CN108396380A - A kind of layered double hydroxide LDH-Cl3-Br- whiskers and its preparation method and application - Google Patents

A kind of layered double hydroxide LDH-Cl3-Br- whiskers and its preparation method and application Download PDF

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CN108396380A
CN108396380A CN201810310654.2A CN201810310654A CN108396380A CN 108396380 A CN108396380 A CN 108396380A CN 201810310654 A CN201810310654 A CN 201810310654A CN 108396380 A CN108396380 A CN 108396380A
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whisker
preparation
layered double
ldh
double hydroxide
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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
    • C30B29/12—Halides
    • 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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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention belongs to technical field of inorganic material, specifically disclose a kind of layered double hydroxide LDH Cl3‑Br‑Whisker and its preparation method and application.The chemical formula of the whisker is Mg6Al2(OH)14Cl3Br·3H2O, the whisker pass through metal cation Mg2+、Al3+With anion Cl‑、Br‑、NO3 ‑、OH‑Evaporable water obtains after reacting to precipitate.Layered double hydroxide LDH Cl provided by the invention3‑Br‑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-Cl3-Br-Whisker and preparation method thereof and Using
Technical field
The present invention relates to technical field of inorganic material, and in particular, to a kind of layered double hydroxide LDH-Cl3- Br-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-Cl3-Br-Whisker, except classes neatlys such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeabilities with aperture Outside the function of stone class 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-Cl3-Br-The preparation side of whisker Method.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl3-Br-Whisker is preparing increasing Application in tough supporting 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-Cl3-Br-Whisker, chemical formula Mg6Al2(OH)14Cl3Br·3H2O。
Preferably, the whisker passes through metal cation Mg2+、Al3+With anion Cl-、Br-、NO3 -、OH-React to obtain precipitation Evaporable water obtains afterwards.
The present invention provides a kind of layered double hydroxide LDH-Cl of specific composition3-Br-Whisker, the substance are crystalline substance The draw ratio of palpus shape, whisker is 15~25:1, there is good dispersion, good crystalline toughening caused by the typical structure of whisker to mend Powerful；In addition, adjustable denaturation, larger specific surface area and interlayer ion also with aperture possessed by HTLc class compounds The function of interchangeability, before there is very extensive application in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material Scape.
Layered double-metal hydroxide LDH-Cl3-Br-The preparation method of whisker, includes the following steps：
S1. MgCl is prepared2·6H2O、MgBr2·6H2O and Al (NO3)3·9H2The mixed solution of O, with 0.05~ The NaOH solution of 0.15mol/L adjusts pH to 7.45~7.55；Mg in the mixed solution2+A concentration of 2.1~2.5mol/ L, Al3+A concentration of 0.6~0.8mol/L；
S2. after 0.01~0.02mol/L NaOH solutions adjusting pH to 8.05~8.35 is added into mixed solution, 5 are placed in 104~108h is reacted at~45 DEG C and generates precipitation, is filtered and is washed precipitation, up to layered bimetal hydroxide after drying Object LDH-Cl3-Br-Whisker.
The present inventor is to layered double hydroxide LDH-Cl3-Br-It is found unintentionally in the exploration of preparation process, it is former Material and its proportioning, pH regulation and control, reaction temperature and time have a significant impact to the pattern tool of final layered double hydroxide.Such as Metal cation Mg2+And Al3+, anion Cl-、Br-、NO3 -And OH-Concentration it is excessive or too small, pH is excessively high or pH fluctuation ranges Excessive, reaction temperature excessively high (water evaporation rate is too fast) is unable to get whisker morphology or obtains the yield of whisker morphology very It is low.The present invention finally prepares the layered double hydroxide LDH-Cl of crystal whisker-shaped by the preferred of this series of conditions3- Br-, 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-Cl3-Br-The extremely excellent natural resources of whisker.But these resources cannot get always science, effectively 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.Using 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 can derive from Qinghai Salt Lake bittern.
Preferably, pH to 7.5 is adjusted in S1.
