CN105585041B - A kind of preparation method of tangerine flap calcium carbonate microparticle - Google Patents
A kind of preparation method of tangerine flap calcium carbonate microparticle Download PDFInfo
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- CN105585041B CN105585041B CN201610053318.5A CN201610053318A CN105585041B CN 105585041 B CN105585041 B CN 105585041B CN 201610053318 A CN201610053318 A CN 201610053318A CN 105585041 B CN105585041 B CN 105585041B
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- calcium chloride
- alcoholic solution
- sodium carbonate
- calcium
- aqueous sodium
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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 56
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 27
- 241000675108 Citrus tangerina Species 0.000 title claims abstract description 23
- 239000011859 microparticle Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 60
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 33
- 239000001110 calcium chloride Substances 0.000 claims abstract description 33
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 33
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 31
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010406 interfacial reaction Methods 0.000 claims abstract description 9
- 238000000746 purification Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000011049 filling Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 4
- 239000011575 calcium Substances 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000005374 membrane filtration Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- GDESEHSRICGNDP-UHFFFAOYSA-L [Cl-].[Cl-].[Ca+2].CCO Chemical compound [Cl-].[Cl-].[Ca+2].CCO GDESEHSRICGNDP-UHFFFAOYSA-L 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000725 suspension 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
-
- 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
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- 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)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to a kind of preparation method of tangerine flap calcium carbonate microparticle, using sodium carbonate as raw material, the aqueous sodium carbonate that concentration is 0.3~0.8mol/L is configured to water；Using calcium chloride as raw material, the calcium chloride alcoholic solution that concentration is 0.3~0.8mol/L is configured to absolute ethyl alcohol, then aqueous sodium carbonate and calcium chloride alcoholic solution are distinguished into Purification by filtration, calcium chloride alcoholic solution is slowly added into aqueous sodium carbonate again, the addition of calcium chloride alcoholic solution is based on 1: 1~1.1 by the molal quantity of the molal quantity: sodium carbonate of calcium chloride, enter water-filling/0.5~2h of alcoholic solution interfacial reaction, pelleting centrifugation will be generated, and after alternately being washed with redistilled water and absolute ethyl alcohol, in being dried at 95~105 DEG C, tangerine flap calcium carbonate microparticle is obtained.The present invention has synthesized tangerine flap calcium carbonate microparticle first, and product morphology is unique, and particle size is evenly distributed at 3 ~ 6 μm.And present invention process method is simple to operate, raw material environmental protection, safety non-toxic.
Description
Technical field
The present invention relates to a kind of preparation method of tangerine flap calcium carbonate microparticle, belong to field of inorganic chemical engineering.
Background technology
Calcium carbonate is there are one of most commonly used mineral in nature, while being also a kind of highly important inorganic fill out
Material, is applied in industries such as rubber, papermaking, coating, medicine by substantial amounts of.Calcium carbonate belongs to ABO3The polytype crystal of class, mainly has
Calcite（It is most stable）, aragonite, vaterite（Least stablize）.In actual applications, the calcium carbonate material of different crystal forms has not
The difference of same property and purposes, its grain graininess and pattern, also determines its different property and application field, artificial synthesized
Calcium carbonate microparticle pattern with cubic type, ball-type, pin must type etc. it is relatively conventional.
At present, it is in the majority with microspheric calcium carbonate granule in calcium carbonate microparticle preparation.Being added in white lime suspension has
Machine solvent methanol (United States Patent (USP), patent No. US5275651), water-soluble natural macromolecule (Japan Patent, the patent No.
JP3060427), carbon dioxide is then passed to, calcium carbonate microspheres are made.With a kind of dissaving polymer of parents' water type point
Son is as template (Chinese patent CN102515236A), by the precipitation reaction between water-soluble Ca salt and carbonate, and carbonic acid is made
Calcium microballoon.In certain density calcium chloride water, pH value of solution is adjusted to 9.0 ~ 11.5 with ammoniacal liquor, then be passed through pre- through Bubbled stone
Carbon dioxide after scattered（Chinese patent CN103864127A）, obtain flower ball-shaped calcium carbonate microparticle.In the above method still
There is complex operation, be passed through gas and using weak points such as poisonous organic solvents.And there are no and be prepared into tangerine flap carbon
The correlation technique of sour calcium particulate is disclosed.
The content of the invention
The technical problem to be solved in the present invention is：A kind of preparation method of tangerine flap calcium carbonate microparticle, this method institute are provided
Obtained calcium carbonate product pattern is tangerine flap particulate, and particle size is evenly distributed at 3 ~ 6 μm.
