CN108396386A - A kind of layered double hydroxide LDH-Cl-NO3-SO42-Whisker and its preparation method and application - Google Patents

A kind of layered double hydroxide LDH-Cl-NO3-SO42-Whisker and its preparation method and application Download PDF

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CN108396386A
CN108396386A CN201810310696.6A CN201810310696A CN108396386A CN 108396386 A CN108396386 A CN 108396386A CN 201810310696 A CN201810310696 A CN 201810310696A CN 108396386 A CN108396386 A CN 108396386A
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whisker
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layered double
ldh
mixed solution
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吴健松
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Lingnan Normal University
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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
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • 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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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention belongs to technical field of inorganic material, specifically disclose a kind of layered double hydroxide LDH Cl NO3‑SO4 2‑Whisker and its preparation method and application.The chemical formula of the whisker is Mg6Al2(OH)14ClNO3SO4·5H2O, the whisker pass through metal cation Mg2+、Al3+With anion Cl‑、NO3 ‑、SO4 2‑、OH‑Evaporable water obtains after reacting to precipitate.Layered double hydroxide LDH Cl NO provided by the invention3‑SO4 2‑Whisker is a kind of houghite compound of crystal whisker-shaped, in addition to the houghites class compounds such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeability with aperture, also has the function of crystal whisker toughened reinforcement, there is very extensive application prospect in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material.Preparation method provided by the invention, it is simple for process easy to operate, it is of low cost, it is suitble to large-scale promotion application.

Description

A kind of layered double hydroxide LDH-Cl-NO3-SO42-Whisker and preparation method thereof And application
Technical field
The present invention relates to technical field of inorganic material, and in particular, to a kind of layered double hydroxide LDH-Cl- NO3-SO4 2-Whisker and its preparation method and application.
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 in this magnalium hydrotalcite Mg2+、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+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 claims For sheet-metal layers, byThe layer of composition is known as anion layer.This layer structure can be indicated with Fig. 5.
Since HTLc has the adjustable denaturation in aperture, and there are larger specific surface area and interlayer ion interchangeability, therefore its There is very extensive application prospect in the fields such as catalysis, fire-retardant, absorption, medicine, gene storage.
For LDH, HTLc class compound, the research that domestic and international many is engaged in this respect at present is done a lot of work, and Gratifying achievement is all achieved in respective field.It is both domestic and external to study the displacement for being concentrated mainly on sheet-metal layers bivalent cation On, such as magnesium ion is replaced into copper ion or cobalt ions etc., anion metathesis is some such as amino acid by the design also having Equal organic biomolecules.At home, Beijing University of Chemical Technology achieves prodigious achievement to the research of LDH.They contain in design Prodigious achievement in research is achieved in the intercalations LDH field of compound material such as copper, cobalt, nickel, organic acid, polyacid.At abroad, also having very More scholars synthesize numerous important organic compounds and inorganic chemical on preparing LDH technologies or using LDH as catalyst On object or as many gratifying achievements are also achieved in the researchs such as fire retardant, adsorbent, a large amount of useful realities are provided Test data.But to currently, LDH and HTLc class compounds are mainly laminated structure, LDH the and HTLc classes compound of crystal whisker-shaped is almost Do not report.And there is the inorganic material of crystal whisker-shaped toughened and reinforced function, LDH the or HTLc class compounds for developing crystal whisker-shaped then may be used The preferably toughened and reinforced function of LDH and HTLc classes inorganic material is assigned, to further expand its application.
It is using certain whisker (such as magnesium hydroxide crystal whisker) as predecessor, again that LDH, which is prepared into whisker mostly, at present Or technology of preparing route is tediously long, of high cost etc., is not suitable for large-scale application.Therefore, develop a kind of crystal whisker-shaped LDH and/or HTLc classes compound and its corresponding preparation process have great research significance and application value.
Invention content
The purpose of the invention is to overcome the above-mentioned deficiency of the prior art, a kind of layered double hydroxide is provided LDH-Cl-NO3-SO4 2-Whisker, except classes such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeabilities with aperture Outside the function of hydrotalcite-based compound, also has the function of crystal whisker toughened reinforcement.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl-NO3-SO4 2-The system of whisker Preparation Method.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker is being made Application in standby toughened and reinforced material, catalysis material, fire proofing or sorbing material.
