CN108807986A - A kind of preparation method of mineral yellow micro-nano structure crystal - Google Patents
A kind of preparation method of mineral yellow micro-nano structure crystal Download PDFInfo
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- CN108807986A CN108807986A CN201810520316.1A CN201810520316A CN108807986A CN 108807986 A CN108807986 A CN 108807986A CN 201810520316 A CN201810520316 A CN 201810520316A CN 108807986 A CN108807986 A CN 108807986A
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Abstract
The invention discloses a kind of preparation method of mineral yellow micro-nano structure crystal, preparation method belongs to technical field of micro nano material preparation.This method uses deionized water dissolving lead chloride, and triethylamine react is added under Elevated Temperature Conditions, obtains mineral yellow micro-nano structure crystal.The powder of mineral yellow micro-nano structure crystal is obtained by filtering and drying.Prepared mineral yellow micro-nano structure crystal is rodlike, and length range is about 300 nm-1600 nm, and thickness range is about 30 nm-400 nm.Its advantage is that building-up process is simple, reproducible, of low cost, safety and environmental protection.Based on the above feature, the present invention either has very high value in terms of laboratory research or commercial Application.
Description
Technical field
The present invention relates to the preparation fields of mineral yellow, and in particular to a kind of system of mineral yellow micro-nano structure crystal
Preparation Method.
Background technology
In recent years, the large capacity negative material of lithium ion battery becomes one of research hotspot.In the past few years, a variety of
Transition metal oxide has been reported as the large capacity negative material of lithium ion battery, such as CoO, CuO, NiO and MnO etc..But
These material prices are expensive, and manufacturing process is complicated, therefore are difficult to be used as business electrode material.In addition, transition metal
Catalytic action can lead to the decomposition of electrolyte in reduction process.Therefore, other cheap materials with appropriate metallic element should be developed
Material, to meet the requirement of energy-storage battery electrode material.
A few years ago, someone reports electrode material of the mineral yellow as lithium ion battery, with preferable performance table
It is existing.But about the study on the synthesis of mineral yellow, report is seldom.It has been reported that and uniform Pb is prepared for by reverse micelle system
(OH) Cl nanotubes also have been reported that and prepare Pb (OH) Cl nano wires by solvent-thermal method, in addition, also group is prepared for Pb (OH)
The random particle of Cl.But these methods otherwise complex steps, otherwise raw material are more expensive, can not meet scale, it is low at
This industrial requirements.
Invention content
The present invention proposes a kind of preparation method of mineral yellow micro-nano structure crystal, is prepared in aqueous phase system
Mineral yellow (Pb (OH) Cl) micro-nano structure crystal.
Realize the technical scheme is that：A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Lead chloride is add to deionized water, is sufficiently stirred, lead chloride is warming up to and fully dissolves and obtain clear solution, to clear solution
The molar ratio of middle addition triethylamine, triethylamine and lead chloride is（0.1-5）：3, white flock precipitate is obtained, through filtering, drying,
Obtain mineral yellow micro-nano structure crystal.
The size of the mineral yellow micro-nano structure crystal is 30 nm-1.6 μm.
The lead chloride is add to deionized water, and is sufficiently stirred, and is warming up to 40-90 DEG C so that lead chloride fully dissolves
To clear solution.
The chemical formula of the mineral yellow is Pb (OH) Cl.
The beneficial effects of the invention are as follows：Method process is simple, easy to operation, and the solvent used is water, and environmental protection is at low cost.
Mineral yellow (Pb (OH) Cl) micro-nano structure crystal of preparation has good dispersion, and good crystallinity, quality is high, and size is more equal
It is even, the advantages that stability is good.This method either all has huge application value in laboratory synthesis or commercial synthesis.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Obtain other attached drawings according to these attached drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph (a) of mineral yellow crystal prepared by embodiment 1, x-ray diffraction（XRD）Figure（b）,
With absorption spectrum (c).
