CN108425151A - A kind of layered double hydroxide LDH-Cl-I-CO3Whisker and its preparation method and application - Google Patents

A kind of layered double hydroxide LDH-Cl-I-CO3Whisker and its preparation method and application Download PDF

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CN108425151A
CN108425151A CN201810297640.1A CN201810297640A CN108425151A CN 108425151 A CN108425151 A CN 108425151A CN 201810297640 A CN201810297640 A CN 201810297640A CN 108425151 A CN108425151 A CN 108425151A
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whisker
layered double
preparation
double hydroxide
ldh
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吴健松
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Lingnan Normal University
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/041—Oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/232—Carbonates
    • B01J27/236—Hydroxy carbonates
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    • C09K21/00—Fireproofing materials
    • C09K21/02—Inorganic materials
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    • 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
    • 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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Abstract

The present invention relates to a kind of layered double hydroxide LDH Cl I CO3Whisker and its preparation method and application.The chemical formula of the whisker is Mg6Al2（OH）14ClICO3·4H2O；The whisker passes through metal cation Mg2+And Al3+With anion I‑、Cl‑、CO32‑And OH‑Evaporable water obtains after reacting to precipitate.Layered double hydroxide LDH Cl I CO provided by the invention3Whisker 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-Cl-I-CO3Whisker and preparation method thereof and Using
Technical field
The invention belongs to Material Fields, more particularly, to a kind of layered double hydroxide LDH-Cl-I-CO3It is brilliant Must 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 be Coating combination water number mesh) byThe plate layer formed Referred to as sheet-metal layers, byThe layer of composition is known as anion layer.This layer structure can indicate as follows：
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.But extremely currently, LDH and HTLc class compounds are mainly laminated structure, LDH the and HTLc class compounds of crystal whisker-shaped Almost without report.And the inorganic material of crystal whisker-shaped has toughened and reinforced function, can such as develop LDH the or HTLc classes of crystal whisker-shaped Closing object can then assign LDH and HTLc classes inorganic material preferably toughened and reinforced function, further to widen its application.
Therefore, developing a kind of LDH and/or HTLc class compounds of crystal whisker-shaped has great research significance and application value.
Invention content
Present invention aims at the research blank for the LDH and HTLc class compounds for making up crystal whisker-shaped in the prior art, provide A kind of layered double hydroxide LDH-Cl-I-CO3Whisker.Layered double hydroxide LDH-Cl- provided by the invention I-CO3Whisker removes the classes talcs chemical combination such as adjustable denaturation, larger specific surface area and the interlayer ion interchangeability with aperture Outside the function of object, also has the function of crystal whisker toughened reinforcement in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material With very extensive application prospect.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl-I-CO3The preparation of whisker Method.
Another object of the present invention is to provide above-mentioned layered double hydroxide LDH-Cl-I-CO3It 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-Cl-I-CO3The chemical formula of whisker, the whisker is Mg6Al2(OH)14ClICO3·4H2O；The whisker passes through metal cation Mg2+And Al3+With anion I-、 Cl-、CO32-And OH-React heavy Evaporable water obtains behind shallow lake.
The present invention provides a kind of layered double hydroxide LDH-Cl-I-CO of specific composition3Whisker, the substance are The draw ratio of crystal whisker-shaped, whisker is 15~25:1, good dispersion, whisker crystal form is good, and there is toughening caused by whisker structure to mend Strong function；Simultaneously the substance have again the adjustable denaturation in aperture, larger specific surface area possessed by HTLc class compounds and The function of interlayer ion interchangeability has very extensive in toughened and reinforced material, the fields such as catalysis, fire-retardant, sorbing material Application prospect.
The present invention provides a kind of above-mentioned layered double hydroxide LDH-Cl-I-CO3The preparation method of whisker, the system Preparation Method includes the following steps：
S1：Prepare MgI2And AlCl3Mixed solution, be adjusted to NaOH the or KOH solution of 0.0085~0.0115mol/L PH is 7.45~7.55；Mg in the mixed solution2+A concentration of 2.1~2.7mol/L, Al3+A concentration of 0.65~ 0.95mol/L；
S2：1.05~1.35mol/L Na are added into mixed solution2CO3Or K2CO3Solution to pH be 8.25~8.35 Afterwards, reaction generates precipitation；
S3：Precipitation obtained by S2 is placed at 5~45 DEG C evaporable water to get layered double-metal hydroxide LDH- Cl-I-CO3Whisker.