To achieve the goals above, the present invention is achieved by following scheme：
A kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, chemical formula Mg6Al2(OH)14ClNO3SO4·5H2O。
Preferably, the whisker passes through metal cation Mg2+、Al3+With anion Cl-、NO3 -、SO4 2-、OH-React heavy Evaporable water obtains behind shallow lake.
The present invention provides a kind of layered double hydroxide LDH-Cl-NO of specific composition3-SO4 2-Whisker, the object Matter is crystal whisker-shaped, and the draw ratio of whisker is 15~25:1, good dispersion, good crystalline has caused by the typical structure of whisker Toughened and reinforced function；In addition, adjustable denaturation, larger specific surface area and layer also with aperture possessed by HTLc class compounds Between ion interchangeability function, have in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material very extensive Application prospect.
Layered double-metal hydroxide LDH-Cl-NO3-SO4 2-The preparation method of whisker, includes the following steps：
S1. MgCl is prepared2·6H2O、MgSO4·7H2O and Al (NO3)3·9H2The mixed solution A of O, with 0.05~ The NaOH solution of 0.15mol/L adjusts pH to 7.45~7.55；Mg in the mixed solution A2+A concentration of 2.5~3.1mol/ L, Al3+A concentration of 0.6~0.9mol/L；
S2. NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1mol/L, NaOH A concentration of 0.01~0.05mol/L；Mixed solution B is added into mixed solution A obtained by S1 and adjusts pH to 8.05~8.35 Afterwards, it is placed at 5~45 DEG C and reacts 178~186h generation precipitations, filter and wash precipitation, up to layered bimetallic after drying Hydroxide LDH-Cl-NO3-SO4 2-Whisker.
The present inventor is to layered double hydroxide LDH-Cl-NO3-SO4 2-It is sent out unintentionally in the exploration of preparation process Existing, raw material and its proportioning, pH regulation and control, reaction temperature and time have very big shadow to the pattern of final layered double hydroxide It rings.Such as metal cation Mg2+And Al3+, anion Cl-、NO3 -、SO4 2-And OH-Concentration it is excessive or too small, pH is excessively high or pH waves Dynamic range is excessive, and reaction temperature excessively high (water evaporation rate is too fast) is unable to get whisker morphology or obtains the production of whisker morphology Rate is very low.The present invention finally prepares the layered double hydroxide of crystal whisker-shaped by the preferred of this series of conditions LDH-Cl-NO3-SO4 2-, preparation method is simple.
In addition, Qinghai Salt Lake (such as Hoh Yanhu bittern, Chaka Salt lake bittern or Cha Er Han Salt Lake) has the hardship of enormous amount Halogen, these bitterns are to prepare LDH-Cl-NO3-SO4 2-The extremely excellent natural resources of whisker.But these resources cannot get always science, It efficiently uses, but leaves unused always, this not only wastes salt lake resources, also so that the serious salination of salt lake Soil Surrounding and plant Object is withered, is damaged to the ecological environment in salt lake, while also bringing difficulty to saltern resource exploitation in future.Utilize bittern in salt lake As Mg2+And Al3+Source, the natural resources can be made full use of, it is cost-effective, have important economic value.
Preferably, the MgCl2·6H2O、MgSO4·7H2O can derive from Qinghai Salt Lake bittern.
Preferably, pH to 7.5 is adjusted in S1.
Preferably, Mg in mixed solution A described in S12+A concentration of 2.8mol/L, Al3+A concentration of 0.6mol/L.
Preferably, a concentration of 0.1mol/L of NaOH solution described in S1.
Preferably, in mixed solution B described in S2 NaOH a concentration of 0.02mol/L.
Preferably, NaOH solution is added in S2 and adjusts pH to 8.1.
In order to preferably regulate and control pH, prevents pH too low or fluctuation is excessive, it is preferable that by adding NaNO in S23And NaOH Solution keeps the pH of mixed solution, and NaNO is added every 8h3And NaOH solution so that pH value of reaction system increases 0.05。
It is carried out to enable reaction to stablize at 5~45 DEG C, it is preferable that the reaction time described in S2 is to expose to the weather The wind speed of 182h, the wind are 4~5m/s.
