CN107916452A - A kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern - Google Patents
A kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern Download PDFInfo
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- CN107916452A CN107916452A CN201711122887.1A CN201711122887A CN107916452A CN 107916452 A CN107916452 A CN 107916452A CN 201711122887 A CN201711122887 A CN 201711122887A CN 107916452 A CN107916452 A CN 107916452A
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- calcium carbonate
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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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- 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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- Crystallography & Structural Chemistry (AREA)
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern, its method is：First calcium oxide is added in deionized water, digested at a certain temperature, then crystal control agent is added to stir evenly, being passed through carbon dioxide using double-tube air breather with certain flow makes it carry out carbonation reaction, finally obtained suspension is filtered, is washed, is dry, obtains sample.The method have the characteristics that prepared multi-arm whisker is a kind of new pattern calcium carbonate crystal whisker, and whisker minor matters number can be controlled by by reaction condition.This whisker is used as the packing material of composite material, has very big advantage in lifting its chemical property and mechanical property etc..
Description
Technical field
The present invention relates to technical field of preparation for inorganic material, the continuous controllable calcium carbonate crystal whisker of more particularly to a kind of pattern
Preparation method.
Background technology
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 ratio organic crystalline must be good, 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 of high cost, and calcium carbonate crystal whisker raw material sources are wide
General and production cost is low, it might even be possible to is prepared using industrial residue, is expected to become most important inorganic crystal whisker material.
At present, numerous studies have been done in preparation of the domestic and foreign scholars to aragonite calcium carbonate whisker, mainly there is five class preparation methods：
(1) double decomposition；(2)Ca(HCO3)2Thermal decomposition method；(3) ureal antigen；(4) sol-gel process；(5) carbonation method.Wherein
Carbonation method is domestic and international most study also a kind of more mature method, since preparation process is simple, cost is low, is expected to earliest
Realize the industrialization of calcium carbonate.
Rapid to the Morphology Control Technology progress of calcium carbonate product both at home and abroad, researcher has synthesized a variety of crystalline substances
It is the calcium carbonate of shape, such as spindle, cube, chain, sheet, spherical, needle-shaped, but multi-arm whisker is rarely found.By to structure
Analysis it was found that multi-arm whisker has the advantage of bigger in lifting chemical property and mechanical property etc., due to multi-arm
The functional group of structure whisker is more compared with single whisker, and its " pinning " effect is stronger as filler, thus chemical property and mechanical property
Can all more rod-shaped whisker it is more excellent.Therefore our goal in research is exactly to find a kind of preparation side of more arm calcium carbonate crystal whiskers
Method, it is contemplated that continuing the position of crystallization on increase whisker can cause whisker growth to become more arm configurations, we are attempted using double
The device of pipe ventilation is tested, and based on carbonation method, prepares the calcium carbonate crystal whisker of multi-arm.Verified, prepared by this method crystalline substance
Must be more arm configurations, and the branch arm number of whisker can be controlled by according to reaction condition.
The content of the invention
The object of the present invention is to provide a kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern, it is characterized in that utilizing
Carbonation method, using the device of two-tube ventilation, synthesizes multi-arm calcium carbonate crystal whisker, and the branch arm number for obtaining whisker is 2~16.It is specific real
It is now as follows：
Step 1, a certain amount of calcium oxide is weighed, is added to the Ca for obtaining that concentration is 0.1-0.3mol/L in deionized water
(OH)2Suspension, heating make its digestion；
Step 2, magnesium chloride is weighed as crystal control agent, is dissolved in water, and magnesium chloride solution is added to postdigestive
Ca(OH)2In suspension, stirring makes its uniform；
Step 3, carbon dioxide is passed through to reaction unit bottom using double-tube air breather, carry out carbonation reaction,
Gained precipitation is filtered after having reacted, is washed, it is dry, obtain sample.
In above-mentioned technical proposal, the temperature of hot digestion is 70~100 DEG C in the step 1.
The addition of magnesium chloride is to make magnesium calcium molar ratio be 1 in the step 2:1~2.5:1.
Carbon dioxide flux is usually 60~150ml/min in the step 3.
Double-tube air breather described in the step 3 can use three neck round bottom flask, and carbon dioxide is from its both sides
Opening enters in round-bottomed flask at the same time.