Fig. 2 is the scanning electron microscope (SEM) photograph (a) of mineral yellow crystal prepared by embodiment 2, XRD（b）.
Fig. 3 is the scanning electron microscope (SEM) photograph (a) of mineral yellow crystal prepared by embodiment 3, XRD（b）.
Fig. 4 is the scanning electron microscope (SEM) photograph (a) of mineral yellow crystal prepared by embodiment 4, XRD（b）.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical scheme of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
The every other embodiment that those of ordinary skill in the art are obtained under the premise of not making the creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, are stirred and heated to 60oC forms clear
Solution.3 mmol are added（0.42 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops adding
Solution is cooled to room temperature by heat.And by filtering, after dry, solid powder is obtained.（Scanning electron microscope (SEM) photograph, X-ray diffractogram and
Absorption spectrum is respectively such as Fig. 1 a, 1b and 1c）.
In terms of the XRD diffraction patterns of product, peak position be located at 2 θ=15.370 °, 18.201 ° 22.150 °, 23.901 °,
24.992°、26.667°、27.080°、30.304°、31.148°、31.474°、33.626°、34.910°、35.567°、
36.962°、37.522°、37.833°、38.524°、39.116°、42.401°、43.983°、45.346°、48.307°、
50.773 °, 52.251 °, 53.938 °, 55.820 °, 56.587 °, 59.152 °, 61.186 °, 63.049 °, 63.608 °, respectively
The corresponding indices of crystallographic plane are（101）,（002）,（102）,（011）,（200）,（201）,（111）,（103）,（202）,（112）,
（210）,（211）,（013）,（004）,（203）,（113）,（212）,（301）,（302）,（213）,（311）,（312）,
（122）,（220）,（115）,（222）,（410）,（314）,（321）,（206）,（322）.The corresponding peak position position of the angle of diffraction with
PDF numbers are that Pb corresponding to 89-0623 (OH) Cl is consistent, structure cell basic vector a=7.112, b=4.019, c=9.714.When spreading out
When 2 θ=22.150 ° of firing angle are with 27.080 °, corresponding there are two highest peaks.And as can be seen that peak shape is very sharp from diffraction pattern
It is sharp and without other miscellaneous peaks, illustrate that the purity of product is high, advantages of good crystallization, without apparent impurity.
Scanning electron microscope result shows that product is small rodlike, and spillikin length range is about the nm of 300 nm ~ 1600, thickness range
The about nm of 30 nm ~ 400.There are two characteristic absorption peaks in 407 nm and 277 nm for absorption spectrum.
Embodiment 2
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, are stirred and heated to 60oC forms clear
Solution.1 mmol is added（0.14 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops adding
Solution is cooled to room temperature by heat.And by filtering, after dry, solid powder is obtained.（Scanning electron microscope (SEM) photograph and X-ray diffractogram point
Not such as Fig. 2 a and 2b）.
Embodiment 3
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, are stirred and heated to 60oC forms clear
Solution.2 mmol are added（0.28 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops adding
Solution is cooled to room temperature by heat.And by filtering, after dry, solid powder is obtained.（Scanning electron microscope (SEM) photograph and X-ray diffractogram point
Not such as Fig. 3 a and 3b）.
Embodiment 4
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, are stirred and heated to 60oC forms clear
Solution.4 mmol are added（0.56 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops adding
Solution is cooled to room temperature by heat.And by filtering, after dry, solid powder is obtained.（Scanning electron microscope (SEM) photograph and X-ray diffractogram point
Not such as Fig. 4 a and 4b）.
Embodiment 5
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, be stirred and heated to 40 DEG C, form clear
Solution.0.1 mmol is added（0.014 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops
Heating, solution is cooled to room temperature.And by filtering, after dry, solid powder is obtained.
Embodiment 6
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, be stirred and heated to 80 DEG C, form clear
Solution.2 mmol are added（0.28 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops adding
Solution is cooled to room temperature by heat.And by filtering, after dry, solid powder is obtained.