Qinghai Salt Lake area has abundant solar energy resources and wind energy resources, and long-term temperature is at 5~45 DEG C, and wind speed is 4 Therefore the reaction system of S2 can be placed at the spaciousness of Qinghai Salt Lake area, be provided using natural solar energy and wind energy by~5m/s Moisture slow evaporation is realized in source, is not only saved energy and is realized green chemical industry.
Layered double-metal hydroxide LDH-Cl-NO is also claimed in the present invention3-SO4 2-Whisker is preparing toughening benefit Application in strong material, catalysis material, fire proofing or sorbing material.
Compared with prior art, the invention has the advantages that：
Layered double hydroxide LDH-Cl-NO provided by the invention3-SO4 2-Whisker is a kind of class neatly of crystal whisker-shaped Stone compound, except houghites classes such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeabilities with aperture Outside the function of closing object, also has the function of crystal whisker toughened reinforcement, in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material In have very extensive application prospect.Preparation method provided by the invention, it is simple for process easy to operate, it is of low cost, it is suitble to big Scale promotes and applies.
Description of the drawings
Fig. 1 is that embodiment 1 prepares layered double hydroxide LDH-Cl-NO3-SO4 2-The route map of whisker.
Fig. 2 is layered double hydroxide LDH-Cl-NO prepared by embodiment 13-SO4 2-The SEM spectrum of whisker.
Fig. 3 is layered double hydroxide LDH-Cl-NO prepared by comparative example 13-SO4 2-SEM spectrum.
Fig. 4 is layered double hydroxide LDH-Cl-NO prepared by embodiment 13-SO4 2-The XRD spectrum of whisker.
Fig. 5 is the layer structure figure of LDH.
Specific implementation mode
With reference to the accompanying drawings of the specification and specific embodiment is made the present invention and is further elaborated, the embodiment It is served only for explaining the present invention, be not intended to limit the scope of the present invention.Test method used in following embodiments is such as without spy Different explanation, is conventional method；Used material, reagent etc., unless otherwise specified, for the reagent commercially obtained And material.
Embodiment 1
Present embodiments provide a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, chemical formula are Mg6Al2(OH)14ClNO3SO4·5H2O, preparation process are following (as shown in Figure 1)：
1,4.8mol/L MgCl are prepared2·6H2O、3.6mol/L MgSO4·7H2O and 1.8mol/L Al (NO3)3· 9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and the pH value of mixed system is used The NaOH solution of 0.1mol/L is adjusted to pH=7.50, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate This phenomenon does not interfere with follow-up LDH-Cl-NO3-SO4 2-The growth of whisker.
2, NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1.0mol/L, A concentration of 0.02mol/L of NaOH is added in the mixed solution A obtained by previous step, adds to the pH of system always while stirring To pH=8.1；Then by system be placed in sun-drenched place allowed (at 5~45 DEG C) expose to the weather 182h after generate precipitate, mistake It filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl-NO after drying3-SO4 2-Whisker.This 182h when Between in, every 8h be added a NaNO3With NaOH solution (i.e. mixed solution B), the amount being added every time is：First measure current arrangements PH value, mixed solution B is then added so that pH value increases by 0.05 unit and measured at this time for example, after the 90h that exposes to the weather System pH is 8.25, then the alkali being added, which is added to always when system pH is 8.3, to be terminated.
The layered double hydroxide LDH-Cl-NO that the present embodiment is prepared3-SO4 2-The draw ratio of whisker is 18： 1, good dispersion, whisker good crystalline.Layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker in toughened and reinforced material, There is very extensive application prospect in the fields such as catalysis, fire-retardant, sorbing material.
Embodiment 2
Present embodiments provide a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, chemical formula are Mg6Al2(OH)14ClNO3SO4·5H2O, preparation process are as follows：
1,4.4mol/L MgCl are prepared2·6H2O、3.4mol/L MgSO4·7H2O and 1.9mol/L Al (NO3)3· 9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and the pH value of mixed solution A is used The NaOH solution of 0.1mol/L is adjusted to pH=7.5, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this Kind phenomenon does not interfere with follow-up LDH-Cl-NO3-SO4 2-The growth of whisker.
2, NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1.0mol/L, A concentration of 0.02mol/L of NaOH is added in the mixed solution A obtained by previous step, adds to the pH of system always while stirring To pH=8.1；Then by system be placed in sun-drenched place allowed (at 5~45 DEG C) expose to the weather 182h after generate precipitate, mistake It filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl-NO after drying3-SO4 2-Whisker.This 182h when Between in, every 8h be added a NaNO3With NaOH solution (i.e. mixed solution B), the amount being added every time is：First measure current arrangements PH value, mixed solution B is then added so that pH value increases by 0.05 unit and measured at this time for example, after the 90h that exposes to the weather System pH is 8.25, then the alkali being added, which is added to always when system pH is 8.3, to be terminated.
The layered double hydroxide LDH-Cl-NO that the present embodiment is prepared3-SO4 2-The draw ratio of whisker is 19： 1, good dispersion, whisker good crystalline.Layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker in toughened and reinforced material, There is very extensive application prospect in the fields such as catalysis, fire-retardant, sorbing material.
Embodiment 3
Present embodiments provide a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, chemical formula are Mg6Al2(OH)14ClNO3SO4·5H2O, preparation process are as follows：
1,4.8mol/L MgCl are prepared2·6H2O、3.6mol/L MgSO4·7H2O and 1.8mol/L Al (NO3)3· 9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and the pH value of mixed solution A is used The NaOH solution of 0.1mol/L is adjusted to pH=7.51, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate This phenomenon does not interfere with follow-up LDH-Cl-NO3-SO4 2-The growth of whisker.
2, NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1.0mol/L, A concentration of 0.01mol/L of NaOH is added in the mixed solution A obtained by previous step, adds to the pH of system always while stirring To pH=8.1；Then by system be placed in sun-drenched place allowed (at 5~45 DEG C) expose to the weather 182h after generate precipitate, mistake It filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl-NO after drying3-SO4 2-Whisker.This 182h when Between in, every 8h be added a NaNO3With NaOH solution (i.e. mixed solution B), the amount being added every time is：First measure current arrangements PH value, mixed solution B is then added so that pH value increases by 0.05 unit and measured at this time for example, after the 90h that exposes to the weather System pH is 8.25, then the alkali being added, which is added to always when system pH is 8.3, to be terminated.
The layered double hydroxide LDH-Cl-NO that the present embodiment is prepared3-SO4 2-The draw ratio of whisker is 21： 1, good dispersion, whisker good crystalline.Layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker in toughened and reinforced material, There is very extensive application prospect in the fields such as catalysis, fire-retardant, sorbing material.
Embodiment 4
Present embodiments provide a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, chemical formula are Mg6Al2(OH)14ClNO3SO4·5H2O, preparation process are as follows：
1,4.8mol/L MgCl are prepared2·6H2O、3.6mol/L MgSO4·7H2O and 1.8mol/L Al (NO3)3· 9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and the pH value of mixed solution A is used The NaOH solution of 0.1mol/L is adjusted to pH=7.5, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this Kind phenomenon does not interfere with follow-up LDH-Cl-NO3-SO4 2-The growth of whisker.
2, NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1.0mol/L, A concentration of 0.01mol/L of NaOH is added in the mixed solution A obtained by previous step, adds to the pH of system always while stirring To pH=8.3；Then by system be placed in sun-drenched place allowed (at 5~45 DEG C) expose to the weather 182h after generate precipitate, mistake It filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl-NO after drying3-SO4 2-Whisker.This 182h when Between in, every 8h be added a NaNO3With NaOH solution (i.e. mixed solution B), the amount being added every time is：First measure current arrangements PH value, mixed solution B is then added so that pH value increases by 0.05 unit and measured at this time for example, after the 90h that exposes to the weather System pH is 8.25, then the alkali being added, which is added to always when system pH is 8.3, to be terminated.
