CN108611683B - Layered double metal hydroxide LDH-Cl4Preparation method and application of whisker - Google Patents

Layered double metal hydroxide LDH-Cl4Preparation method and application of whisker Download PDF

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CN108611683B
CN108611683B CN201810276507.8A CN201810276507A CN108611683B CN 108611683 B CN108611683 B CN 108611683B CN 201810276507 A CN201810276507 A CN 201810276507A CN 108611683 B CN108611683 B CN 108611683B
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吴健松
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Abstract

The invention relates to a layered double metal hydroxide LDH-Cl4A preparation method and application of the whisker. The preparation method comprises the following steps: s1, preparing MgCl2Solution with AlCl3Adding alkali to regulate pH value to 7.50, S2, evaporating and crystallizing the mixed solution in S1 until the precipitate is completely precipitated, detecting system pH value every 7.7 ~ 8.3.3 h in the evaporation process, adding 0.02mol/L NaOH solution to increase system pH value by 0.05, filtering and washing the precipitate to obtain the layered double hydroxide LDH-Cl4A whisker. The preparation method provided by the invention forms LDH-Cl with special appearance, composition and crystal structure by controlling the feeding ratio, the pH value of a reaction system, the reaction temperature and the reaction time4The preparation method of the whisker is simple, environment-friendly, efficient and energy-saving, and the obtained LDH-Cl4The whisker can be widely applied to toughening and reinforcing materials, catalytic materials, flame retardant materials and adsorption materials.

