CN108585001A - A kind of layered double hydroxide LDH-CO3-SO42-The preparation method and applications of whisker - Google Patents

A kind of layered double hydroxide LDH-CO3-SO42-The preparation method and applications of whisker Download PDF

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CN108585001A
CN108585001A CN201810276489.3A CN201810276489A CN108585001A CN 108585001 A CN108585001 A CN 108585001A CN 201810276489 A CN201810276489 A CN 201810276489A CN 108585001 A CN108585001 A CN 108585001A
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whisker
ldh
layered double
solution
preparation
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CN108585001B (en
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吴健松
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Lingnan Normal University
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    • 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
    • C01F7/00—Compounds of aluminium
    • C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract

The invention discloses a kind of layered double hydroxide LDH CO3‑SO4 2‑The preparation method and applications of whisker.The preparation method includes the following steps：S1. MgCO is prepared3Solution and Al2(SO4)3Solution, after mixing plus alkali adjusts the pH value of mixed solution to 7.40；S2. 1.40 ~ 1.60 mol/LNa are added in the mixed solution of S12CO3Solution to system pH is 8.0, and evaporative crystallization is complete to precipitating, and every 8.7 ~ 9.3h detects system pH in evaporation process, adds alkali that system pH is made to increase by 0.05, filtration washing precipitation obtains layered double hydroxide LDH CO3‑SO4 2‑The chemical formula of whisker, whisker is Mg6Al2(OH)14CO3SO4·4H2O.The preparation method of the present invention forms the LDH CO with special appearance, composition and crystal structure by controlling rate of charge, pH value of reaction system, reaction temperature and reaction time3‑SO4 2‑Whisker, preparation method is simple and environmentally-friendly, energy-efficient, obtained LDH CO3‑SO4 2‑Whisker can be widely applied in toughened and reinforced material, catalysis material, fire proofing and sorbing material.