The layered double hydroxide LDH-Cl-NO that the present embodiment is prepared3-SO4 2-The draw ratio of whisker is 18： 1, good dispersion, whisker good crystalline.Layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker in toughened and reinforced material, There is very extensive application prospect in the fields such as catalysis, fire-retardant, sorbing material.
Embodiment 5
Present embodiments provide a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, chemical formula are Mg6Al2(OH)14ClNO3SO4·5H2O, preparation process are as follows：
1,4.8mol/L MgCl are prepared2·6H2O、3.6mol/L MgSO4·7H2O and 1.8mol/L Al (NO3)3· 9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and the pH value of mixed solution A is used The NaOH solution of 0.1mol/L is adjusted to pH=7.5, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this Kind phenomenon does not interfere with follow-up LDH-Cl-NO3-SO4 2-The growth of whisker.
2, NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1mol/L, NaOH A concentration of 0.05mol/L, be added to while stirring in the mixed solution A obtained by previous step, add to the pH to pH of system always =8.1；Then by system be placed in sun-drenched place allowed (at 5~45 DEG C) expose to the weather 179h after generate precipitate, filtering simultaneously Washing precipitation, up to layered double-metal hydroxide LDH-Cl-NO after drying3-SO4 2-Whisker.In the time of this 179h In, a NaNO is added every 8h3With NaOH solution (i.e. mixed solution B), the amount being added every time is：First measure current arrangements Then mixed solution B is added in pH value so that pH value increases by 0.05 unit and measures body at this time for example, after the 90h that exposes to the weather Be pH value be 8.05, then the alkali being added be added to always system pH be 8.1 when terminates.
The layered double hydroxide LDH-Cl-NO that the present embodiment is prepared3-SO4 2-The draw ratio of whisker is 19： 1, good dispersion, whisker good crystalline.Layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker in toughened and reinforced material, There is very extensive application prospect in the fields such as catalysis, fire-retardant, sorbing material.
Comparative example 1
This comparative example provides a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Preparation method, the preparation Method removes Mg in step 12+、Al3+Concentration is different from embodiment 1, Mg2+A concentration of 1.1mol/L, Al3+A concentration of 0.28mol/L, Remaining step is same as Example 1.The layered double hydroxide LDH-Cl- of crystal whisker-shaped cannot be prepared in this method NO3-SO4 2-。
Comparative example 2
This comparative example provides a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Preparation method, the preparation PH value in method except step 1 is different from embodiment 1, pH=9, remaining step is same as Example 1.This method cannot be prepared Obtain the layered double hydroxide LDH-Cl-NO of crystal whisker-shaped3-SO4 2-。
Comparative example 3
This comparative example provides a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Preparation method, the preparation PH value in method except step 2 is different from embodiment 1, pH=10, remaining step is same as Example 1.This method cannot be made It is standby to obtain the layered double hydroxide LDH-Cl-NO of crystal whisker-shaped3-SO4 2-。
Comparative example 4
This comparative example provides a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Preparation method, the preparation Except NaNO in the mixed solution B of step 2 in method3, NaOH concentration it is different from embodiment 1, NaNO3A concentration of 0.4mol/L, NaOH concentration is 0.5mol/L, remaining step is same as Example 1.The double gold of stratiform of crystal whisker-shaped cannot be prepared in this method Belong to hydroxide LDH-Cl-NO3-SO4 2-。
Comparative example 5
This comparative example provides a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Preparation method, the preparation It is controlled every 8h addition mixed once solution Bs except no in step 2 in method so that pH value increases by 1 unit, remaining step is equal It is same as Example 1.The layered double hydroxide LDH-Cl-NO of crystal whisker-shaped cannot be prepared in this method3-SO4 2-。
Performance evaluation
1, scanning electron microscope (SEM) is analyzed
As shown in Fig. 2, the shape appearance figure for the sample being prepared for embodiment 1.It can be seen from the figure that prepared by embodiment 1 What is obtained is almost all whisker, and yield is high, and the draw ratio of whisker is 15~25：1, good dispersion, whisker good crystalline.And comparative example 1 sample being prepared not instead of crystal whisker-shaped, other non-crystal whisker-shapeds, as shown in Figure 3.
