CN107162032B - A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle - Google Patents
A kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle Download PDFInfo
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- CN107162032B CN107162032B CN201710485978.5A CN201710485978A CN107162032B CN 107162032 B CN107162032 B CN 107162032B CN 201710485978 A CN201710485978 A CN 201710485978A CN 107162032 B CN107162032 B CN 107162032B
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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 68
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 33
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 108
- 159000000007 calcium salts Chemical class 0.000 claims description 28
- 239000008367 deionised water Substances 0.000 claims description 25
- 229910021641 deionized water Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000002202 Polyethylene glycol Substances 0.000 claims description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 24
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical group [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 24
- 229920001223 polyethylene glycol Polymers 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 15
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910001424 calcium ion Inorganic materials 0.000 claims description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 12
- 235000017550 sodium carbonate Nutrition 0.000 claims description 12
- 238000002604 ultrasonography Methods 0.000 claims description 11
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 239000012074 organic phase Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000000654 additive Substances 0.000 abstract description 3
- 239000008346 aqueous phase Substances 0.000 abstract description 3
- 230000000977 initiatory effect Effects 0.000 abstract description 3
- 239000012071 phase Substances 0.000 abstract description 3
- 238000010406 interfacial reaction Methods 0.000 abstract description 2
- 230000006641 stabilisation Effects 0.000 abstract 1
- 238000011105 stabilization Methods 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 20
- 229910021532 Calcite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 102000005701 Calcium-Binding Proteins Human genes 0.000 description 1
- 108010045403 Calcium-Binding Proteins Proteins 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- -1 papermaking Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 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
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to a kind of methods that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle.Using butyl glycol ether as chemical additives and pattern controlling agent, the interfacial reaction collided between organic phase and aqueous phase droplets by ultrasonic initiation reaction object, so as to be had the vaterite phase trigonal biyramid shape cium carbonate nanoparticles of the stabilization in (100) face, particle size is about 200 300nm.
Description
Technical field
The invention belongs to calcium carbonate material preparation fields, and in particular to a kind of method for preparing nano-calcium carbonate.
Background technology
Calcium carbonate is widely used in the industries such as rubber, plastics, coating, papermaking, ink, Jiao Dot agent, fluid sealant, can also apply
In industries such as toothpaste, food, medicine, word material, building materials, chemical fibres.The crystal form of calcium carbonate includes calcite, aragonite, three kinds of vaterite
Type, wherein calcite structure is most stable, and aragonite and vaterite belong to unstable state, and vaterite is difficult to be stabilized.
Nano-calcium carbonate grain size is small, large specific surface area, compared with ordinary calcium carbonate, has excellent performance.Grain size is in 10-
Nano-calcium carbonate between 100nm has strengthening action to rubber, plastics etc.；And the super fine calcium carbonate that grain size is 5-20nm,
Its reinforcing effect can be suitable with white carbon.However, the nano-calcium carbonate prepared in the prior art is mostly micron, submicron-scale,
The nano-calcium carbonate of super-small is hardly resulted in, and with stable vaterite crystal form.
Invention content
The technical scheme is that in order to overcome the shortcoming of prior art, proposition is a kind of to prepare vaterite-type carbonic acid
Calcium nano-powder.
The present invention proposes a kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle, which is characterized in that
Include the following steps：
1) solution a is prepared：Calcium salt is dissolved in deionized water, butyl glycol ether is added in, stirs evenly；
2) solution b is prepared：Sodium carbonate, ammonium carbonate or ammonium hydrogen carbonate are dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, adds in solution a, 40-60 DEG C is stirred 1h, after being cooled to room temperature, under ultrasound, is added
Enter solution b, ultrasonic reaction 10-20min；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate nano particle.
Wherein, the calcium salt is calcium nitrate or calcium chloride.
Wherein, in solution a, a concentration of 0.8-1.5mol/L of calcium salt.
Wherein, in solution a, the molar ratio of calcium salt and butyl glycol ether is 1: 0.7-1.
Wherein, in step 3), calcium ion and the molar ratio of carbanion or bicarbonate ion are 1 in reaction system:
1-1.2。
Wherein, in step 3), polyethylene glycol mass concentration in toluene is 10-15%.
Wherein, in step 3), the volume ratio of toluene and solution a are 3-10: 1.
Wherein, in step 3), ultrasonic power 150-200W.
The present invention, as chemical additives and pattern controlling agent, can pass through electrostatic adsorption using butyl glycol ether
It is trigonal biyramid shape particle, and form vaterite-type calcium carbonate so as to make particle that anisotropic growth occur with calcium binding,
And (100) face rich in positive electricity calcium ion is exposed, be conducive to further be combined with electronegative biomolecule.
Calcium ion is scattered in organic phase by the present invention, adds the solution containing carbonic acid root or bicarbonate ion,
By ultrasonic initiation reaction, reaction is made to occur between organic phase and aqueous phase droplets.