The present invention is to layered double hydroxide LDH-Cl-I-CO3Preparation process explore it is found that raw material and its Proportioning, pH regulation and control and temperature regulation and control have significant impact to the pattern of final layered double hydroxide.Such as metal cation Mg2+And Al3+, anion I-、Cl-、CO32-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-Cl-I- of crystal whisker-shaped by the preferred of this series of conditions CO3, 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-I-CO3The extremely excellent natural resources of whisker.But these resources cannot get always science, high level It 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 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 Cl-Source, the natural resources can be made full use of, it is cost-effective, have important economic value.
Preferably, the MgI2And AlCl3From Qinghai Salt Lake bittern.It is further preferable that the MgI2And AlCl3Come Derived from Cha Er Han Salt Lake bittern bittern.
Preferably, it is 7.5 that pH is adjusted in S1.
Preferably, Mg in S1 mixed solutions2+A concentration of 1.2mol/L；Al in S1 mixed solutions3+It is a concentration of 0.8mol/L。
Preferably, Na described in S22CO3Or K2CO3A concentration of 1.2mol/L of solution.
Preferably, Na is added in S22CO3Or K2CO3Solution to pH be 8.3.
Preferably, the reaction time of S2 is 135~145h.
It is further preferable that the reaction time of S2 is 140h.
In order to preferably regulate and control pH, prevent pH too low or fluctuation be excessive, it is preferable that in S2 per 6h by add NaOH or KOH solution adjusts the pH of mixed solution, and the changing value for adding the pH before and after NaOH or KOH solution every time is less than 0.05.
Preferably, the NaOH of the addition or a concentration of 0.0085~0.0115mol/L of KOH solution.
In order to enable moisture evaporation is more uniformly distributed, it is preferable that further including wind step in S3 makes moisture evaporation, the wind Wind speed be 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 S2 can be placed at the spaciousness of Qinghai Salt Lake area, water is realized using natural solar energy and wind energy resources by~5m/s Divide slow evaporation, not only saves energy and realize green chemical industry.
Above-mentioned layered double hydroxide (LDH-Cl-I-CO3) whisker prepare toughened and reinforced material, catalysis material, Application in 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-Cl-I-CO provided by the invention3Whisker 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-Cl-I-CO3The route map of whisker；
Fig. 2 is the layered double hydroxide LDH-Cl-I-CO that embodiment 1 provides3The shape appearance figure of whisker；
Fig. 3 is layered double hydroxide LDH-Cl-I-CO prepared by the embodiment of the present invention 13The XRD diagram of whisker；
Fig. 4 is the shape appearance figure of sample prepared by comparative example 1 of the present invention.
Specific implementation mode
With reference to embodiment, the present invention will be further described.These embodiments are retouched to the typical case of the present invention It states, however, the present invention is not limited thereto.Test method as used in the following examples is conventional method unless otherwise specified；Made Raw materials and reagents etc. are unless otherwise specified that can be commercially available from conventional commercial sources.
Embodiment 1
The present embodiment provides a kind of layered double hydroxide LDH-Cl-I-CO3Whisker, chemical formula Mg6Al2 (OH)14ClICO3·4H2O, preparation method are following (such as Fig. 1)：
S1：Prepare 4.80molL-1MgI2·8H2O and 1.6molL-1AlCl3·6H2O solution takes this two kinds of solution to exist Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to pH with the NaOH solution of 0.01mol/L =7.50, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this phenomenon and do not interfere with follow-up LDH- Cl-I-CO3The growth of whisker.
S2：Prepare the Na of 1.2mol/L2CO3Solution is added to while stirring in the mixed liquor obtained by two steps, is added always To the pH to pH=8.30 of system, then by system be placed in sun-drenched place allow expose to the weather 140h (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 140h, added every 6 hours The NaOH solution for entering a 0.010mol/L, the amount being added every time are：The pH value for first measuring current arrangements, is then added alkali, makes PH value increase by 0.05 unit, for example, measure at this time system pH be 8.05, then be added alkali when be added to system pH always Terminate when being 8.10.
