CN108483468A - A kind of layered double hydroxide LDH-Br-I-CO32-Whisker and its preparation method and application - Google Patents

A kind of layered double hydroxide LDH-Br-I-CO32-Whisker and its preparation method and application Download PDF

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CN108483468A
CN108483468A CN201810277955.XA CN201810277955A CN108483468A CN 108483468 A CN108483468 A CN 108483468A CN 201810277955 A CN201810277955 A CN 201810277955A CN 108483468 A CN108483468 A CN 108483468A
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whisker
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CN108483468B (en
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吴健松
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Lingnan Normal University
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    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/78Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/782Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen containing carbonate ions, e.g. dawsonite
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    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

The present invention relates to a kind of layered double hydroxide LDH Br I CO3 2‑Whisker and its preparation method and application.The chemical formula of the whisker is Mg6Al2(OH)14BrICO3·6H2O, the whisker pass through metal cation Mg2+And Al3+With anion Br、I、CO3 2‑And OHEvaporable water obtains after reacting to precipitate.Layered double hydroxide LDH Br I CO provided by the invention3 2‑Whisker is a kind of houghite compound of crystal whisker-shaped in addition to the classes talcs 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, it is suitble to large-scale promotion.

Description

A kind of layered double hydroxide LDH-Br-I-CO32-Whisker and preparation method thereof And application
Technical field
The invention belongs to field of material technology.More particularly, to a kind of layered double hydroxide LDH-Br-I- CO3 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.In LDH crystal structures, due to by the minimum effect of lattice energy and its lattice orientation effect It influencing so that metal ion is uniformly distributed in a certain way on laminate, i.e., on laminate in each small structural unit, Its chemical composition and structure is constant;And positioned at interlayer anion due to being attracted by laminate charge, the row between interlayer ion Reprimand, the limitation of inner layer space, the coordination of interlayer ion and laminate group, electronics transfer effect etc. influence, and distribution is also very uniformly. Due to the Modulatory character and entirety uniformity in this chemical composition and microstructure of LDH, itself is again two-dimension nano materials, So the material of this special construction and composition be synthesis with multicomponent reactive component height metal composite oxide it is good before Body.Since the special structures of LDH determine that it has alkalinity, the interchangeability of interlayer anion, thermal stability, the Nomenclature Composition and Structure of Complexes Controllability, acidity etc. to the fields such as catalysis, absorption, fire-retardant, environment, medicine, nano material, functional high molecule material by To being widely applied, there is broad prospect of application in purification of water quality, sewage disposal, prevention and cure of pollution and environment remediation etc..
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-、 I-、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 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 Many scholars synthesize numerous important organic compounds and inorganization on preparing LDH technologies or using LDH as catalyst It closes on object or as many gratifying achievements are also achieved in the researchs such as fire retardant, adsorbent, provides a large amount of useful Experimental data.Currently, LDH is typically to pass through coprecipitation, sol-gel method, hydro-thermal method, calcine-recovering method and ion-exchange Etc. conventional methods prepare.In the method for the above conventional synthesis LDH, coprecipitation needs to control rate of titration and pH ranges, The LDH crystallinity of preparation is relatively low, and the hydroxylated laminate degree of order is inadequate, and complicated for operation cumbersome, the technological process of production is long;Colloidal sol- Organic solvent is used in gel method preparation process, it is of high cost to be easy to cause environmental pollution, and the not pure and mild pattern of interlayer anion Irregularly.
What is more important, so far, LDH and HTLc class compounds are mainly laminated structure, the LDH of crystal whisker-shaped and HTLc class compounds are almost without report.And the inorganic material of crystal whisker-shaped has toughened and reinforced function, as crystal whisker-shaped can be developed LDH or HTLc classes compound can then assign LDH and HTLc classes inorganic material preferably toughened and reinforced function, further to widen it Using.
Invention content
The technical problem to be solved by the present invention is to overcome the research blank of the LDH and HTLc class compounds of existing crystal whisker-shaped, A kind of layered double hydroxide LDH-Br-I-CO is provided3 2-Whisker.Layered double hydroxide provided by the invention LDH-Br-I-CO3 2-Whisker, which removes the classes such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeability with aperture, to be slided Outside the function of stone class compound, also has the function of crystal whisker toughened reinforcement in toughened and reinforced material, catalysis, fire-retardant, sorbing material There is very extensive application prospect in equal fields.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Br-I-CO3 2-The preparation of whisker Method.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Br-I-CO3 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-Br-I-CO3 2-Whisker, the whisker pass through metal cation Mg2+With Al3+With anion Br-、I-、CO3 2-And OH-Evaporable water obtains after reacting to precipitate;Contain 15%~25% in the whisker The H of Mg, 5%~9% Al, 1%~2% C, 5%~15% Br, 5%~10% I and 2%~4%.
