CN108893775A - A kind of preparation method of purity calcium carbonate whisker - Google Patents
A kind of preparation method of purity calcium carbonate whisker Download PDFInfo
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- CN108893775A CN108893775A CN201810779834.5A CN201810779834A CN108893775A CN 108893775 A CN108893775 A CN 108893775A CN 201810779834 A CN201810779834 A CN 201810779834A CN 108893775 A CN108893775 A CN 108893775A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of preparation method of purity calcium carbonate whisker, this method is：It is first calcium oxide by calcium carbonate raw material calcining and decomposing, calcium oxide is add to deionized water again and is digested at a certain temperature, then injection is added and stirs evenly into crystal controlling agent solution, carbon dioxide is passed through with given pace using aerator, the bubble volume for being passed through gas, dispersibility i.e. carbon acid ion concentration are controlled with this, make carburizing reagent uniformity everywhere, so that high-purity whisker be made.It utilizes in emulsion tube ventilation preparation process this solves previous since gas disperses the uneven problem for causing whisker purity low in the solution, and gas more comes into full contact with solution realization, higher purity whisker can not only be prepared, carbon dioxide gas used can also be largely saved, preparation cost is reduced.
Description
Technical field
The present invention relates to inorganic filling material preparation technical field, in particular to a kind of preparation of purity calcium carbonate whisker
Method.
Background technique
Because structure is more complete and defect is seldom, intensity and modulus hinders inorganic crystal whisker close to the theoretical value of perfect crystal
Firing performance must be good than organic crystalline, becomes the activeness and quietness material of highly desirable composite material, such as ZnO, SiC, potassium titanate, Mo Lai
Stone, aluminium borate etc. have realized industrialization production but have hindered scale application because at high cost, and calcium carbonate crystal whisker raw material sources are wide
General and production cost is low, it might even be possible to be prepared using industrial residue, be expected to become most important inorganic crystal whisker material.
Currently, domestic and foreign scholars have done numerous studies to the preparation of aragonite calcium carbonate whisker, mainly there are five class preparation methods：
(1) double decomposition；(2)Ca(HCO3)2Thermal decomposition method；(3) ureal antigen；(4) sol-gel method；(5) carbonation method.Wherein
Carbonation method is domestic and international most study also a kind of more mature method, since preparation process is simple, at low cost, is expected to earliest
Realize the industrialization of calcium carbonate.The general process of carbonation method is that calcium oxide is digested to suspension slurry in deionized water, should
Suspension is passed through carbon dioxide gas after mixing with chemical additives solution, reacts under the crystal form control action of chemical additives
Generate calcium carbonate crystal whisker.Preparing a critical issue existing for high-purity whisker is that carbanion is unevenly distributed in suspension
It is even, lead to the excessively high calcite phase calcium carbonate easily generated of partial region degree of supersaturation, reduces whisker purity；Main reason is that previous
Generate air pocket in solution bottom when ventilating using emulsion tube, these air pocket distributions are small, in the position that bubble is emerged and
The excessive concentration of top carbanion quickly generates calcite, and it is mutually brilliant that aragonite is then slowly generated at other low saturations
Must, it is unfavorable for the preparation of purity calcium carbonate whisker.