Beneficial effects of the present invention：This method by using butyl glycol ether as chemical additives and pattern controlling agent,
The interfacial reaction collided between organic phase and aqueous phase droplets by ultrasonic initiation reaction object, so as to be had (100) face
Stable vaterite phase trigonal biyramid shape cium carbonate nanoparticles, particle size is about 200-300nm.
Specific embodiment
With reference to embodiment, further illustrate the present invention.
Embodiment 1
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 2
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 0.5, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 3
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1.5, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 4
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol in toluene mass concentration be 5%, add in solution a, toluene with
The volume ratio of solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min, surpasses
Acoustical power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 5
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 20%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 6
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under stirring, adds in solution b, is stirred to react 15min,
The molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 7
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 100W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 8
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 5: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 300W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 9
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 1: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
Embodiment 10
1) solution a is prepared：Calcium nitrate is dissolved in deionized water so that a concentration of 1mol/L of calcium salt adds in ethylene glycol fourth
The molar ratio of ether, calcium salt and butyl glycol ether is 1: 1, is stirred evenly；
2) solution b is prepared：Sodium carbonate is dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, polyethylene glycol mass concentration in toluene is 12%, adds in solution a, toluene
Volume ratio with solution a is 15: 1,50 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, adds in solution b, ultrasonic reaction 15min,
Ultrasonic power is 150W, and the molar ratio of calcium ion and carbanion is 1: 1 in reaction system；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate triangular pyramidal nano particle.
The pattern for the product that embodiment 1-10 is obtained see the table below
Embodiment 11
The vaterite-type calcium carbonate particle that embodiment 1 is obtained in ultrasonic disperse to deionized water, is heated to 80 DEG C of stirrings
3h, centrifugation, obtained precipitation remain as vaterite-type calcium carbonate nano double cone shaped granule.Although illustrate vaterite in the prior art
For the unstable crystalline phase of calcium carbonate, but the vaterite-type calcium carbonate nanometer obtained due to the effect of butyl glycol ether, the present invention
Grain can more steadily exist.
Claims (4)
1. a kind of method that ultrasonic wave added prepares vaterite-type calcium carbonate nano particle, which is characterized in that include the following steps：
1) solution a is prepared：Calcium salt is dissolved in deionized water, butyl glycol ether is added in, stirs evenly；
2) solution b is prepared：Sodium carbonate, ammonium carbonate or ammonium hydrogen carbonate are dissolved in deionized water；
3) polyethylene glycol is dissolved in toluene, adds in solution a, 40-60 DEG C of stirring 1h, after being cooled to room temperature, under ultrasound, addition is molten
Liquid b, ultrasonic reaction 10-20min；
4) product is collected, is centrifuged, is washed, it is dry, obtain vaterite-type calcium carbonate nanometer trigonal biyramid shape particle；
Wherein, the molar ratio of calcium salt and butyl glycol ether is 1: 1；Mass concentration of the polyethylene glycol in toluene is 12%, toluene
Volume ratio with solution a is 5, ultrasonic power 150W.
2. according to the method described in claim 1, it is characterized in that：The calcium salt is calcium nitrate or calcium chloride.
3. according to the method described in claim 1, it is characterized in that：In solution a, a concentration of 0.8-1.5mol/L of calcium salt.
4. according to the method described in claim 1, it is characterized in that：In step 3), in reaction system calcium ion and carbonate from
The molar ratio of son or bicarbonate ion is 1: 1-1.2.
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| CN1887716A (en) * | 2006-07-31 | 2007-01-03 | 南京大学 | Monodisperse micron level spherical vaterite-type calcium carbonate and its prepn process |
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| CN106348332B (en) * | 2016-11-21 | 2017-11-28 | 中国科学院上海高等研究院 | A kind of method and device that vaterite is prepared using dynamic magnetic agitating paddle |
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Effective date of registration: 20191118 Address after: 311407 building 4, No. 215, xiaojiawu, Xintong village, Xintong Township, Fuyang District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou HANGGANG Sanjiang Mining Co., Ltd Address before: 315400 room 1, 315, international business center, China Plastics City, Ningbo, Zhejiang, Yuyao Patentee before: LI CHUNSONG |
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| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 311407 building 4, 215 xiaojiawu, Xintong village, Xintong Township, Fuyang District, Hangzhou City, Zhejiang Province Patentee after: Hangzhou Zhenxin Mining Co.,Ltd. Address before: 311407 building 4, 215 xiaojiawu, Xintong village, Xintong Township, Fuyang District, Hangzhou City, Zhejiang Province Patentee before: Hangzhou HANGGANG Sanjiang Mining Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 311407 building 4, 215 xiaojiawu, Xintong village, Xintong Township, Fuyang District, Hangzhou City, Zhejiang Province Patentee after: Zhejiang Zhenxin New Material Technology Co.,Ltd. Address before: 311407 building 4, 215 xiaojiawu, Xintong village, Xintong Township, Fuyang District, Hangzhou City, Zhejiang Province Patentee before: Hangzhou Zhenxin Mining Co.,Ltd. |