Preferably, in the whisker containing 19.22% Mg, 7.21% Al, 1.62% C, 10.69% Br, 4.72% I and 3.46% H.
Preferably, the chemical formula of the whisker is Mg6Al2(OH)14BrICO3·6H2O。
The present invention provides a kind of layered double hydroxide LDH-Br-I-CO of specific composition3 2-Whisker, the substance For crystal whisker-shaped, have the function of toughened and reinforced caused by whisker structure;The substance again there is HTLc class compounds to be had simultaneously The adjustable denaturation in some apertures, the function of larger specific surface area and interlayer ion interchangeability are urged in toughened and reinforced material There is very extensive application prospect in the fields such as change, fire-retardant, sorbing material.
The present invention additionally provides layered double-metal hydroxide LDH-Br-I-CO simultaneously3 2-The preparation method of whisker, It is prepared, is included the following steps using natural evaporation concentration technology:
S1. the MgI of 3.60~3.90mol/L is prepared respectively2·8H2The MgBr of O solution, 3.60~3.90mol/L2· 6H2Al (the NO of O solution and 2.20~2.40mol/L3)3·9H2O solution takes this 3 kinds of solution mixed in stirring volumetric It closes, the pH that mixed system is adjusted to the aqueous slkali of 0.05~0.15mol/L is 7.45~7.55;
S2. the Na that 1.25~1.55mol/L is added is stirred into the mixed solution of step S12CO3Or K2CO3Solution is to body The pH of system is 8.05~8.25, after natural evaporation concentrates, filters and washs precipitation, dry to get layered bimetallic Hydroxide whisker;Wherein in natural evaporation concentration process, need that a NaOH or KOH is added every 7~9h (preferably 8h) Solution so that the pH value of system increases by 0.05 unit.
The MgI2·8H2O、MgBr2·6H2O can derive from Qinghai Salt Lake bittern.
Preferably, in step S1, before mixing, the MgI2·8H2O、MgBr2·6H2O and Al (NO3)3·9H2O's is dense Degree is respectively 3.90mol/L, 3.90mol/L and 2.40mol/L.
Preferably, in step S1, after 3 kinds of solution mixing, Mg is controlled2+A concentration of 2.20~3.00mol/L; Br-It is dense Degree is 2.20~3.00mol/L;I-A concentration of 2.20~3.00mol/L;Al3+A concentration of 0.70~0.90mol/L.
It is highly preferred that in step S1, after 3 kinds of solution mixing, Mg is controlled2+、Br-、I-Concentration be 2.60 mol/L;Al3 +A concentration of 0.80mol/L
The present invention is to layered double hydroxide LDH-Br-I-CO3 2-Preparation process carry out exploration discovery, raw material and It is matched, pH regulation and control and temperature regulation and control have significant impact to the pattern of final layered double hydroxide.As metal sun from Sub- Mg2+And Al3+, anion Br-、I-、CO3 2-And OH-Concentration it is excessive or too small, pH is excessively high or pH fluctuation ranges are excessive, moisture When evaporation temperature excessively high (water evaporation rate is too fast) be unable to get whisker morphology or obtain whisker morphology yield it is very low. The present invention finally prepares the layered double hydroxide LDH-Br-I- of crystal whisker-shaped by the preferred of this series of conditions CO3 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-Br-I-CO3 2-The extremely excellent natural resources of whisker.But these resources cannot get always science, height Value utilizes, but leaves unused always, this not only wastes salt lake resources, also so that the serious salination of salt lake Soil Surrounding and plant It is withered, it is damaged to the ecological environment in salt lake, while also bringing difficulty to saltern resource exploitation in future.Made using bittern in salt lake For Mg2+And Al3+Source, the natural resources can be made full use of, it is cost-effective, have important economic value.
Preferably, it is 7.5 that pH is adjusted in step S1.
Preferably, in step S1, the aqueous slkali is NaOH or KOH.
It is highly preferred that in step S1, the aqueous slkali is NaOH solution, a concentration of 0.10mol/L.
Preferably, in step S2, the time of the natural evaporation is 157~167h;Temperature is 5~45 DEG C.
In order to further shorten evaporation time, while the generation quality of whisker is improved, it is further preferred that step S2 In, the time of the natural evaporation is 162h;Temperature is 5~45 DEG C.