Therefore, the present invention proposes a kind of to be passed through carbon dioxide gas using aerator to prepare purity calcium carbonate whisker
Method, such as quartzy air stone of aerator is a kind of porous gas distributor, and stomata is tiny, the titanium dioxide that can will be passed through
Carbon gas is broken into the bubble of many volume very littles, and is passed through in solution these rear minute bubbles and spreads out, gas distribution
Expand, so that the carbanion for being conducive to generate is uniformly distributed in the solution, the ventilation by regulation of carbon dioxide is achieved
Rate controls the degree of supersaturation of solution carbanion everywhere, to generate the calcium carbonate crystal whisker of high-purity.In addition, using exposing
Device of air contacts carbon dioxide gas more fully with solution realization, and the utilization rate of carbon dioxide being passed through is high, needs at this time
Ventilatory capacity than emulsion tube ventilate it is much lower, largely reduce production cost.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of purity calcium carbonate whisker, this method is based on carbonating
Calcium carbonate raw material calcining and decomposing is first calcium oxide by method, and subsequent calcium oxide digests under high temperature in deionized water, with magnesium chloride
Solution is crystal control agent, and the injection of postdigestive calcium hydroxide suspension is added in magnesium chloride solution, certain stomata is utilized
The aerator in aperture is passed through carbon dioxide with given pace, and the bubble volume for being passed through gas, dispersibility are controlled with this and then is made
Carbanion is uniformly distributed in the solution, so that it is carried out carburizing reagent under given pace stirring, until pH value of solution is reduced to 7 reactions
Terminate, obtains the calcium carbonate crystal whisker of high-purity.It is implemented as follows：
Step 1：By calcining and decomposing is oxidation at high temperature after the calcium carbonate mineral obtained from mining area exploitation screening grinding
Calcium；The high temperature is the decomposition temperature for being higher than calcium carbonate.
Step 2：Above-mentioned calcium oxide, which is add to deionized water, digests it sufficiently, obtains Ca (OH)2Suspension；
Step 3：It using magnesium chloride as crystal control agent, is dissolved in water, and by above-mentioned postdigestive Ca (OH)2Suspension
It is added in magnesium chloride solution in a manner of atomized spray, stirs evenly acquisition mixed liquor；
Step 4：Carbon dioxide gas is passed through by aerator in above-mentioned mixed liquor, stirring carries out carburizing reagent, directly
Reaction stops when being reduced to 7 to solution ph, and gained precipitating is filtered, is washed, dry, obtains purity calcium carbonate whisker.
In above-mentioned technical proposal, further, average grain diameter of the calcium carbonate mineral after screening grinding in the step 1
It is 1.29~4.24 μm；
Further, calcium oxide is added in 80~100 DEG C of deionized water in step 2, digestion time is at least 1h；
Further, the amount of magnesium chloride described in the step 3 should make the ratio between magnesium calcium atom molar concentration CMg/CCa?
Between 1.5~2.5；
Further, the aerator used in the step 4 includes quartzy air stone, porous ceramics or porous brick,
Aperture answer it is as small as possible, and be no more than 5mm.
Further, the step 4 stirring rate is between 100~200r/min.
Further, aerator is placed on the bottom of mixed liquor in the step four.
Compared with having and preparing the technology of calcium carbonate crystal whisker, prominent feature and significant progress are the present invention：
1. the carbon dioxide gas being passed through is smashed using aerators such as air stones as air-breather, be conducive to gas
It is uniformly dispersed in the solution, and then it is uniform to be conducive to carbonate concentration in solution, keeps everywhere conducive to reactive ion identical low
Degree of supersaturation, and it was found that the air stone of more spilehole is conducive to generate the whisker of higher purity；Simultaneously because bubble and solution are real
It now more fully contacts, improves carbon dioxide utilization efficiency, reduce preparation cost.
2. postdigestive calcium hydroxide suspension is added in magnesium chloride solution in a manner of atomized spray, spraying
Misty suspension obtains certain dispersion in journey, is conducive to the Quick uniform in magnesium chloride solution, the entirety of solution system is uniformly
Property for preparation high-purity whisker be very important.
Calcium carbonate crystal whisker purity produced by the present invention may be up to 99.7%.
Detailed description of the invention
Fig. 1 is calcium carbonate crystal whisker optical microscope picture；
Fig. 2 is the XRD spectra that the embodiment of the present invention prepares whisker.