Description

A kind of layered double hydroxide LDH-CO3-SO42-The preparation method of whisker and its Using
Technical field
The invention belongs to layered double hydroxide Material Fields, more particularly, to a kind of layered bi-metal hydrogen-oxygen Compound LDH-CO3-SO4 2-The 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 Material.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 bivalent metal ion, such as Mg2+, Ni2+, Co2+, Zn2+, Cu2+；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 layer structure is as shown in Figure 1.
For LDH compounds, research both domestic and external is concentrated mainly in the displacement of sheet-metal layers bivalent cation, such as Magnesium ion is replaced into copper ion or cobalt ions etc., anion metathesis is that some amino acid etc. are organic by the design also having Biomolecule.Beijing University of Chemical Technology devises the intercalations LDH composite materials such as cupric, cobalt, nickel, organic acid, polyacid, in foreign countries Also there are many scholars to have studied LDH technologies of preparing, using LDH as the catalyst organic compound that have synthesized numerous important and Inorganic compound is used as the researchs such as fire retardant, adsorbent.But to currently, to preparing LDH-CO3-SO4 2-The report of whisker is still Retrieval less than, can retrieve LDH is prepared as Whiskers shape report it is also seldom, and its preparation route be mostly with certain crystalline substance Must (such as magnesium hydroxide crystal 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 apply valence 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-CO3-SO4 2-The preparation method of whisker.
Another object of the present invention is to provide LDH-CO prepared by a kind of this method3-SO4 2-Whisker.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-CO3-SO4 2-It is prepared by whisker Application in toughened and reinforced 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-CO3-SO4 2-The preparation method of whisker, includes the following steps：
S1. MgCO is prepared3Solution and Al2(SO4)3Solution, after mixing plus alkali adjusts the pH value of mixed solution to 7.40, Middle Mg2+A concentration of 2.10~2.70mol/L, middle Al3+A concentration of 0.50~0.70mol/L, CO3 2-With SO4 2-Molar ratio be 1: 1；
S2. 1.40~1.60mol/LNa is added in the mixed solution of S12CO3Solution to system pH is 8.0, evaporation Crystallizing to that precipitation is complete, every 8.7~9.3h detects system pH in evaporation process, adds alkali that system pH is made to increase by 0.05, Filtration washing precipitation obtains layered double hydroxide LDH-CO3-SO4 2-The chemical formula of whisker, whisker is Mg6Al2 (OH)14CO3SO4·4H2O。
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-CO that is prepared with reaction time etc.3-SO4 2-Pattern, composition and the crystal structure of whisker generate prodigious It influences, as the layered double hydroxide LDH-CO that can just obtain the present invention under specific preparation condition of the invention3- SO4 2-Whisker.
Preferably, S1Mg2+A concentration of 2.40mol/L, Al3+A concentration of 0.80mol/L.
For low energy consumption, the layered double hydroxide CO of the preparation present invention of clean environment firendly3-SO4 2-Whisker, it is described In lower progress of exposing to the weather, the condition of the evaporation is for evaporation：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 S2 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, MgCO described in S13Solution and Al2(SO4)3The mixed solution of solution is prepared by bittern in salt lake.It is more excellent Selection of land, bittern in salt lake are Qinghai Salt Lake bittern.
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-CO3-SO4 2-The extremely excellent natural resources of whisker.But these resources cannot get always science, high level profit With, but leave unused always, this not only wastes salt lake resources, also so that the serious salination of salt lake Soil Surrounding and plant are withered Extremely, it is damaged to the ecological environment in salt lake, while also bringing difficulty to saltern resource exploitation in future.Make full use of salt lake bitter High-quality Mg in halogen2+And Al3+As preparation LDH- CO3-SO4 2-On the one hand it is excellent can to make good use of salt lake for the raw material sources of whisker Matter resource realizes higher value application, on the other hand protects salt lake ecological environment, is conducive to saltern development of resources.
A kind of layered double hydroxide LDH-CO prepared by the above method3-SO4 2-Whisker, the chemical formula of whisker For Mg6Al2(OH)14CO3SO4·4H2O。
The LDH-CO of the present invention3-SO4 2-Whisker 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, have aperture adjustable Denaturation, is a kind of multifunctional inorganic material of environment-friendly type.