Preferably, Mg in mixed solution described in S12+A concentration of 2.3mol/L, Al3+A concentration of 0.6mol/L.
Preferably, a concentration of 0.1mol/L of NaOH solution described in S1.
Preferably, a concentration of 0.01mol/L of NaOH solution described in S2.
Preferably, NaOH solution is added in S2 and adjusts pH to 8.2.
In order to preferably regulate and control pH, prevents pH too low or fluctuation is excessive, it is preferable that protected in S2 by adding NaOH solution A NaOH solution is added every 6h so that pH value of reaction system increases by 0.05 in the pH for holding mixed solution.
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 106h, 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 mixed solution in S2 can be placed at the spaciousness of Qinghai Salt Lake area, utilize natural solar energy and wind energy by~5m/s Resource realizes moisture slow evaporation, not only saves energy and realizes green chemical industry.
Layered double-metal hydroxide LDH-Cl is also claimed in the present invention3-Br-Whisker is preparing toughened and reinforced material Application in material, catalysis material, fire proofing or sorbing material.
Compared with prior art, the invention has the advantages that：
Layered double hydroxide LDH-Cl provided by the invention3-Br-Whisker is a kind of houghite of crystal whisker-shaped Object is closed, except houghites class compounds such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeabilities with aperture Function outside, also have the function of crystal whisker toughened reinforcement, in toughened and reinforced material, catalysis, fire-retardant, sorbing material etc. have in fields There is 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 extensive It promotes and applies.
Description of the drawings
Fig. 1 is that embodiment 1 prepares layered double hydroxide LDH-Cl3-Br-The route map of whisker.
Fig. 2 is layered double hydroxide LDH-Cl prepared by embodiment 13-Br-The SEM spectrum of whisker.
Fig. 3 is layered double hydroxide LDH-Cl prepared by comparative example 13-Br-SEM spectrum.
Fig. 4 is layered double hydroxide LDH-Cl prepared by embodiment 13-Br-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-Cl3-Br-Whisker, chemical formula Mg6Al2 (OH)14Cl3Br·3H2O, preparation process are following (as shown in Figure 1)：
1,5.3mol/L MgCl are prepared2·6H2O、1.8mol/L MgBr2·6H2O 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 system 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 phenomenon does not interfere with follow-up LDH-Cl3-Br-The growth of whisker.
2, the NaOH solution for preparing 0.01mol/L, is added to while stirring in the mixed solution obtained by previous step, adds always To the pH to pH=8.2 of system；Then system is placed in after sun-drenched place allows (at 5~45 DEG C) and expose to the weather 106h Precipitation is generated, filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl after drying3-Br-Whisker.At this In the time of 106h, the NaOH solution of a 0.01mol/L is added every 6h, the amount being added every time is：First measure current arrangements PH value, alkali is then added so that pH value increase by 0.05 unit measure system pH at this time for example, after the 50h that exposes to the weather Value is 8.05, then the alkali being added, which is added to always when system pH is 8.1, to be terminated.
The layered double hydroxide LDH-Cl that the present embodiment is prepared3-Br-The draw ratio of whisker is 18：1, dispersion Good, the whisker good crystalline of property.Layered double hydroxide LDH-Cl3- Br whiskers are in toughened and reinforced material, catalysis, fire-retardant, suction There is very extensive application prospect in the fields such as enclosure material.
Embodiment 2
Present embodiments provide a kind of layered double hydroxide LDH-Cl3-Br-Whisker, chemical formula Mg6Al2 (OH)14Cl3Br·3H2O, preparation process are as follows：
1,5.2mol/L MgCl are prepared2·6H2O、1.5mol/L MgBr2·6H2O and 2mol/L Al (NO3)3·9H2O Solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and by the pH value 0.1mol/L of mixed system NaOH solution be 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 phenomenon not It can influence follow-up LDH-Cl3-Br-The growth of whisker.