2, X-ray diffraction (XRD) is analyzed
As shown in figure 4, the layered double hydroxide LDH-Cl-NO prepared for embodiment 13-SO4 2-The XRD of whisker Figure.From its diffractive features peak it is found that sample peak shape is sharp, the LDH of layer structure is in (003) crystal face diffracted intensity maximum, secondly It is (006) crystal face, minimum is (009), this is because caused by " delustring " effect of lamellar compound to XRD, each main diffraction The position at peak shows that the substance is the LDH-Cl-NO with layer structure with intensity3-SO4 2-。
3, elemental analysis
Elemental analysis is carried out to sample prepared by each embodiment, the results are shown in Table 1.Table 1 statistics indicate that, embodiment 1 carries The sample of confession substantially conforms to nMg:nAl:nCl:nN:nS=6:2:1:1, in conjunction with oxygen (content of oxygen is obtained by minusing), protium Content can deduce that its chemical formula is Mg6Al2(OH)14ClNO3SO4·5H2O。
Table 1LDH-Cl-NO3-SO4 2-Elemental analysis result
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention The limitation of shield range can also be made on the basis of above description and thinking for those of ordinary skill in the art Other various forms of variations or variation, there is no necessity and possibility to exhaust all the enbodiments.It is all the present invention All any modification, equivalent and improvement etc., should be included in the protection of the claims in the present invention made by within spirit and principle Within the scope of.

Claims (10)

1. a kind of layered double hydroxide LDH-Cl-NO3-SO4 2-Whisker, which is characterized in that the chemical formula of the whisker is Mg6Al2(OH)14ClNO3SO4·5H2O。
2. the layered double-metal hydroxide LDH-Cl-NO of claim 13-SO4 2-The preparation method of whisker, which is characterized in that Include the following steps：
S1. MgCl is prepared2·6H2O、MgSO4·7H2O and Al (NO3)3·9H2The mixed solution A of O, with 0.05~0.15mol/L NaOH solution adjust pH to 7.45~7.55；Mg in the mixed solution A2+A concentration of 2.5~3.1mol/L, Al3+It is dense Degree is 0.6~0.9mol/L；
S2. NaNO is prepared3With NaNO in the mixed solution B, the mixed solution B of NaOH3A concentration of 1mol/L, NaOH's is dense Degree is 0.01~0.05mol/L；After mixed solution B adjustings pH to 8.05~8.35 is added into mixed solution A obtained by S1, it is placed in 178~186h is reacted at 5~45 DEG C and generates precipitation, is filtered and is washed precipitation, up to layered bimetal hydroxide after drying Object LDH-Cl-NO3-SO4 2-Whisker.
3. preparation method according to claim 2, which is characterized in that adjust pH to 7.5 in S1.
4. preparation method according to claim 2, which is characterized in that Mg in mixed solution A described in S12+It is a concentration of 2.8mol/L, Al3+A concentration of 0.6mol/L.
5. preparation method according to claim 2, which is characterized in that a concentration of 0.1mol/L of NaOH solution described in S1.
6. preparation method according to claim 2, which is characterized in that NaOH's is a concentration of in mixed solution B described in S2 0.02mol/L。
7. preparation method according to claim 2, which is characterized in that NaOH solution is added in S2 and adjusts pH to 8.1.
8. preparation method according to claim 7, which is characterized in that by adding NaNO in S23It is kept with NaOH solution mixed A NaNO is added every 8h in the pH for closing solution3And NaOH solution so that pH value of reaction system increases by 0.05.
9. preparation method according to claim 2, which is characterized in that the reaction time described in S2 is the 182h that exposes to the weather, institute The wind speed for stating wind is 4~5m/s.
10. the layered double-metal hydroxide LDH-Cl-NO of claim 13-SO4 2-Whisker is preparing toughened and reinforced material, is urging Change the application in material, fire proofing or sorbing material.
CN201810310696.6A 2018-03-30 2018-03-30 A kind of layered double hydroxide LDH-Cl-NO3-SO42-Whisker and its preparation method and application Withdrawn CN108396386A (en)

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