The layered double hydroxide LDH-Cl-I-CO that the present embodiment is prepared3The draw ratio of whisker be 15~ 25:1, good dispersion, whisker good crystalline have preferable toughened and reinforced function, such as Fig. 1；In addition, from its XRD diffraction pattern (as schemed 2) as can be seen that layered double hydroxide LDH-Cl-I-CO3Layer structure of the compound with LDH be (layer structure LDH is in (003) crystal face diffracted intensity maximum, followed by (006) crystal face, and minimum is (009), this is because lamellar compound pair Caused by " delustring " effect of XRD.
Whisker manufactured in the present embodiment is prepared into sample and carries out elemental analysis, elemental analysis of samples result acquired results row In table 1, table 1 statistics indicate that, embodiment 1 provide sample substantially conform to nMg:nAl:nCl:nI:nC=6:2:1:1, in conjunction with oxygen (oxygen Content be to be obtained by minusing), protium content, can deduce its chemical formula be Mg6Al2(OH)14ClICO3·4H2O。
1 LDH-Cl-I-CO of table3Elemental analysis result
Embodiment 2
The present embodiment provides a kind of layered double hydroxide LDH-Cl-I-CO3Whisker, chemical formula Mg6Al2 (OH)14ClICO3·4H2O, preparation method are as follows：
S1：Prepare 4.2molL-1MgI2·8H2O and 1.9molL-1AlCl3·6H2O solution takes this two kinds of solution to exist Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to the NaOH solution of 0.0085mol/L PH=7.45, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this phenomenon and do not interfere with subsequently LDH-Cl-I-CO3The growth of whisker.
S2：Prepare the Na of 1.05mol/L2CO3Solution is added to while stirring in the mixed liquor obtained by two steps, is added always To the pH to pH=8.25 of system, then by system be placed in sun-drenched place allow expose to the weather 145h (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 145h, added every 6 hours The NaOH solution for entering a 0.0085mol/L, the amount being added every time are：The pH value for first measuring current arrangements, is then added alkali, makes PH value increase by 0.05 unit, for example, measure at this time system pH be 8.10, then be added alkali when be added to system pH always Terminate when being 8.15.
The layered double hydroxide LDH-Cl-I-CO that the present embodiment is prepared3The draw ratio of whisker be 15~ 25:1, good dispersion, whisker good crystalline, XRD diffraction patterns have the diffractive features of LDH.Therefore, it has LDH structures Whisker.
Embodiment 3
The present embodiment provides a kind of layered double hydroxide LDH-Cl-I-CO3Whisker, chemical formula Mg6Al2 (OH)14ClICO3·4H2O, preparation method are as follows：
S1：Prepare 5.4molL-1MgI2·8H2O and 1.3molL-1AlCl3·6H2O solution takes this two kinds of solution to exist Stirring volumetric is mixed in a beaker, and the pH value of mixed system is adjusted to the NaOH solution of 0.0115mol/L PH=7.55, at this point, due to Al3+The hydrolysis of ion and so that solution is become muddy, but generate this phenomenon and do not interfere with subsequently LDH-Cl-I-CO3The growth of whisker.
S2：Prepare the Na of 1.35mol/L2CO3Solution is added to while stirring in the mixed liquor obtained by two steps, is added always To the pH to pH=8.35 of system, then by system be placed in sun-drenched place allow expose to the weather 135h (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 135h, added every 6 hours The NaOH solution for entering a 0.0115mol/L, the amount being added every time are：The pH value for first measuring current arrangements, is then added alkali, makes PH value increase by 0.05 unit, for example, measure at this time system pH be 8.25, then be added alkali when be added to system pH always Terminate when being 8.30.
The layered double hydroxide LDH-Cl-I-CO that the present embodiment is prepared3The draw ratio of whisker be 18~ 23:1, good dispersion, whisker good crystalline, XRD diffraction patterns have the diffractive features of LDH.Therefore, it has LDH structures Whisker.
Comparative example 1
This comparative example provides a kind of layered double hydroxide LDH-Cl-I-CO3Preparation method, in the preparation method Except preparing MgI in S12·8H2Outside a concentration of 1.8mol/L of O solution, remaining step and operation consistent, the party with embodiment 1 Method cannot get whisker, and scanning electron microscope (SEM) photograph is as shown in Figure 3：Sample does not have crystal whisker-shaped as seen from Figure 3.