2, the NaOH solution for preparing 0.01mol/L, is added to while stirring in the mixed solution obtained by previous step, adds always To the pH to pH=8.2 of system；Then system is placed in after sun-drenched place allows (at 5~45 DEG C) and expose to the weather 106h Precipitation is generated, filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl after drying3-Br-Whisker.At this In the time of 106h, the NaOH solution of a 0.01mol/L is added every 6h, the amount being added every time is：First measure current arrangements PH value, alkali is then added so that pH value increase by 0.05 unit measure system pH at this time for example, after the 50h that exposes to the weather Value is 8.05, then the alkali being added, which is added to always when system pH is 8.1, to be terminated.
The layered double hydroxide LDH-Cl that the present embodiment is prepared3-Br-The draw ratio of whisker is 19：1, dispersion Good, the whisker good crystalline of property.Layered double hydroxide LDH-Cl3- Br whiskers are in toughened and reinforced material, catalysis, fire-retardant, suction There is very extensive application prospect in the fields such as enclosure material.
Embodiment 3
Present embodiments provide a kind of layered double hydroxide LDH-Cl3-Br-Whisker, chemical formula Mg6Al2 (OH)14Cl3Br·3H2O, preparation process are as follows：
1,5.3mol/L MgCl are prepared2·6H2O、1.8mol/L MgBr2·6H2O 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 system is used The NaOH solution of 0.1mol/L is adjusted to pH=7.48, 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-Cl3-Br-The growth of whisker.
2, the NaOH solution for preparing 0.01mol/L, is added to while stirring in the mixed solution obtained by previous step, adds always To the pH to pH=8.2 of system；Then system is placed in after sun-drenched place allows (at 5~45 DEG C) and expose to the weather 106h Precipitation is generated, filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl after drying3-Br-Whisker.At this In the time of 106h, the NaOH solution of a 0.01mol/L is added every 6h, the amount being added every time is：First measure current arrangements PH value, alkali is then added so that pH value increase by 0.05 unit measure system pH at this time for example, after the 50h that exposes to the weather Value is 8.05, then the alkali being added, which is added to always when system pH is 8.1, to be terminated.
The layered double hydroxide LDH-Cl that the present embodiment is prepared3-Br-The draw ratio of whisker is 18：1, dispersion Good, the whisker good crystalline of property.Layered double hydroxide LDH-Cl3- Br whiskers are in toughened and reinforced material, catalysis, fire-retardant, suction There is very extensive application prospect in the fields such as enclosure material.
Embodiment 4
Present embodiments provide a kind of layered double hydroxide LDH-Cl3-Br-Whisker, chemical formula Mg6Al2 (OH)14Cl3Br·3H2O, preparation process are as follows：
1,5.3mol/L MgCl are prepared2·6H2O、1.8mol/L MgBr2·6H2O 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 system 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 phenomenon does not interfere with follow-up LDH-Cl3-Br-The growth of whisker.
2, the NaOH solution for preparing 0.01mol/L, is added to while stirring in the mixed solution obtained by previous step, adds always To the pH to pH=8.3 of system；Then system is placed in after sun-drenched place allows (at 5~45 DEG C) and expose to the weather 106h Precipitation is generated, filters and washs precipitation, up to layered double-metal hydroxide LDH-Cl after drying3-Br-Whisker.At this In the time of 106h, the NaOH solution of a 0.01mol/L is added every 6h, the amount being added every time is：First measure current arrangements PH value, alkali is then added so that pH value increase by 0.05 unit measure system pH at this time for example, after the 50h that exposes to the weather Value is 8.05, then the alkali being added, which is added to always when system pH is 8.1, to be terminated.
The layered double hydroxide LDH-Cl that the present embodiment is prepared3-Br-The draw ratio of whisker is 20：1, dispersion Good, the whisker good crystalline of property.Layered double hydroxide LDH-Cl3- Br whiskers are in toughened and reinforced material, catalysis, fire-retardant, suction There is very extensive application prospect in the fields such as enclosure material.
