CN108611683A - A kind of layered double hydroxide LDH-Cl4The preparation method and applications of whisker - Google Patents
A kind of layered double hydroxide LDH-Cl4The preparation method and applications of whisker Download PDFInfo
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- 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
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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Abstract
The present invention relates to a kind of layered double hydroxide LDH Cl4The preparation method and applications of whisker.The preparation method includes the following steps：S1. MgCl is prepared2Solution and AlCl3Solution, after mixing plus alkali adjusts the pH value of mixed solution to 7.50；S2. mixed solution evaporative crystallization in above-mentioned S1 is complete to precipitating, every 7.7 ~ 8.3h detects system pH in evaporation process, adds the NaOH solution of 0.02mol/L that system pH is made to increase by 0.05, filtration washing precipitation obtains layered double hydroxide LDH Cl4Whisker.Preparation method provided by the invention forms the LDH Cl with special appearance, composition and crystal structure by controlling rate of charge, pH value of reaction system, reaction temperature and reaction time4Whisker, preparation method is simple and environmentally-friendly, energy-efficient, obtained LDH Cl4Whisker can be widely applied in toughened and reinforced material, catalysis material, fire proofing and sorbing material.
Description
Technical field
The invention belongs to layered double hydroxide Material Fields, more particularly, to a kind of layered bi-metal hydrogen-oxygen
Compound LDH-Cl4The preparation method and applications of whisker.
Background technology
Layered double hydroxide (Layered Double Hydroxide, LDH) is hydrotalcite
The general designation of (Hydrotalcite, HT) and houghite compound (Hydrotalcite-Like Compounds, HTLc) is
A kind of important inorganic functional material has the function of catalysis, absorption, fire-retardant etc., is a kind of multifunctional inorganic material of environment-friendly type.
Most typical LDH is Mg6Al2(OH)16CO3.4H2O, also referred to as magnalium hydrotalcite, if the Mg in this magnalium hydrotalcite2+、A13+Or
CO3 2-Ion is replaced by other ions, you can obtains houghite (HTLc).
The general formula of HTLc is：(wherein M2+For divalent
Metal ion, such as Mg2+、Ni2+、Co2+、Zn2+、Cu2+Deng；M3+For trivalent metal ion, such as Al3+、Cr3+、Fe3+、Sc3+Deng；A is
Interlayer anion, such as CO3 2-、NO3-、Cl-、SO4 2-、 PO4 3-、C6H4(COO)2 2-Deng；M is Coating combination water number mesh), byThe plate layer formed is known as sheet-metal layers, byThe layer of composition is known as anion layer, this stratiform
Structure is as shown in Fig. 1.
For LDH compounds, research both domestic and external is concentrated mainly in the displacement of sheet-metal layers bivalent cation, such as will
Magnesium ion is replaced into copper ion or cobalt ions etc., and anion metathesis is the organic-biologicals such as some amino acid by the design also having
Molecule.Beijing University of Chemical Technology devises the intercalations LDH composite materials such as cupric, cobalt, nickel, organic acid, polyacid, also has very in foreign countries
More scholars have studied LDH technologies of preparing, the organic compound and inorganic chemical that have synthesized numerous as catalyst using LDH important
Object is used as the researchs such as fire retardant, adsorbent.But to currently, to preparing LDH-Cl4The report of whisker is still retrieved less than can examine
Rope is also seldom to the report that LDH is prepared as to Whiskers shape, and its preparation route is mostly with certain whisker (such as magnesium hydroxide
Whisker) as predecessor, technology of preparing route is tediously long, of high cost etc..
Therefore, a kind of LDH compounds of simple and practicable crystal whisker-shaped of exploitation have great research significance and application value.
Invention content
Present invention aims to overcome that it is tediously long to prepare crystal whisker-shaped LDH compounding techniques routes in the prior art, manufacturing cost
The deficiencies of high, provides a kind of layered double hydroxide LDH-Cl4Crystal whisker preparation method.