Specific embodiment
Technical solution of the present invention will be clearly and completely described by embodiment below, it is clear that described reality
Applying example is only a part of the embodiments of the present invention, and instead of all the embodiments, air-breather of the invention includes but not only limits
In the aerators such as quartzy air stone and porous ceramics, porous brick.Based on the embodiment of the present invention, ordinary skill
Personnel's every other embodiment obtained under the premise of not making any creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
Step 1：Calcining and decomposing is calcium oxide under the calcium carbonate high temperature for being 1.29 μm by average grain diameter；
Step 2：7.84g calcium oxide is weighed, is added in 600ml deionized water and is sufficiently digested at 100 DEG C；
Step 3：42.693g magnesium chloride is weighed as crystal control agent (making magnesium calcium atom molar ratio 1.5), is added
The dissolution of 100ml water, and by postdigestive Ca (OH)2Suspension is added in magnesium chloride solution with atomized spray, is stirred evenly；
Step 4：Titanium dioxide is passed through with the flow of 10ml/min using the quartzy air stone that stomata average pore size is 0.92mm
Carbon gas is to reaction unit bottom, and stirring rate 100r/min, carrying out carburizing reagent to solution ph is that 7 reactions stop, most
Gained precipitating is filtered afterwards, is washed, it is dry.
The SEM image of prepared calcium carbonate crystal whisker is shown in Fig. 1 (1#).
Embodiment 2
Step 1：Calcining and decomposing is calcium oxide under the calcium carbonate high temperature for being 2.77 μm by average grain diameter；
Step 2：7.84g calcium oxide is weighed, is added in 600ml deionized water and is sufficiently digested at 90 DEG C；
Step 3：56.942g magnesium chloride (making magnesium calcium molar ratio 2) is weighed as crystal control agent, it is water-soluble that 100ml is added
Solution, and by postdigestive Ca (OH)2Suspension injection is added in magnesium chloride solution, is stirred evenly；
Step 4：Carbon dioxide gas is passed through to anti-with 25ml/min flow using the air stone that air vent aperture is 2.82mm
Bottom of device is answered, stirring rate 150r/min, carrying out carburizing reagent to solution ph is that 7 reactions stop, and finally gained sinks
Shallow lake is filtered, and is washed, dry.
The SEM image of prepared calcium carbonate crystal whisker is shown in Fig. 1 (2#).
Embodiment 3
Step 1：Calcining and decomposing is calcium oxide under the calcium carbonate high temperature for being 4.24 μm by average grain diameter；
Step 2：7.84g calcium oxide is weighed, is added in 600ml deionized water and is sufficiently digested at 80 DEG C；
Step 3：71.155g magnesium chloride (making magnesium calcium molar ratio 2.5) is weighed as crystal control agent, 100ml water is added
Dissolution, and by postdigestive Ca (OH)2Suspension injection is added in magnesium chloride solution, is stirred evenly；
Step 4：Carbon dioxide gas is passed through with 40ml/min flow using the quartzy air stone that air vent aperture is 4.94mm
To reaction unit bottom, stirring rate 200r/min, carrying out carburizing reagent to solution ph is that 7 reactions stop, finally by institute
It must precipitate and be filtered, be washed, it is dry.
The SEM image of prepared calcium carbonate crystal whisker is shown in Fig. 1 (3#).
In addition, the present invention, which has also carried out multiple groups control experiment, obtains 4-6# sample：Compared with Example 1, only change following
Condition, other conditions are all the same, and 4# is directly to pour into calcium hydroxide suspension into magnesium chloride solution rather than atomized spray
Mode is added；5# is to be ventilated with the air stone of stomata average pore size 10mm；6# be with flexible rubber hose (diameter about 6mm) rather than bubble
Stone ventilation.The SEM figure of 6 samples is detailed in Fig. 1, and XRD diagram is detailed in Fig. 2.