In order to enable moisture evaporation is more uniformly distributed, it is preferable that in step S2, the wind speed in the natural evaporation is 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 Precipitation obtained by step S2 can be placed at the spaciousness of Qinghai Salt Lake area by~5m/s, real using natural solar energy and wind energy resources Existing moisture slow evaporation, not only saves energy and realizes green chemical industry.
Preferably, Na described in step S22CO3Or K2CO3A concentration of 1.4mol/L of solution.
Preferably, Na is added in step S22CO3Or K2CO3Solution to pH be 8.1.
Preferably, step S2 needs that a NaOH or KOH solution is added every 8h, makes in natural evaporation concentration process The pH value for the system of obtaining increases by 0.05 unit;And a concentration of 0.01mol/L of the NaOH or KOH solution solution.
Preferably, washing described in step S2 is washing 4~6 times.
Preferably, the drying described in step S2 is dried at 70~90 DEG C.
In the present invention, for the whisker in threadiness, the draw ratio of whisker is 15~25:1;Yield is up to 98%;Purity is 98%.
Correspondingly, above-mentioned layered double hydroxide LDH-Br-I-CO3 2-Whisker is preparing toughened and reinforced material, catalysis Application in material, fire proofing or sorbing material is also within the scope of the present invention.
Compared with prior art, the present invention has the advantages that:
Layered double hydroxide LDH-Br-I-CO provided by the invention3 2-Whisker is a kind of houghite of crystal whisker-shaped Compound had not only had the function of crystal whisker toughened reinforcement, but also had adjustable denaturation, larger specific surface area and the interlayer ion in aperture can The function of the classes talcs compound such as exchangeability has non-in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material Often it is widely applied foreground.Preparation method provided by the invention, it is simple for process, it is suitble to large-scale promotion.
Description of the drawings
Fig. 1 is that embodiment 1 prepares layered double hydroxide LDH-Br-I-CO3 2-The route map of whisker.
Fig. 2 is the layered double hydroxide LDH-Br-I-CO that embodiment 1 provides3 2-The shape appearance figure of whisker.
Fig. 3 is the shape appearance figure of sample prepared by comparative example 1 of the present invention.
Fig. 4 is layered double hydroxide LDH-Br-I-CO prepared by the embodiment of the present invention 13 2-The XRD diagram of whisker.
Fig. 5 serves as reasonsWithThe layer structure figure of composition.
Specific implementation mode
Further illustrated the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagent, methods and apparatus.
Unless stated otherwise, following embodiment agents useful for same and material are purchased in market.
Embodiment 1
The present embodiment provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Whisker, chemical formula Mg6Al2 (OH)14BrICO3·6H2O, preparation method are following (such as Fig. 1):
S1. the MgI of 3.90mol/L is prepared respectively2·8H2The MgBr of O solution, 3.90mol/L2·6H2O solution with Al (the NO of 2.40mol/L3)3·9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and will The pH value of mixed system is adjusted to pH=7.50 with the NaOH solution of 0.1mol/L, at this point, due to Al3+The hydrolysis of ion and make solution Become muddy, but generates this phenomenon and do not interfere with follow-up LDH-Br-I-CO3 2--The growth of whisker;
S2. the Na of 1.4mol/L is prepared2CO3Solution liquid is added in the mixed liquor obtained by previous step, always while stirring It adds to the pH to pH=8.10 of system then system is placed in after sun-drenched place allows and expose to the weather 162h, filters and wash Precipitation is washed, is dried to get sample.In the time of this 162h, a NaOH solution, the amount being added every time was added every 8 hours It is:The pH value for first measuring current arrangements, is then added mixed liquor so that pH value increases by 0.05 unit, for example, exposing to the weather After 100h (temperature is 5~45 DEG C, and wind speed is 4~5m/s), it is 8.05 to measure system pH at this time, then the amount that mixed liquor is added is It is added to always when system pH is 8.10 and terminates.
The layered double hydroxide LDH-Br-I-CO that the present embodiment is prepared3 2-The draw ratio of whisker be 15~ 25:1, good dispersion, whisker good crystalline have preferable toughened and reinforced function.