Another object of the present invention is to provide a kind of layered double hydroxide LDH-Cl prepared by this method4
Whisker.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl4Whisker is preparing toughening benefit
Application in strong material, catalysis material, fire proofing or sorbing material.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of layered double hydroxide LDH-Cl4The preparation method of whisker is：
S1. MgCl is prepared2·6H2O solution and AlCl3·6H2O solution, after mixing plus alkali adjusts the pH value of mixed solution
To 7.50, wherein Mg2+A concentration of 2.10~2.70mol/L, middle Al3+A concentration of 0.80~1.00mol/L；
S2. mixed solution evaporative crystallization in above-mentioned S1 is complete to precipitating, every 7.7~8.3h is detected in evaporation process
System pH adds the NaOH solution of 0.02mol/L that system pH is made to increase by 0.05, and filtration washing precipitation obtains layered bi-metal
Hydroxide LDH-Cl4The chemical formula of whisker, whisker is Mg6Al2(OH)14Cl4·4H2O。
In the preparation process that stumbles in inventor's heuristic process to rate of charge, pH value of reaction system, reaction temperature
It all can be to the LDH-Cl that is prepared with reaction time etc.4Pattern, composition and the crystal structure of whisker have a huge impact, until
In the layered double hydroxide LDH-Cl that can just obtain the present invention under specific preparation condition of the invention4Whisker.
Preferably, S1Mg2+A concentration of 2.40mol/L, Al3+A concentration of 0.80mol/L.
The alkali that pH is adjusted in S1 is the sodium hydroxide solution of 0.02mol/L.
For low energy consumption, the layered double hydroxide LDH-Cl of the preparation present invention of clean environment firendly4Whisker, the steaming
In lower progress of exposing to the weather, the condition of the evaporation is hair：Solution temperature is 5~45 DEG C, and solution surface wind speed is 3~5m/s.
Qinghai Salt Lake area has abundant solar energy resources and wind energy resources, and long-term temperature is at 4~45 DEG C, and wind speed is 3
The reaction system of S3 can be placed at the spaciousness of Qinghai Salt Lake area, be realized using natural solar energy and wind energy resources by~5m/s
Moisture slow evaporation not only saves energy and realizes green chemical industry.
Preferably, MgCl described in S12Solution and AlCl3Solution
Qinghai Salt Lake (such as Hoh Yanhu bittern, Chaka Salt lake bittern or Cha Er Han Salt Lake) has the bittern of enormous amount, this
A little bitterns are to prepare LDH-Cl4The extremely excellent natural resources of whisker.But these resources cannot get always science, high-value-use, but
It leaves unused always, this not only wastes salt lake resources, also so that the serious salination of salt lake Soil Surrounding and plant are withered, gives salt lake
Ecological environment damage, while also bringing difficulty to saltern resource exploitation in future.It makes full use of high-quality in bittern in salt lake
Mg2+And Al3+As preparation LDH-Cl4On the one hand the raw material sources of whisker can make good use of salt lake high-quality resource, realize high-valued
It utilizes, on the other hand protects salt lake ecological environment, be conducive to saltern development of resources.
A kind of layered double hydroxide LDH-Cl for thering is the above method to prepare4The chemical formula of whisker, whisker is
Mg6Al2(OH)14Cl4·4H2O。
The LDH-Cl of the present invention4Whisker not only has the function of being catalyzed of LDH compounds, fire-retardant and absorption, has larger
Specific surface area and interlayer ion interchangeability, but also have the function of the toughened and reinforced of whisker, there is the adjustable denaturation in aperture, be
A kind of multifunctional inorganic material of environment-friendly type.
Above-mentioned layered double hydroxide LDH-Cl4Whisker is preparing toughened and reinforced material, catalysis material, fire proofing
Or the application in sorbing material is also within protection scope of the present invention.
Compared with prior art, the present invention has the advantages that：
The present invention provides a kind of layered double hydroxide LDH-Cl4Whisker, LDH-Cl4Whisker compound not only has
There are being catalyzed of LDH compounds, fire-retardant and adsorption function, but also have the function of the toughened and reinforced of whisker, has aperture adjustable
Denaturation, is a kind of multifunctional inorganic material of environment-friendly type.The preparation process of the compound is by controlling rate of charge, reaction system pH
Value, reaction temperature and reaction time form the LDH-Cl with special appearance, composition and crystal structure4Whisker, preparation method letter
Monocycle is protected, energy-efficient, obtained LDH-Cl4Whisker can be widely applied to toughened and reinforced material, catalysis material, fire proofing and
In sorbing material.
Description of the drawings
Fig. 1 is the layer structure schematic diagram of HTLc.
Fig. 2 is to prepare layered double hydroxide LDH-Cl4The route map of whisker.
Fig. 3 is layered double hydroxide LDH-Cl prepared by embodiment 14The XRD diagram of whisker.