Comparative example 2
This comparative example provides a kind of layered double hydroxide LDH-Cl-I-CO3Preparation method, in the preparation method Except preparing AlCl in S13·6H2Outside a concentration of 0.6mol/L of O solution, remaining step and operation consistent, the party with embodiment 1 Method cannot get whisker.
Comparative example 3
This comparative example provides a kind of layered double hydroxide LDH-Cl-I-CO3Preparation method, in the preparation method Except Na is added in S22CO3The pH of solution to system is outside 10.0, remaining step is consistent with embodiment 1 with operation, and this method obtains Less than whisker.
Comparative example 4
This comparative example provides a kind of layered double hydroxide LDH-Cl-I-CO3Preparation method, in the preparation method Except Na is added in S22CO3Outside a concentration of 0.2mol/L of solution, remaining step is consistent with embodiment 1 with operation, and this method obtains Less than whisker.
Comparative example 5
This comparative example provides a kind of layered double hydroxide LDH-Cl-I-CO3Preparation method, in the preparation method In addition to system is placed in 90 DEG C in S2, remaining step is consistent with embodiment 1 with operation, and this method cannot get whisker.

Claims (10)

1. a kind of layered double hydroxide LDH-Cl-I-CO3Whisker, which is characterized in that the chemical formula of the whisker is Mg6Al2（OH）14ClICO3·4H2O；The whisker passes through metal cation Mg2+And Al3+With anion I-、Cl-、CO32-With OH-Evaporable water obtains after reacting to precipitate.
2. the layered double-metal hydroxide LDH-Cl-I-CO of claim 13The preparation method of whisker, which is characterized in that institute Preparation method is stated to include the following steps：
S1：Prepare MgI2And AlCl3Mixed solution, being adjusted to pH with the NaOH of 0.0085 ~ 0.0115mol/L or KOH solution is 7.45~7.55；Mg in the mixed solution2+A concentration of 2.1 ~ 2.7mol/L, Al3+A concentration of 0.65 ~ 0.95mol/L；
S2：1.05 ~ 1.35 mol/L Na are added into mixed solution2CO3Or K2CO3After solution is 8.25 ~ 8.35 to pH, reaction Generate precipitation；
S3：Precipitation obtained by S2 is placed at 5 ~ 45 DEG C evaporable water to get layered double-metal hydroxide LDH-Cl-I-CO3 Whisker.
3. layered double hydroxide LDH-Cl-I-CO according to claim 23The preparation method of whisker, feature exist In it is 7.5 to adjust pH in S1.
4. layered double hydroxide LDH-Cl-I-CO according to claim 23The preparation method of whisker, feature exist In Mg in S1 mixed solutions2+A concentration of 2.4mol/L；Al in S1 mixed solutions3+A concentration of 0.8mol/L.
5. layered double hydroxide LDH-Cl-I-CO according to claim 23The preparation method of whisker, feature exist In Na described in S22CO3Or K2CO3A concentration of 1.2 mol/L of solution.
6. layered double hydroxide LDH-Cl-I-CO according to claim 23The preparation method of whisker, feature exist In Na is added in S22CO3Or K2CO3Solution to pH be 8.3.
7. layered double hydroxide LDH-Cl-I-CO according to claim 23The preparation method of whisker, feature exist In the reaction time of S2 is 135 ~ 145h.
8. layered double hydroxide LDH-Cl-I-CO according to claim 73The preparation method of whisker, feature exist In the pH of mixed solution being adjusted by adding NaOH or KOH solution per 6h in S2, before and after adding NaOH or KOH solution every time PH changing value be not more than 0.05.
9. layered double hydroxide LDH-Cl-I-CO according to claim 23The preparation method of whisker, feature exist In further including wind step in S3 makes moisture evaporation, and the wind speed of the wind is 4 ~ 5m/s.
10. the layered double-metal hydroxide LDH-Cl-I-CO of claim 13Whisker is preparing toughened and reinforced material, catalysis Application in material, fire proofing or sorbing material.
CN201810297640.1A 2018-03-30 2018-03-30 A kind of layered double hydroxide LDH-Cl-I-CO3Whisker and its preparation method and application Withdrawn CN108425151A (en)

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