Embodiment 2
The present embodiment provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Whisker, preparation method are as follows:
S1. the MgI of 3.70mol/L is prepared respectively2·8H2The MgBr of O solution, 3.70mol/L2·6H2O solution with Al (the NO of 2.30mol/L3)3·9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and will The pH value of mixed system is adjusted to pH=7.50 with the NaOH solution of 0.1mol/L, at this point, due to Al3+The hydrolysis of ion and make solution Become muddy, but generates this phenomenon and do not interfere with follow-up LDH-Br-I-CO3 2--The growth of whisker;
S2. the Na of 1.4mol/L is prepared2CO3Solution liquid is added in the mixed liquor obtained by previous step, always while stirring It adds to the pH to pH=8.10 of system then system is placed in after sun-drenched place allows and expose to the weather 162h, filters and wash Precipitation is washed, is dried to get sample.In the time of this 162h, a NaOH solution, the amount being added every time was added every 8 hours It is:The pH value for first measuring current arrangements, is then added mixed liquor so that pH value increases by 0.05 unit, for example, exposing to the weather After (temperature is 5~45 DEG C, and wind speed is 4~5m/s) 100h, it is 8.05 to measure system pH at this time, then the amount that mixed liquor is added is It is added to always when system pH is 8.10 and terminates.
The layered double hydroxide LDH-Br-I-CO that the present embodiment is prepared3 2-The draw ratio of whisker be 15~ 25:1, good dispersion, whisker good crystalline have preferable toughened and reinforced function.
Embodiment 3
The present embodiment provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Whisker, preparation method are as follows:
S1. the MgI of 3.60mol/L is prepared respectively2·8H2The MgBr of O solution, 3.60mol/L2·6H2O solution with Al (the NO of 2.20mol/L3)3·9H2O solution takes this 3 kinds of solution to be mixed in a beaker in stirring volumetric, and will The pH value of mixed system is adjusted to pH=7.50 with the NaOH solution of 0.1mol/L, at this point, due to Al3+The hydrolysis of ion and make solution Become muddy, but generates this phenomenon and do not interfere with follow-up LDH-Br-I-CO3 2--The growth of whisker;
S2. the Na of 1.55mol/L is prepared2CO3Solution is added to while stirring in the mixed liquor obtained by two steps, is added always To system pH to pH=8.25 then by system be placed in sun-drenched place allow expose to the weather 174h (temperature be 5~45 DEG C, wind speed is 4~5m/s) after, precipitation is filtered and washed, is dried to get sample;
In the time of this 174h, every the NaOH solution that 8 hours are added a 0.01mol/L, the amount being added every time is: The pH value for first measuring current arrangements, is then added alkali so that pH value increases by 0.05 unit, for example, measuring system pH at this time Be 8.25, then be added aqueous slkali when be added to always system pH be 8.3 when terminate.
The layered double hydroxide LDH-Br-I-CO that the present embodiment is prepared3 2-The draw ratio of whisker be 15~ 25:1, good dispersion, whisker good crystalline have preferable toughened and reinforced function.
Comparative example 1
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In except in step S1, in addition to " after mixing, Mg2+、Br-、I-Concentration be 1.80mol/L;Al3+A concentration of 0.60mol/L " Except, remaining step is consistent with embodiment 1 with operation.
As a result:Crystal whisker-shaped object has been not observed under SEM and has held generation.
Comparative example 2
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In in addition to the concentration of aqueous slkali in step S1 is respectively 6.00mol/L, remaining step is consistent with embodiment 1 with operation.
As a result:Crystal whisker-shaped object has been not observed under biomicroscope and has held generation.
Comparative example 3
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In except Na is added in step S22CO3The pH of solution to system is respectively outside 10, remaining step is consistent with embodiment 1 with operation.
As a result:Crystal whisker-shaped object has been not observed under biomicroscope and has held generation.
Comparative example 4
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In except in step S2 be added NaOH solution concentration be respectively 6.00mol/L in addition to, remaining step with operation with embodiment 1 one It causes.
As a result:Crystal whisker-shaped object has been not observed under biomicroscope and has held generation.
Comparative example 5
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In except step S2 is in natural evaporation concentration process, the disposable NaOH solution for increasing 0.01mol/L so that the pH value of system is tieed up It keeps steady surely outer, remaining step is consistent with embodiment 1 with operation.
As a result:Crystal whisker-shaped object has been not observed under biomicroscope and has held generation.
Comparative example 6
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In except step S2 in natural evaporation concentration process, need every 3h be added a 0.01mol/L NaOH solution so that body The pH value of system increases outside 0.5 unit, remaining step is consistent with embodiment 1 with operation.
As a result:Crystal whisker-shaped object has been not observed under biomicroscope and has held generation.
Comparative example 7
This comparative example provides a kind of layered double hydroxide LDH-Br-I-CO3 2-Preparation method, the preparation method In except step S2 in natural evaporation concentration process, need every 11h be added a 0.01mol/L NaOH solution so that body The pH value of system increases outside 1 unit, remaining step is consistent with embodiment 1 with operation.