Embodiment 7
A kind of preparation method of mineral yellow micro-nano structure crystal, steps are as follows：
Synthesize mineral yellow（Pb(OH)Cl）Micro-nano structure crystal.Take the lead chloride of 3 mmol (0.8343 g)（PbCl2）,
It is put into after grinding in the three-necked bottle of 100 mL capacity, 80 mL deionized waters is added, be stirred and heated to 90 DEG C, form clear
Solution.5 mmol are added（0.70 mL）Triethylamine, there is White Flocculus in solution.Reaction after ten minutes, stops adding
Solution is cooled to room temperature by heat.And by filtering, after dry, solid powder is obtained.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (5)
1. a kind of preparation method of mineral yellow micro-nano structure crystal, it is characterised in that steps are as follows：Lead chloride is added to
In deionized water, be sufficiently stirred, be warming up to lead chloride and fully dissolve and obtain clear solution, be added into clear solution triethylamine into
Row reacts, and the molar ratio of triethylamine and lead chloride is（0.1-5）：3 obtain white flock precipitate, and through filtering, drying obtains alkali formula
Lead chloride micro-nano structure crystal powder.
2. the preparation method of mineral yellow micro-nano structure crystal according to claim 1, it is characterised in that：The alkali
Formula lead chloride micro-nano structure crystal is rodlike, and crystal length is 300 nm-1600 nm, and thickness is 30 nm-400 nm.
3. the preparation method of mineral yellow micro-nano structure crystal according to claim 1, it is characterised in that：The chlorination
Lead is add to deionized water, and is sufficiently stirred, and is warming up to 40-90 DEG C and is obtained clear solution so that lead chloride fully dissolves.
4. the preparation method of mineral yellow micro-nano structure crystal according to claim 1, it is characterised in that：The alkali formula
The chemical formula of lead chloride is Pb (OH) Cl.
5. the preparation method of mineral yellow micro-nano structure crystal according to claim 1, it is characterised in that：Clear solution
The middle addition triethylamine react time is 1-60min, and reaction temperature is 40-90 DEG C.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589877A (en) * | 2019-09-24 | 2019-12-20 | 浙江大学 | Preparation method of lead-halogen perovskite |
| CN110697765A (en) * | 2019-11-26 | 2020-01-17 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN111635759A (en) * | 2020-06-16 | 2020-09-08 | 南昌大学 | Preparation method of lead sulfide colloidal quantum dots |
| CN113428892A (en) * | 2021-07-27 | 2021-09-24 | 王伟建 | Simple and controllable preparation method for ultralong hydroxohalic lead ore nanowire |
| CN114315591A (en) * | 2021-07-27 | 2022-04-12 | 王伟建 | Preparation of MAPbX3Method of nanowires |
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| CN102627317A (en) * | 2012-04-01 | 2012-08-08 | 中国科学院新疆理化技术研究所 | Compound-basic lead nitrate and basic lead nitrate nonlinear optical crystal as well as preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110589877A (en) * | 2019-09-24 | 2019-12-20 | 浙江大学 | Preparation method of lead-halogen perovskite |
| CN110589877B (en) * | 2019-09-24 | 2020-11-24 | 浙江大学 | Preparation method of lead-halogen perovskite |
| CN110697765A (en) * | 2019-11-26 | 2020-01-17 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN110697765B (en) * | 2019-11-26 | 2022-04-29 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN111635759A (en) * | 2020-06-16 | 2020-09-08 | 南昌大学 | Preparation method of lead sulfide colloidal quantum dots |
| CN111635759B (en) * | 2020-06-16 | 2021-08-06 | 南昌大学 | Preparation method of lead sulfide colloidal quantum dots |
| CN113428892A (en) * | 2021-07-27 | 2021-09-24 | 王伟建 | Simple and controllable preparation method for ultralong hydroxohalic lead ore nanowire |
| CN114315591A (en) * | 2021-07-27 | 2022-04-12 | 王伟建 | Preparation of MAPbX3Method of nanowires |
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