Solving the technical scheme of above-mentioned technical problem is：A kind of preparation method of tangerine flap calcium carbonate microparticle, with sodium carbonate
For raw material, the aqueous sodium carbonate that concentration is 0.3~0.8mol/L is configured to water；Using calcium chloride as raw material, absolute ethyl alcohol is used
The calcium chloride alcoholic solution that concentration is 0.3~0.8mol/L is configured to, then aqueous sodium carbonate and calcium chloride alcoholic solution is distinguished
Purification by filtration, then calcium chloride alcoholic solution is slowly added into aqueous sodium carbonate, the addition of calcium chloride alcoholic solution presses chlorination
The molal quantity of the molal quantity: sodium carbonate of calcium is 1: 1~1.1 meters, enters water-filling/alcoholic solution 0.5~2h of interfacial reaction, and generation is precipitated
Centrifugation, and with after redistilled water and absolute ethyl alcohol alternately washing, in being dried at 95~105 DEG C, obtain tangerine flap calcium carbonate micro-
Grain.
The present invention further technical scheme be：Purification by filtration is to lead to aqueous sodium carbonate and calcium chloride alcoholic solution respectively
Cross 0.45 μm of membrane filtration purifying.
Calcium chloride alcoholic solution is added in aqueous sodium carbonate, it is desirable to which calcium chloride alcoholic solution need to be slowly added to, and keeps chlorination
Calcium alcoholic solution is stable to float over aqueous sodium carbonate upper strata, carries out follow-up interfacial reaction until reaction terminates.
The present invention has synthesized tangerine flap calcium carbonate microparticle first, and product morphology is unique, and particle size is at 3 ~ 6 μm, and distribution is equal
It is even.And present invention process method is simple to operate, raw material environmental protection, safety non-toxic.
Brief description of the drawings
Fig. 1：Scanning electron microscope (SEM) photograph when tangerine flap calcium carbonate microparticle magnification ratio prepared by the present invention is smaller.
Fig. 2：Scanning electron microscope (SEM) photograph when tangerine flap calcium carbonate microparticle magnification ratio prepared by the present invention is larger.
Embodiment
Embodiment 1：Prepare 0.3mol/L aqueous sodium carbonate and 0.3mol/L calcium chloride respectively in 50ml beakers
Ethanol solution, matched somebody with somebody solution is purified by 0.45 μm of membrane filtration.It is slowly added in aqueous sodium carbonate after purification
The calcium chloride alcoholic solution of amount, keeps stable and floats over aqueous solution upper strata, enter water-filling/alcoholic solution interfacial reaction 1.5h, generation is precipitated
Centrifuge and use redistilled water and absolute ethyl alcohol alternately wash after, at 100 DEG C dry, obtain tangerine flap calcium carbonate microparticle.This
Product pattern obtained by invention is tangerine flap particulate, and particle size is evenly distributed at 3 ~ 6 μm.
Embodiment 2：Prepare 0.5mol/L aqueous sodium carbonate and 0.5mol/L calcium chloride respectively in 50ml beakers
Ethanol solution, matched somebody with somebody solution is purified by 0.45 μm of membrane filtration.It is slowly added in aqueous sodium carbonate after purification
The calcium chloride alcoholic solution of amount, keeps stable and floats over aqueous solution upper strata, enter water-filling/alcoholic solution interfacial reaction 1h, will generation precipitation from
The heart is simultaneously replaced after washing with redistilled water and absolute ethyl alcohol, in being dried at 100 DEG C, obtains tangerine flap calcium carbonate microparticle.This hair
Product pattern obtained by bright is tangerine flap particulate, and particle size is evenly distributed at 3 ~ 6 μm.
Embodiment 3：Prepare 0.7mol/L aqueous sodium carbonate and 0.7mol/L calcium chloride respectively in 50ml beakers
Ethanol solution, matched somebody with somebody solution is purified by 0.45 μm of membrane filtration.It is slowly added in aqueous sodium carbonate after purification
The calcium chloride alcoholic solution of amount, keeps stable and floats over aqueous solution upper strata, enter water-filling/alcoholic solution interfacial reaction 0.5h, generation is precipitated
Centrifuge and use redistilled water and absolute ethyl alcohol alternately wash after, at 100 DEG C dry, obtain tangerine flap calcium carbonate microparticle.This
Product pattern obtained by invention is tangerine flap particulate, and particle size is evenly distributed at 3 ~ 6 μm.