Preferably, the carbonation reaction time is 2~3h in the step 3, and the branch arm number of gained sample calcium carbonate crystal whisker is 2
~16, the branch arm number of whisker is different and different with the reaction time, is 2h such as when the carbonation reaction time, obtains product with containing 4
It is 2.5h when the carbonation reaction time based on the whisker of branch arm, obtains product based on the whisker containing 5-7 branch arm, work as carbonic acid
The change reaction time is 3h, obtains product based on the whisker containing more than 10 branch arms, can be by regulating and controlling its carbonation reaction duration
To regulate and control calcium carbonate crystal whisker branch arm number.
The present invention compared with the technology for having prepared calcium carbonate crystal whisker, it is prominent the characteristics of and significant progress be：
1. CO is passed through using double-tube air breather2Gas, is conducive to increase the position for continuing crystallization on whisker, increase growth
Point so that whisker growth becomes more arm configurations；
2. the whisker morphology being prepared is multi-arm, and the number of the branch arm of whisker can be with continuous control, more arm configurations
Whisker functional group it is more compared with single whisker, as filler, its " pinning " effect is stronger, has more preferable chemical property and mechanical property
Energy.
Brief description of the drawings
Fig. 1 is 1 whisker electron scanning micrograph of embodiment；
Fig. 2 is 2 whisker electron scanning micrograph of embodiment；
Fig. 3 is 3 whisker electron scanning micrograph of embodiment；
Fig. 4 is double-tube air breather schematic diagram used in the present invention.
Embodiment
Embodiment 1
Step 1：Calcium oxide is added to the Ca (OH) for obtaining that concentration is 0.1mol/L in deionized water2Suspension, at the same time
70 DEG C are heated to, digests 2h；
Step 2：Magnesium chloride is weighed as crystal control agent, it is 1 to make magnesium calcium ratio:1, it is dissolved in water, and by magnesium chloride solution
It is added to postdigestive Ca (OH)2In suspension, stirring 0.5h makes uniformly；Step 3：Using three neck round bottom flask, by 150ml/
The flux of min is passed through CO from both-side opening2Gas to reaction unit bottom carries out carbonation reaction；
Step 4：Carburizing reagent terminates after carrying out 2h, and gained precipitation is filtered, is washed, drying, obtains sample.
The branch arm number of prepared calcium carbonate crystal whisker is mainly 4, its SEM image is shown in Fig. 1.
Embodiment 2
Step 1：Calcium oxide is added to the Ca (OH) for obtaining that concentration is 0.2mol/L in deionized water2Suspension, at the same time
80 DEG C are heated to, digests 2h；
Step 2：Magnesium chloride is weighed as crystal control agent, it is 2 to make magnesium calcium ratio:1, it is dissolved in water, and by magnesium chloride solution
It is added to postdigestive Ca (OH)2In suspension, stirring 0.5h makes uniformly；Step 3：Using three neck round bottom flask, by 100ml/
The flux of min is passed through CO from both-side opening2Gas to reaction unit bottom carries out carbonation reaction；
Step 4：Carburizing reagent terminates after carrying out 2.5h, and gained precipitation is filtered, is washed, drying, obtains sample.
For the branch arm number of prepared calcium carbonate crystal whisker mainly 7 or so, its SEM image is shown in Fig. 2.
Embodiment 3
Step 1：Calcium oxide is added to the Ca (OH) for obtaining that concentration is 0.3mol/L in deionized water2Suspension, at the same time
100 DEG C are heated to, digests 2h；
Step 2：Magnesium chloride is weighed as crystal control agent, it is 2.5 to make magnesium calcium ratio:1, it is dissolved in water, and magnesium chloride is molten
Liquid is added to postdigestive Ca (OH)2In suspension, stirring 0.5h makes uniformly；
Step 3：Using three neck round bottom flask, CO is passed through from both-side opening by the flux of 60ml/min2Gas to react dress
Bottom set portion carries out carbonation reaction；
Step 4：Carburizing reagent terminates after carrying out 3h, and gained precipitation is filtered, is washed, drying, obtains sample.
The branch arm number of prepared calcium carbonate crystal whisker can up to 16, its SEM image is shown in Fig. 3.
Claims (7)
1. a kind of preparation method of the continuous controllable calcium carbonate crystal whisker of pattern, it is comprised the following steps that：
Step 1, a certain amount of calcium oxide is weighed, is added to the Ca (OH) for obtaining that concentration is 0.1-0.3mol/L in deionized water2It is outstanding
Supernatant liquid, heating make its digestion；
Step 2, magnesium chloride is weighed as crystal control agent, is dissolved in water, and magnesium chloride solution is added to postdigestive Ca
(OH)2In suspension, stirring makes its uniform；
Step 3, carbon dioxide is passed through to reaction unit bottom using double-tube air breather, carry out carbonation reaction, reaction
Gained precipitation is filtered after complete, is washed, it is dry, obtain sample.