Above-mentioned layered double hydroxide LDH-CO3-SO4 2-Whisker is preparing toughened and reinforced material, catalysis material, resistance Application in combustible material or 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-CO3-SO4 2-Whisker, LDH-CO3-SO4 2-Whiskerizing Object is closed not only with being catalyzed of LDH compounds, fire-retardant and adsorption function, but also has the function of the toughened and reinforced of whisker, tool There is the adjustable denaturation in aperture, is a kind of multifunctional inorganic material of environment-friendly type.The preparation process of the compound is fed intake by control Than, pH value of reaction system, reaction temperature and reaction time form the LDH-CO with special appearance, composition and crystal structure3- SO4 2-Whisker, preparation method is simple and environmentally-friendly, energy-efficient, obtained LDH-CO3-SO4 2-Whisker can be widely applied to toughening benefit In strong material, catalysis material, fire proofing and 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-CO3-SO4 2-The route map of whisker.
Fig. 3 is layered double hydroxide LDH-CO prepared by embodiment 13-SO4 2-The XRD diagram of whisker.
Fig. 4 is 1 layered double hydroxide LDH-CO of embodiment3-SO4 2-The SEM of whisker schemes.
Fig. 5 is layered double hydroxide LDH-CO prepared by comparative example 13-SO4 2-The 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.
Examples 1 to 8
A kind of layered double hydroxide LDH-CO3-SO4 2-Whisker, chemical formula are
Mg6Al2(OH)14CO3SO4·4H2O, preparation method flow is as shown in Figure 1, include the following steps：
S1. MgCO is prepared3Solution and Al2(SO4)3Solution, after mixing plus alkali adjusts the pH value of mixed solution to 7.40；
S2. Na is added in the mixed solution of S12CO3Solution to system pH is 8.0, and evaporation reaction is complete to precipitating, Every 8 detect system pH in evaporation process, add alkali that system pH is made to increase by 0.05, filtration washing precipitation obtains stratiform Double-metal hydroxide LDH-CO3-SO4 2-Whisker.
The wherein MgCO of Examples 1 to 73Solution is by MgCO3·6H2O is prepared, Al2(SO4)3Solution is by Al2(SO4)3· 18H2O is prepared；
The MgCO of embodiment 83Solution and Al2(SO4)3The mixed solution of solution is prepared by Qinghai Salt Lake bittern.
The parameter of specific each embodiment is shown in Table 1, Mg in wherein S12+A concentration of A mol/L, Al3+A concentration of B mol/L；S2 Middle Na2CO3A concentration of C mol/L.
Table 1
Serial number A B C
Embodiment 1 2.40 0.60 1.5
Embodiment 2 2.10 0.60 1.5
Embodiment 3 2.70 0.60 1.50
Embodiment 4 2.40 0.50 1.50
Embodiment 5 2.40 0.70 1.50
Embodiment 6 2.40 0.60 1.40
Embodiment 7 2.40 0.60 1.60
Embodiment 8 2.40 0.60 1.5
Comparative example 1~7
The operating procedure of comparative example is substantially the same manner as Example 1, and chemicals are also same as Example 1, and design parameter value is shown in Table 2.
Table 2
Serial number A B C D
Comparative example 1 2.40 0.4 1.50 8.0
Comparative example 2 2.40 0.8 1.50 8.0
Comparative example 3 2.00 0.80 1.50 8.0
Comparative example 4 2.80 0.80 1.50 8.0
Comparative example 5 2.40 0.80 1.30 8.0
Comparative example 6 2.40 0.80 1.70 8.0
Comparative example 7 2.40 0.80 1.50 9.0
Comparative example 8 2.40 0.80 1.5 0 7.0
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-CO made from embodiment 13-SO4 2-The XRD of whisker Test results are shown in figure 1.The layered double hydroxide LDH-CO obtained of embodiment 2~53-SO4 2-Whisker The test result of XRD is same as Example 1.
As shown in Figure 1, the layered double hydroxide LDH-CO prepared for embodiment 13-SO4 2-The XRD diagram of whisker. From its diffractive features 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 stratiform The LDH-CO of structure3-SO4 2-Layered double hydroxide LDH-CO is can be seen that from its XRD diffraction pattern3-SO4 2-Chemical combination (LDH of layer structure is maximum in (003) crystal face diffracted intensity, followed by (006) crystal face, most for layer structure of the object with LDH Small is (009), this is because caused by " delustring " effect of lamellar compound to XRD.I marked in the accompanying drawings (003), (006), the corresponding diffraction maximum of (009) crystal face.As described above, as long as the XRD diffraction patterns with LDH stratiforms, you can prove it It is exactly the substance with LDH structures, that is, the necessarily general character with LDH.This Shao- general character just need not do experiment again and testify .Sample Scan figure manufactured in the present embodiment is as shown in Figure 1, it is seen that sample has Whiskers shape.The XRD diagram of sample is shown in Fig. 2, It can be seen that sample has the diffraction-type model (i.e. diffraction pattern) of LDH.
(2) Shape measure
The layered double hydroxide LDH-CO of the preparation of embodiment 1 is had detected by scanning electron microscope (SEM)3-SO4 2-It is brilliant The appearance of palpus calculates the layered double hydroxide LDH-CO of preparation by biomicroscope observation3-SO4 2-Whisker Draw ratio.Whisker aspect ratio structures such as the following table 3, LDH-CO prepared by embodiment 13-SO4 2-The scanning electron microscope (SEM) photograph of whisker such as Fig. 3 Show, sample has crystal whisker-shaped, LDH-CO prepared by comparative example 13-SO4 2-The scanning electron microscope (SEM) photograph of whisker such as Fig. 4 does not have whisker shape 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=6:2:1:1, in conjunction with oxygen (content of oxygen is obtained by minusing), protium content, it can deduce that its chemical formula is Mg6Al2 (OH)14CO3SO4·4H2O。
Table 4LDH-CO3-SO4 2-Elemental analysis result
(Mg) % (Al) % (S) % (C) % (H) % Mg/Al/S/C
21.59 8.21 4.84 1.83 3.31 0.900:0.304:0.151:0.153