In various embodiments of the present invention, calcium chloride alcoholic solution is added in aqueous sodium carbonate, it is desirable to which calcium chloride alcoholic solution is needed
It is slowly added to, keeps calcium chloride alcoholic solution is stable to float over aqueous sodium carbonate upper strata, carries out follow-up interfacial reaction until reaction
Terminate.
The water that various embodiments of the present invention prepare used in aqueous sodium carbonate is redistilled water, prepares calcium chloride ethanol solution
Ethanol used is absolute ethyl alcohol.
In various embodiments of the present invention, generation precipitation is centrifuged under conditions of 3500~4000rpm.
In various embodiments of the present invention, generate pelleting centrifugation and alternately washed with redistilled water and absolute ethyl alcohol, with secondary
Distilled water washed once with absolute ethyl alcohol as alternately washing 1 time, altogether alternately washing 2~3 times again after washed once.
Claims (2)
1. a kind of preparation method of tangerine flap calcium carbonate microparticle, it is characterised in that：Using sodium carbonate as raw material, concentration is configured to water
For 0.3~0.8mol/L aqueous sodium carbonate；Using calcium chloride as raw material, be configured to absolute ethyl alcohol concentration for 0.3~
0.8mol/L calcium chloride alcoholic solution, then distinguishes Purification by filtration by aqueous sodium carbonate and calcium chloride alcoholic solution, then by chlorination
Calcium alcoholic solution is slowly added into aqueous sodium carbonate, and the addition of calcium chloride alcoholic solution presses the molal quantity: sodium carbonate of calcium chloride
Molal quantity for 1: 1~1.1 meter, enter water-filling/alcoholic solution 0.5~2h of interfacial reaction, pelleting centrifugation will be generated, and use second distillation
After water and absolute ethyl alcohol are alternately washed, in being dried at 95~105 DEG C, tangerine flap calcium carbonate microparticle is obtained；
Calcium chloride alcoholic solution is added in aqueous sodium carbonate, it is desirable to which calcium chloride alcoholic solution need to be slowly added to, and keeps calcium chloride alcohol
It is solution-stabilized to float over aqueous sodium carbonate upper strata, follow-up interfacial reaction is carried out until reaction terminates.
2. a kind of preparation method of tangerine flap calcium carbonate microparticle according to claim 1, it is characterised in that：Purification by filtration is
Aqueous sodium carbonate and calcium chloride alcoholic solution are purified by 0.45 μm of membrane filtration respectively.
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| CN201610053318.5A CN105585041B (en) | 2016-01-26 | 2016-01-26 | A kind of preparation method of tangerine flap calcium carbonate microparticle |
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| CN107055584B (en) * | 2017-03-29 | 2018-09-07 | 河南师范大学 | A kind of preparation method of cellular porous calcium carbonate |
| CN112456532B (en) * | 2020-12-08 | 2023-10-24 | 理光感热技术（无锡）有限公司 | Preparation method of calcium carbonate |
| CN116675240B (en) * | 2023-06-21 | 2023-11-10 | 广西科学院 | Preparation method of mildew-proof antibacterial superfine active precipitated calcium carbonate |
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| JPH02153819A (en) * | 1988-09-12 | 1990-06-13 | Sanyo Kokusaku Pulp Co Ltd | Production of hollow and spherical vaterite type calcium carbide and stabilization thereof |
| CN1194944A (en) * | 1997-03-31 | 1998-10-07 | 龚德和 | Oral superfine calcium carbonate for human calcium supplement and its producing method |
| JP2009067605A (en) * | 2007-09-10 | 2009-04-02 | Oita Univ | Method for producing aragonite type calcium carbonate with hexagonal plate form |
| CN104324674B (en) * | 2014-10-09 | 2016-04-13 | 哈尔滨工业大学宜兴环保研究院 | The drop obtained after meeting water-soluble solution based on nucleus in ethanol prepares the method for inorganic mineralising microcapsules |
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Application publication date: 20160518 Assignee: ADANA FOOD TECH (LIUZHOU) Co.,Ltd. Assignor: GUANGXI University OF SCIENCE AND TECHNOLOGY Contract record no.: X2023980054175 Denomination of invention: A preparation method for orange petal shaped calcium carbonate particles Granted publication date: 20170901 License type: Common License Record date: 20231226 |
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Application publication date: 20160518 Assignee: GUANGXI CHUNHUI ENVIRONMENTAL PROTECTION ENGINEERING Co.,Ltd. Assignor: GUANGXI University OF SCIENCE AND TECHNOLOGY Contract record no.: X2024980016743 Denomination of invention: Preparation method of orange petal shaped calcium carbonate particles Granted publication date: 20170901 License type: Common License Record date: 20240926 |