Fig. 4 is 1 layered double hydroxide LDH-Cl of embodiment4The SEM of whisker schemes.
Fig. 5 is layered double hydroxide LDH-Cl prepared by comparative example 14The SEM of whisker schemes.
Specific implementation mode
With reference to embodiment, the present invention will be further described.These embodiments are retouched to the typical case of the present invention
It states, however, the present invention is not limited thereto.Test method as used in the following examples is conventional method unless otherwise specified；Made
Raw materials and reagents etc. are unless otherwise specified that can be commercially available from conventional commercial sources.
Embodiment 1
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula Mg6Al2(OH)14Cl4·4H2O.Preparation side
Method flow is as shown in Fig. 2, include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.40mol/L, middle Al3+A concentration of 0.80mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitation obtains layered double hydroxide LDH-Cl4Whisker.
Above-mentioned evaporation process is 40 DEG C in solution temperature, and solution surface wind speed carries out under conditions of being 4m/s.
Embodiment 2
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. Qinghai Salt Lake bittern is used to prepare MgCl2Solution and AlCl3Solution takes this two kinds of solution in the inferior body of stirring
Product is mixed in a beaker, and the pH value of mixed system is adjusted to pH=7.50, wherein Mg with the NaOH solution of 0.01mol/L2+
A concentration of 2.20mol/L, middle Al3+A concentration of 0.90mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitation obtains layered double hydroxide LDH-Cl4Whisker.
Above-mentioned evaporation process is 10 DEG C in solution temperature, and solution surface wind speed carries out under conditions of being 5m/s.
Embodiment 3
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.60mol/L, middle Al3+A concentration of 0.90mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitation obtains layered double hydroxide LDH-Cl4Whisker.
Embodiment 4
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.10mol/L, middle Al3+A concentration of 0.80mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitation obtains layered double hydroxide LDH-Cl4Whisker.
Comparative example 1
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.00mol/L, middle Al3+A concentration of 0.80mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitates.
Comparative example 2
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.80mol/L, middle Al3+A concentration of 0.80mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitates.
Comparative example 3
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.40mol/L, middle Al3+A concentration of 0.70mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitates.
Comparative example 4
A kind of layered double hydroxide LDH-Cl4Whisker, chemical formula be, preparation method flow as shown in Fig. 2,
Include the following steps：
S1. MgCl is used2·6H2O prepares MgCl2Solution uses AlCl3·6H2O prepares AlCl3Solution takes this two kinds of solution to exist
Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01 mol/L
=7.50, wherein Mg2+A concentration of 2.40mol/L, middle Al3+A concentration of 1.10mol/L；
S2. the NaOH solution for preparing 0.02mol/L, is added in batches in above-mentioned mixed system, is added every 8 hours
Once, the amount being added every time is：The pH value for first measuring current arrangements, then adds alkali so that and pH value increases by 0.05 unit,
Filtration washing precipitates.
As a result it detects
(1) whisker structure detects
The whisker knot that embodiment 1 is prepared is detected by X-ray diffraction (XRD) detection.
It is tested by XRD, it is known that layered double hydroxide LDH-Cl made from embodiment 14The survey of the XRD of whisker
Test result is as shown in Figure 3.The layered double hydroxide LDH-Cl obtained of embodiment 2~54The test knot of the XRD of whisker
Fruit is same as Example 1.
It is tested by XRD, it is known that layered double hydroxide LDH-Cl made from embodiment 14The survey of the XRD of whisker
Test result is as shown in Figure 3.The layered double hydroxide LDH-Cl obtained of embodiment 2~54The test knot of the XRD of whisker
Fruit is same as Example 1.
As shown in figure 3, layered double hydroxide LDH-Cl prepared by embodiment 14The XRD diagram of whisker.From its diffraction
For characteristic peak it is found that sample peak shape is sharp, position and the intensity of each main diffraction peak show that the substance is with layer structure
LDH-Cl4Layered double hydroxide LDH-Cl is can be seen that from its XRD diffraction pattern4Compound has the stratiform knot of LDH
Structure (for the LDH of layer structure in (003) crystal face diffracted intensity maximum, followed by (006) crystal face, minimum is (009), this be by
Caused by " delustring " effect of lamellar compound to XRD.As long as the XRD diffraction patterns with LDH stratiforms, you can prove that it is exactly
Substance with LDH structures, that is, the necessarily general character with LDH.The visible sample of XRD diagram of sample has the diffraction of LDH
Formula model (i.e. diffraction pattern).