2. the preparation method of the continuous controllable calcium carbonate crystal whisker of pattern according to claim 1, it is characterised in that：The step
The temperature of hot digestion is 70~100 DEG C in 1.
3. the preparation method of the continuous controllable calcium carbonate crystal whisker of pattern according to claim 1, it is characterised in that：The step
The addition of magnesium chloride is to make magnesium calcium molar ratio be 1 in 2:1~2.5:1.
4. the preparation method of the continuous controllable calcium carbonate crystal whisker of pattern according to claim 1, it is characterised in that：The step
Carbon dioxide flux is 60~150ml/min in 3.
5. the preparation method of the continuous controllable calcium carbonate crystal whisker of pattern according to claim 1, it is characterised in that：The step
Double-tube air breather described in 3 refers to three neck round bottom flask, and carbon dioxide enters round-bottomed flask at the same time from the opening of its both sides
In.
6. the preparation method of the continuous controllable calcium carbonate crystal whisker of pattern according to claim 1, it is characterised in that：The step
The carbonation reaction time is 2~3h in 3.
7. the preparation method of the continuous controllable calcium carbonate crystal whisker of pattern according to claim 6, it is characterised in that：Gained sample
The branch arm number of calcium carbonate crystal whisker is 2~16.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728899A (en) * | 2018-07-16 | 2018-11-02 | 浙江大学 | A method of purity calcium carbonate whisker is mixed with using circulating mother liquor pressurization spray |
| CN108893775A (en) * | 2018-07-16 | 2018-11-27 | 浙江大学 | A kind of preparation method of purity calcium carbonate whisker |
| CN110183126A (en) * | 2019-06-06 | 2019-08-30 | 长沙紫宸科技开发有限公司 | A method of carbonate cementitious material is prepared by raw material of lime stone |
| CN114875494A (en) * | 2022-06-14 | 2022-08-09 | 湖南大学 | Hyperbranched three-dimensional structure calcium carbonate whisker and preparation method and application thereof |
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| KR100720865B1 (en) * | 2005-12-31 | 2007-05-23 | 한국지질자원연구원 | Novel manufacturing method of aragonite calcium carbonate |
| KR101187267B1 (en) * | 2009-02-12 | 2012-10-02 | 포항공과대학교 산학협력단 | Methods for removing of carbondioxide using bisic polymers |
| CN104790024A (en) * | 2015-04-15 | 2015-07-22 | 广西大学 | Preparation method for aragonite calcium carbonate whisker with high length-diameter ratio |
| CN106430272A (en) * | 2016-11-21 | 2017-02-22 | 广西华纳新材料科技有限公司 | Rodlike aragonite calcium carbonate preparation method |
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Patent Citations (4)
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| KR100720865B1 (en) * | 2005-12-31 | 2007-05-23 | 한국지질자원연구원 | Novel manufacturing method of aragonite calcium carbonate |
| KR101187267B1 (en) * | 2009-02-12 | 2012-10-02 | 포항공과대학교 산학협력단 | Methods for removing of carbondioxide using bisic polymers |
| CN104790024A (en) * | 2015-04-15 | 2015-07-22 | 广西大学 | Preparation method for aragonite calcium carbonate whisker with high length-diameter ratio |
| CN106430272A (en) * | 2016-11-21 | 2017-02-22 | 广西华纳新材料科技有限公司 | Rodlike aragonite calcium carbonate preparation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108728899A (en) * | 2018-07-16 | 2018-11-02 | 浙江大学 | A method of purity calcium carbonate whisker is mixed with using circulating mother liquor pressurization spray |
| CN108893775A (en) * | 2018-07-16 | 2018-11-27 | 浙江大学 | A kind of preparation method of purity calcium carbonate whisker |
| CN110183126A (en) * | 2019-06-06 | 2019-08-30 | 长沙紫宸科技开发有限公司 | A method of carbonate cementitious material is prepared by raw material of lime stone |
| CN110183126B (en) * | 2019-06-06 | 2022-02-18 | 长沙紫宸科技开发有限公司 | Method for preparing carbonate cementing material by taking limestone as raw material |
| CN114875494A (en) * | 2022-06-14 | 2022-08-09 | 湖南大学 | Hyperbranched three-dimensional structure calcium carbonate whisker and preparation method and application thereof |
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| CN107916452B (en) | 2020-03-03 |
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