Whisker purity is by aragonite phase top integrated intensity Ia in XRD spectrum and calcite phase top integrated intensity Ic value
It is calculated：
It is computed, it is 99.7% that embodiment 1 (1#), which prepares whisker purity,；Embodiment 2 (2#) prepares whisker purity
99.3%；It is 99.1% that embodiment 3 (3#), which prepares whisker purity,；The purity of control group 4# is 92.4%, the purity of control group 5#
It is 95.2%, the purity of control group 6# is 90.1%.It can be inferred that：Using the aerator of such as quartzy air stone as
Air-breather and the method for using misty injection that calcium hydroxide suspension is added can significantly improve whisker purity.
Claims (7)
1. a kind of preparation method of purity calcium carbonate whisker, which is characterized in that steps are as follows：
Step 1：By calcining and decomposing is calcium oxide at high temperature after the calcium carbonate mineral obtained from mining area exploitation screening grinding；
Step 2：Above-mentioned calcium oxide, which is add to deionized water, digests it sufficiently, obtains Ca (OH)2Suspension；
Step 3：It using magnesium chloride as crystal control agent, is dissolved in water, and by above-mentioned postdigestive Ca (OH)2Suspension is to be atomized
The mode of injection is added in magnesium chloride solution, stirs evenly acquisition mixed liquor；
Step 4：Carbon dioxide gas is passed through by aerator in above-mentioned mixed liquor, stirring carries out carburizing reagent, until molten
Reaction stops when liquid pH value is reduced to 7, and gained precipitating is filtered, is washed, dry, obtains purity calcium carbonate whisker.
2. the preparation method of purity calcium carbonate whisker according to claim 1, it is characterised in that：Carbon in the step 1
Average grain diameter of the sour calcium ore after screening grinding is 1.29~4.24 μm.
3. the preparation method of purity calcium carbonate whisker according to claim 1, it is characterised in that：It will oxidation in step 2
Calcium is added in 80~100 DEG C of deionized water, and digestion time is at least 1h.
4. the preparation method of purity calcium carbonate whisker according to claim 1, it is characterised in that：Described in step 3
The amount of magnesium chloride should make the ratio between magnesium calcium atom molar concentration CMg/CCaBetween 1.5~2.5.
5. the preparation method of purity calcium carbonate whisker according to claim 1, it is characterised in that：It is used in step 4
Aerator includes quartzy air stone, porous ceramics or porous brick, and aperture is no more than 5mm.
6. the preparation method of purity calcium carbonate whisker according to claim 1, it is characterised in that：It is stirred in the step 4
Rate is mixed between 100~200r/min.
7. the preparation method of purity calcium carbonate whisker according to claim 1, it is characterised in that：In the step four
Aerator is placed on the bottom of mixed liquor.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410882A (en) * | 2020-11-19 | 2021-02-26 | 成都新柯力化工科技有限公司 | Whitening calcium carbonate whisker for plastic reinforcement and preparation method thereof |
| CN113564688A (en) * | 2021-07-09 | 2021-10-29 | 沈阳化工大学 | Preparation method of calcium carbonate whisker |
| CN114314629A (en) * | 2021-12-16 | 2022-04-12 | 浙江大学 | Preparation method of nano calcium carbonate based on surface potential control |
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| CN107916452A (en) * | 2017-11-14 | 2018-04-17 | 浙江大学 | A kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern |
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| CN112410882A (en) * | 2020-11-19 | 2021-02-26 | 成都新柯力化工科技有限公司 | Whitening calcium carbonate whisker for plastic reinforcement and preparation method thereof |
| CN113564688A (en) * | 2021-07-09 | 2021-10-29 | 沈阳化工大学 | Preparation method of calcium carbonate whisker |
| CN113564688B (en) * | 2021-07-09 | 2023-11-28 | 沈阳化工大学 | Preparation method of calcium carbonate whisker |
| CN114314629A (en) * | 2021-12-16 | 2022-04-12 | 浙江大学 | Preparation method of nano calcium carbonate based on surface potential control |
| CN114314629B (en) * | 2021-12-16 | 2022-09-30 | 浙江大学 | Preparation method of nano calcium carbonate based on surface potential control |
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