Claims (8)

1. a kind of layered double hydroxide LDH-CO3-SO4 2-The preparation method of whisker, which is characterized in that including walking as follows Suddenly：
S1. MgCO is prepared3Solution and Al2(SO4)3Solution, after mixing plus alkali adjusts the pH value of mixed solution to 7.40, wherein Mg2 +A concentration of 2.10 ~ 2.70mol/L, Al3+A concentration of 0.50 ~ 0.70 mol/L, CO3 2-With SO4 2-Molar ratio be 1:1；
S2. 1.40 ~ 1.60 mol/LNa are added in the mixed solution of S12CO3Solution to system pH is 8.0, evaporative crystallization Complete to precipitation, every 8.7 ~ 9.3h detects system pH in evaporation process, adds alkali that system pH is made to increase by 0.05, crosses diafiltration It washs precipitation and obtains layered double hydroxide LDH-CO3-SO4 2-The chemical formula of whisker, whisker is Mg6Al2(OH)14CO3SO4·4H2O 。
2. layered double hydroxide LDH-CO as described in claim 13-SO4 2-The preparation method of whisker, which is characterized in that Mg in S12+A concentration of 2.40 mol/L, Al3+A concentration of 0.80 mol/L.
3. layered double hydroxide LDH-CO as described in claim 13-SO4 2-The preparation method of whisker, which is characterized in that In lower progress of exposing to the weather, the condition of the evaporation is for the evaporation：Solution temperature be 5 ~ 45 DEG C, solution surface wind speed be 3 ~ 5m/s。
4. layered double hydroxide LDH-CO as described in claim 13-SO4 2-The preparation method of whisker, which is characterized in that The sodium hydroxide solution that the alkali for adjusting pH is 0.01mol/L.
5. such as 1 layered double-metal hydroxide LDH-CO3-SO4 2-The preparation method of whisker, which is characterized in that described in S1 MgCO3Solution and Al2(SO4)3The mixed solution of solution is prepared by bittern in salt lake.
6. such as 5 layered double-metal hydroxide LDH-CO3-SO4 2-The preparation method of whisker, which is characterized in that the salt lake Bittern is Qinghai Salt Lake bittern.
7. a kind of being required layered double hydroxide LDH-CO prepared by any one of 1 ~ 6 the method by right of appeal3-SO4 2- The chemical formula of whisker, whisker is Mg6Al2(OH)14CO3SO4·4H2O 。
8. the layered double-metal hydroxide LDH-CO of claim 13-SO4 2-Whisker is preparing toughened and reinforced material, catalysis material Application in material, fire proofing or sorbing material.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101187060A (en) * 2007-09-20 2008-05-28 西安电子科技大学 Needle, flake-shaped nano single crystal mg-al hydrotalcite Mg8Al2(OH)16CO3 4H2O preparation method
CN101381890A (en) * 2008-10-10 2009-03-11 西安电子科技大学 Method for producing fibrous basic magnesium chloride Mg2(OH)3Cl.4H2O3monocrystal
CN101717649A (en) * 2009-11-13 2010-06-02 西安电子科技大学 Preparation method of enhanced magnesium-aluminum composite flame retardant
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101187060A (en) * 2007-09-20 2008-05-28 西安电子科技大学 Needle, flake-shaped nano single crystal mg-al hydrotalcite Mg8Al2(OH)16CO3 4H2O preparation method
CN101381890A (en) * 2008-10-10 2009-03-11 西安电子科技大学 Method for producing fibrous basic magnesium chloride Mg2(OH)3Cl.4H2O3monocrystal
CN101717649A (en) * 2009-11-13 2010-06-02 西安电子科技大学 Preparation method of enhanced magnesium-aluminum composite flame retardant
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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