As a result:Crystal whisker-shaped object has been not observed under biomicroscope and has held generation.
Performance test
(1) SEM pattern tests
As shown in Fig. 2, the shape appearance figure for the sample being prepared for Examples 1 to 3.It can be seen from the figure that embodiment 1~ 3 be prepared be almost all whisker, in threadiness, yield is up to 98%, purity 98%, the draw ratio of whisker is 15~ 25:1, good dispersion, whisker good crystalline.And the sample that comparative example 1 is prepared does not have crystal whisker-shaped, but other non-crystal whisker-shapeds, As shown in Figure 3.
(2) XRD is tested
As shown in figure 4, the layered double hydroxide LDH-Br-I-CO provided for embodiment 13 2-The XRD diagram of whisker. It can be seen that sample peak shape is sharp, position and the intensity of each main diffraction peak show that the substance is with layer structure LDH-Br-I-CO3 2-
(3) elemental analysis
Elemental analysis is carried out to sample prepared by embodiment 1, the results are shown in Table 1.Table 1 statistics indicate that, embodiment 1 provide Sample substantially conform to nMg:nAl:nBr:nI:nC=6:2:1:1:1, in conjunction with oxygen (content of oxygen is obtained by minusing), protium Content can deduce that its chemical formula is Mg6Al2(OH)14BrICO3·6H2O。
1 Mg of table6Al2(OH)14BrICO3·6H2O elemental analysis results

Claims (10)

1. a kind of layered double hydroxide LDH-Br-I-CO3 2-Whisker, which is characterized in that the whisker by metal sun from Sub- Mg2+And Al3+With anion Br-、I-、CO3 2-And OH-Evaporable water obtains after reacting to precipitate;Contain 15% in the whisker ~25% Mg, 5%~9% Al, 1%~2% C, 5%~15% Br, 5%~10% I and 2%~4% H.
2. layered double hydroxide LDH-Br-I-CO according to claim 13 2-Whisker, which is characterized in that the crystalline substance The chemical formula of palpus is Mg6Al2(OH)14BrICO3·6H2O。
3. the layered double-metal hydroxide LDH-Br-I-CO of claims 1 or 23 2-The preparation method of whisker, feature exist In including the following steps:
S1. the MgI of 3.60~3.90 mol/L is prepared respectively2•8H2The MgBr of O solution, 3.60~3.90 mol/L2•6H2O is molten Al (the NO of liquid and 2.20~2.40 mol/L3)3·9H2O solution takes this 3 kinds of solution to be mixed in stirring volumetric, uses The pH that the aqueous slkali of 0.05~0.15 mol/L is adjusted to mixed system is 7.45~7.55;
S2. the Na that 1.25~1.55 mol/L are added is stirred into the mixed solution of step S12CO3Or K2CO3Solution is to system PH is 8.05~8.25, after natural evaporation concentrates, filters and washs precipitation, dry to get layered bimetallic hydrogen-oxygen Compound whisker;Wherein in natural evaporation concentration process, need that a NaOH or KOH solution is added every 7~9 h so that body The pH value of system increases by 0.05 unit.
4. preparation method according to claim 3, which is characterized in that in step S1, before mixing, the MgI2•8H2O、 MgBr2•6H2O and Al (NO3)3•9H2The concentration of O is respectively 3.90 mol/L, 3.90 mol/L and 2.40 mol/L.
5. preparation method according to claim 3, which is characterized in that after 3 kinds of solution mixing, control Mg2 +、Br-、I-It is dense Degree is 2.20~3.00 mol/L;Al3+A concentration of 0.70~0.90 mol/L.
6. preparation method according to claim 3, which is characterized in that in step S1, the aqueous slkali be NaOH or KOH。
7. preparation method according to claim 3, which is characterized in that in step S2, the time of the natural evaporation is 157 ~167 h;Temperature is 5~45 DEG C.
8. preparation method according to claim 3, which is characterized in that step S2 needs in natural evaporation concentration process A NaOH or KOH solution is added every 8 h so that the pH value of system increases by 0.05 unit.
9. preparation method according to claim 3, which is characterized in that in step S2, the wind speed in the natural evaporation is 4 ~5 m/s.
10. layered double hydroxide LDH-Br-I-CO as claimed in claim 1 or 23 2-Whisker as or prepare increase Application in tough supporting material, catalysis material, fire proofing or sorbing material.
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