(2) Shape measure
The layered double hydroxide LDH-Cl of the preparation of embodiment 1 is had detected by scanning electron microscope (SEM)4The phase of whisker
Looks calculate the layered double hydroxide LDH-Cl of preparation by biomicroscope observation4The draw ratio of whisker.Whisker is long
Diameter is than LDH-Cl prepared by structure such as the following table 3, embodiment 14The scanning electron microscope (SEM) photograph of whisker such as Fig. 4 shows that sample has crystal whisker-shaped, comparison
LDH-Cl prepared by example 14The scanning electron microscope (SEM) photograph of whisker such as Fig. 5 does not have Whiskers shape.
Table 3
(3) composition detection
Elemental analysis of samples result acquired results are listed in table 4, table 4 statistics indicate that, sample substantially conforms to nMg:nAl:nS:
nC=3:1:2, in conjunction with oxygen (content of oxygen is obtained by minusing), protium content, it can deduce that its chemical formula is Mg6Al2
(OH)14Cl4·4H2O。
4 LDH-Cl of table4L elemental analysis results
| ω (Mg) % | ω (Al) % | ω (Cl) % | ω (H) % | Mg/Al/Cl |
| 22.21 | 8.38 | 21.79 | 3.39 | 0.925:0.310:0.614 |
Claims (8)
1. a kind of layered double hydroxide LDH-Cl4The preparation method of whisker, which is characterized in that include the following steps：
S1. MgCl is prepared2Solution and AlCl3Solution, after mixing plus alkali adjusts the pH value of mixed solution to 7.50, wherein Mg2+It is dense
Degree is 2.1 ~ 2.7 mol/L, middle Al3+A concentration of 0.8 ~ 1.0 mol/L；
S2. mixed solution evaporative crystallization in above-mentioned S1 is complete to precipitating, every 7.7 ~ 8.3h detects system in evaporation process
PH adds the NaOH solution of 0.02mol/L that system pH is made to increase by 0.05, and filtration washing precipitation obtains layered bi-metal hydrogen-oxygen
Compound LDH-Cl4The chemical formula of whisker, whisker is Mg6Al2(OH)14Cl4·4H2O。
2. layered double hydroxide LDH-Cl as described in claim 14The preparation method of whisker, which is characterized in that S1
Mg2+A concentration of 2.40 mol/L, Al3+A concentration of 0.80 mol/L.
3. layered double hydroxide LDH-Cl as described in claim 14The preparation method of whisker, which is characterized in that the steaming
In lower progress of exposing to the weather, the condition of the evaporation is hair：Solution temperature is 5 ~ 45 DEG C, and solution surface wind speed is 3 ~ 5m/s.
4. layered double hydroxide LDH-Cl as described in claim 14The preparation method of whisker, which is characterized in that adjusted in S1
The alkali for saving pH is the sodium hydroxide solution of 0.01mol/L.
5. such as 1 layered double-metal hydroxide LDH-Cl4The preparation method of whisker, which is characterized in that MgCl described in S12
Solution and AlCl3The mixed solution of solution is prepared by bittern in salt lake.
6. such as 5 layered double-metal hydroxide LDH-Cl4The preparation method of whisker, which is characterized in that the bittern in salt lake is
Qinghai Salt Lake bittern.
7. a kind of layered double hydroxide LDH-Cl prepared by any one of the claims 1 ~ 6 the method4Whisker,
The chemical formula of whisker is Mg6Al2(OH)14Cl4·4H2O。
8. the layered double-metal hydroxide LDH-Cl of claim 74Whisker is preparing toughened and reinforced material, catalysis material, resistance
Application in combustible material or sorbing material.
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| CN104003452A (en) * | 2014-05-07 | 2014-08-27 | 北京化工大学 | One-dimensional morphology cobalt-aluminum hydrotalcite and its preparation method and electrochemical application |
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| CN103018303A (en) * | 2012-12-29 | 2013-04-03 | 国家烟草质量监督检验中心 | Preparation method of nickel aluminum stratiform dual-metal hydroxide modified electrode |
| CN104003452A (en) * | 2014-05-07 | 2014-08-27 | 北京化工大学 | One-dimensional morphology cobalt-aluminum hydrotalcite and its preparation method and electrochemical application |
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