Comparative example 1
This comparative example provides a kind of layered double hydroxide LDH-Cl3-Br-Preparation method, in the preparation method Except Mg2+、Al3+Concentration is different from embodiment 1, Mg2+A concentration of 1.1mol/L, Al3+A concentration of 0.2mol/L, remaining step with Embodiment 1 is identical.The layered double hydroxide LDH-Cl of crystal whisker-shaped cannot be prepared in this method3-Br-。
Comparative example 2
This comparative example provides a kind of layered double hydroxide LDH-Cl3-Br-Preparation method, in the preparation method Except the pH value of step 1 is different from embodiment 1, pH=10, remaining step is same as Example 1.This method cannot be prepared The layered double hydroxide LDH-Cl of crystal whisker-shaped3-Br-。
Comparative example 3
This comparative example provides a kind of layered double hydroxide LDH-Cl3-Br-Preparation method, in the preparation method Except the pH value of step 2 is different from embodiment 1, pH=11, remaining step is same as Example 1.This method cannot be prepared The layered double hydroxide LDH-Cl of crystal whisker-shaped3-Br-。
Comparative example 4
This comparative example provides a kind of layered double hydroxide LDH-Cl3-Br-Preparation method, in the preparation method Except the NaOH solution not controlled in step 2 every 0.01mol/L of 6h additions so that pH value increases outside 0.05 unit, Remaining step is same as Example 1.The layered double hydroxide LDH-Cl of crystal whisker-shaped cannot be prepared in this method3- Br-。
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 18：1, good dispersion, whisker good crystalline.And comparative example 3 is made Standby obtained sample 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 prepared for embodiment 13-Br-The XRD diagram of whisker.From it Diffractive features peak is it is found that sample peak shape is sharp, and the LDH of layer structure is in (003) crystal face diffracted intensity maximum, followed by (006) Crystal face, minimum is (009), this is because caused by " delustring " effect of lamellar compound to XRD, the position of each main diffraction peak Show that the substance is the LDH-Cl with layer structure with intensity3-Br-。
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:nBr:nCl=6:2:1:3, contain in conjunction with oxygen (content of oxygen is obtained by minusing), protium Amount can deduce that its chemical formula is Mg6Al2(OH)14Cl3Br·3H2O。
Table 1LDH-Cl3-Br-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-Cl3-Br-Whisker, which is characterized in that the chemical formula of the whisker is Mg6Al2 (OH)14Cl3Br·3H2O。
2. the layered double-metal hydroxide LDH-Cl of claim 13-Br-The preparation method of whisker, which is characterized in that including Following steps：
S1. MgCl is prepared2·6H2O、MgBr2·6H2O and Al (NO3)3·9H2The mixed solution of O, with 0.05~0.15mol/L's NaOH solution adjusts pH to 7.45~7.55；Mg in the mixed solution2+A concentration of 2.1~2.5mol/L, Al3+Concentration For 0.6~0.8mol/L；
S2. after 0.01~0.02mol/L NaOH solutions adjusting pH to 8.05~8.35 is added into mixed solution, 5~45 are placed in 104~108h is reacted at DEG C and generates precipitation, is filtered and is washed precipitation, up to layered double-metal hydroxide LDH- after drying Cl3-Br-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 described in S12+A concentration of 2.3mol/ 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 a concentration of 0.01mol/L of NaOH solution described in S2.
7. preparation method according to claim 2, which is characterized in that NaOH solution is added in S2 and adjusts pH to 8.2.
8. preparation method according to claim 7, which is characterized in that keep mixed solution by adding NaOH solution in S2 PH, every 6h be added a NaOH solution so that pH value of reaction system increase by 0.05.
9. preparation method according to claim 2, which is characterized in that the reaction time described in S2 is the 106h that exposes to the weather, institute The wind speed for stating wind is 4~5m/s.
10. the layered double-metal hydroxide LDH-Cl of claim 13-Br-Whisker is preparing toughened and reinforced material, catalysis material Application in material, fire proofing or sorbing material.
CN201810310654.2A 2018-03-30 2018-03-30 A kind of layered double hydroxide LDH-Cl3-Br- whiskers and its preparation method and application Withdrawn CN108396380A (en)

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Application publication date: 20180814