic balance, 7ml of 25% ammonia water with small amount of water is weighed by a pipette and dissolved in a beaker, and the beaker is transferred to a 100ml volumetric flask after being completely dissolved to achieve constant volume to obtain 0.5mol/L calcium chloride aqueous solution for later use;
2) preparing reverse microemulsion: respectively measuring 15ml of OP-10, 15ml of n-butanol, 50ml of cyclohexane and 4ml of calcium chloride aqueous solution obtained in the step 1) to prepare reverse microemulsion;
3) preparation of micron calcium carbonate: placing the beaker containing the reverse microemulsion prepared in the step 2) on a magnetic stirrer for stirring, and then introducing carbon dioxide into the reverse microemulsion for reaction for 30min without generating precipitates; and then ending the introduction of carbon dioxide, ending the stirring, standing at room temperature, aging for 24 hours, then carrying out centrifugal separation, and drying the obtained precipitate to obtain the micron calcium carbonate.
The obtained sample is shown in fig. 3 and 4, and it can be observed from fig. 3 that the morphology of the calcium carbonate prepared by the preparation method is spherical and has no discus-shaped structure; from fig. 4, it can be seen that diffraction peaks exist at diffraction angles 2 θ around 24.84 °, 27.05 °, 32.78 °, 48.85 °, and 49.91 °, which are consistent with the vaterite standard pattern (see fig. 5), indicating that the prepared crystalline form of the micron calcium carbonate is substantially vaterite.
The above description is intended to describe in detail the preferred embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention, and all equivalent changes and modifications made within the technical spirit of the present invention should fall within the scope of the claims of the present invention.
Claims (6)
1. A preparation method of discus-shaped micron calcium carbonate is characterized by comprising the following steps:
1) preparing reverse microemulsion: fully mixing water, oil, cosurfactant and surfactant according to a volume ratio to prepare clear reverse microemulsion; said aqueous phase is an aqueous calcium chloride solution, said oil phase is cyclohexane, said co-surfactant is n-octanol, said surfactant is OP-10;
2) preparation of discus-shaped micron calcium carbonate: and (2) introducing carbon dioxide into the reversed-phase microemulsion obtained in the step 1) under the stirring state for reacting for a certain time until no precipitate is generated, stopping introducing carbon dioxide gas, ending stirring, standing at room temperature, aging, performing centrifugal separation, and drying the obtained precipitate to obtain the discus-shaped micron calcium carbonate.
2. The method of preparing discus-like micrometer calcium carbonate according to claim 1, wherein the volume ratio of water, oil, co-surfactant and surfactant is 4:50:15: 15.
3. The method for preparing discus-shaped micron calcium carbonate according to claim 1, wherein in the step 2), carbon dioxide is introduced into the reverse microemulsion of the step 1) for reaction for 30 min.
4. The process for preparing discus-shaped monocalcium carbonate according to claim 1, wherein in step 2), the aging time is 24 hours.
5. The method for preparing discus-shaped micron calcium carbonate according to claim 1, wherein in the step 2), the drying treatment is drying in an oven at 80 ℃ for 24 h.
6. The method of preparing discus-like micrometer calcium carbonate according to claim 1, wherein the aqueous calcium chloride solution is prepared by the following method: weighing calcium chloride, dissolving with 25% ammonia water and a small amount of water, and adding water to obtain 0.5mol/L solution after completely dissolving.
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| CN202010394156.8A CN111592026B (en) | 2020-05-11 | 2020-05-11 | Preparation method of discus-shaped micron calcium carbonate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113120936A (en) * | 2021-04-21 | 2021-07-16 | 贺州学院 | Method for preparing superfine calcium carbonate by adopting N235 reversed-phase microemulsion method |
| CN114455620A (en) * | 2022-01-11 | 2022-05-10 | 兰州交通大学 | Preparation method of square and cluster intergrowth integrated micron-sized calcium carbonate |
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| CN113120936A (en) * | 2021-04-21 | 2021-07-16 | 贺州学院 | Method for preparing superfine calcium carbonate by adopting N235 reversed-phase microemulsion method |
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| CN114455620B (en) * | 2022-01-11 | 2023-10-27 | 兰州交通大学 | Preparation method of square and cluster symbiotic micron-sized calcium carbonate |
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Application publication date: 20200828 Assignee: Guangxi Hezhou Asia Pacific powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046438 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 Application publication date: 20200828 Assignee: Guangxi Hezhou Kewei New Material Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046408 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 Application publication date: 20200828 Assignee: Guangxi Hezhou Jinlong Powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046406 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 Application publication date: 20200828 Assignee: Hezhou Xinhua hair powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046344 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 Application publication date: 20200828 Assignee: Hezhou Guangli powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046341 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 Application publication date: 20200828 Assignee: Hezhou Fuyuan Powder Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046335 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 Application publication date: 20200828 Assignee: Hezhou Zhaojun Chemical Co.,Ltd. Assignor: HEZHOU University Contract record no.: X2023980046442 Denomination of invention: A Preparation Method of Iron Cake like Micrometer Calcium Carbonate Granted publication date: 20230509 License type: Common License Record date: 20231108 |
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Effective date of registration: 20240503 Address after: 541208 Jinshan Industrial Zone, Tanxia Town, Lingchuan County, Guilin City, Guangxi Zhuang Autonomous Region Patentee after: GUILIN JINSHAN CHEMICAL INDUSTRIAL Co.,Ltd. Country or region after: China Address before: No. 18, Xihuan Road, Hezhou City, Guangxi Zhuang Autonomous Region Patentee before: HEZHOU University Country or region before: China Patentee before: Lanzhou Jiaotong University |