Description

Layered double metal hydroxide LDH-Cl4Preparation method and application of whisker
Technical Field
The invention belongs to the field of layered double-metal hydroxide materials, and particularly relates to layered double-metal hydroxide LDH-Cl4A preparation method and application of the whisker.
Background
Layered Double Hydroxides (LDH) are a general name of Hydrotalcite (HT) and Hydrotalcite-Like Compounds (HTlc), are important inorganic functional materials, have the functions of catalysis, adsorption, flame retardance and the Like, and are environment-friendly multifunctional inorganic materials. The most typical LDH is Mg6Al2(OH)16CO3.4H2O, also known as Mg-Al hydrotalcite, if the Mg in the Mg-Al hydrotalcite2+、A13+Or CO3 2-The ion is replaced by other ion to obtain hydrotalcite-like compound (HTLc).
The formula of HTLc is:(wherein M is2+Is a divalent metal ion, such as Mg2+、Ni2+、Co2+、Zn2+、Cu2+Etc.; m3+Being trivalent metal ions, e.g. Al3+、Cr3+、Fe3+、Sc3+Etc.; a is an interlayer anion, e.g. CO3 2-、NO3-、Cl-、SO4 2-、 PO4 3-、C6H4(COO)2 2-Etc.; m is the number of interlaminar bound water)
Figure GDA0002208074910000012
The sheet layers formed are called metal sheet layers and are composed of
Figure GDA0002208074910000013
The composed layer is referred to as an anionic layer. Such a layered structure is shown in fig. 1.
For LDH compounds, studies at home and abroad have mainly focused on the substitution of divalent cations of metal sheet layers, for example, magnesium ions by copper ions or cobalt ions, and there are also designs in which anions are substituted by some organic biomolecules such as amino acids. Intercalated LDH composite materials containing copper, cobalt, nickel, organic acid, polyacid and the like are designed by Beijing university of chemical industry, a plurality of scholars study LDH preparation technology abroad, and LDH is used as a catalyst to synthesize a plurality of important organic compounds and inorganic compounds which are used as fire retardants, adsorbents and the like. However, to date, for the preparation of LDH-Cl4Whiskers cannot be reported or searched, few reports can be found for preparing LDH into whisker shapes, most of the preparation routes of LDH are prepared by using certain whiskers (such as magnesium hydroxide whiskers) as precursors, and the preparation technical routes are long and high in cost.
Therefore, the development of a simple and easy whisker-shaped LDH compound has great research significance and application value.
Disclosure of Invention
The invention aims to overcome the defects that the technical route for preparing the whisker-shaped LDH compound is long in the prior art,the preparation cost is high, and the like, and provides a layered double metal hydroxide LDH-Cl4A method for preparing crystal whisker.
It is another object of the present invention to provide a layered double hydroxide LDH-Cl prepared by the method4A whisker.
It is another object of the present invention to provide the layered double hydroxide LDH-Cl as described above4The crystal whisker is applied to preparing toughening and reinforcing materials, catalytic materials, flame-retardant materials or adsorbing materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
layered double metal hydroxide LDH-Cl4The preparation method of the whisker comprises the following steps:
s1, preparing MgCl2·6H2Solution of O and AlCl3·6H2O solution, mixing, adding alkali to adjust pH of the mixed solution to 7.50, wherein Mg2+The concentration is 2.10-2.70 mol/L, and Al is in3+The concentration is 0.80-1.00 mol/L;
s2, evaporating and crystallizing the mixed solution in the S1 until the precipitate is completely precipitated, detecting the pH value of the system every 7.7-8.3 h in the evaporation process, adding 0.02mol/L NaOH solution to increase the pH value of the system by 0.05, filtering, washing and precipitating to obtain the layered double-metal hydroxide LDH-Cl4Whisker of the chemical formula Mg6Al2(OH)14Cl4·4H2O。
During the exploration process, the inventor unexpectedly discovers that the feeding ratio, the pH value of a reaction system, the reaction temperature, the reaction time and the like in the preparation process can be applied to the prepared LDH-Cl4The morphology, composition and crystal structure of the whiskers have a great influence, so that the layered double hydroxide LDH-Cl of the invention can be obtained under the specific preparation conditions of the invention4A whisker.
Preferably, S1 Mg2+Concentration of 2.40mol/L, Al3+The concentration was 0.80 mol/L.
The pH adjusting base in S1 was 0.02mol/L sodium hydroxide solution.
The layered bimetal of the invention is prepared for low energy consumption, cleanness and environmental protectionHydroxide LDH-Cl4The whisker is evaporated under the condition of wind blowing and sun drying, and the evaporation condition is as follows: the temperature of the solution is 5-45 ℃, and the surface air speed of the solution is 3-5 m/s.
The Qinghai salt lake area has abundant solar energy resources and wind energy resources, the temperature is 4-45 ℃ throughout the year, the wind speed is 3-5 m/S, the S3 reaction system can be placed in the open place of the Qinghai salt lake area, the slow evaporation of water is realized by utilizing natural solar energy and wind energy resources, the energy is saved, and the green chemical industry is realized.
Preferably, the MgCl described in S12Solution with AlCl3Solutions of
A great amount of bittern is available in Qinghai salt lake (such as Lithocarpus koenigii, Theaca salt lake bittern or Kaerfeng salt lake), and is used for preparing LDH-Cl4The whisker is an excellent natural resource. However, the resources cannot be scientifically and highly utilized all the time, but are left unused all the time, which wastes salt lake resources, causes serious salinization of soil around the salt lake and withering of plants, damages the ecological environment of the salt lake and brings difficulty to the exploitation of salt field resources in the future. Fully utilizes high-quality Mg in the salt lake bittern2+And Al3+As a preparation of LDH-Cl4The raw material source of the crystal whisker can utilize high-quality resources of the salt lake to realize high-value utilization, and protect the ecological environment of the salt lake and is beneficial to the development of salt field resources.
Layered double hydroxide LDH-Cl prepared by the method4Whisker of the chemical formula Mg6Al2(OH)14Cl4·4H2O。
LDH-Cl of the invention4The whisker not only has the functions of catalysis, flame retardance and adsorption of an LDH compound, has larger specific surface area and interlaminar ion exchangeability, but also has the functions of toughening and reinforcing the whisker, has adjustable pore diameter and is an environment-friendly multifunctional inorganic material.
The layered double hydroxide LDH-Cl described above4The application of the whisker in preparing toughening reinforcing material, catalytic material, flame retardant material or adsorption material is also protected by the inventionWithin the range.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a layered double metal hydroxide LDH-Cl4Whiskers, LDH-Cl4The whisker compound not only has the functions of catalysis, flame retardance and adsorption of the LDH compound, but also has the functions of toughening and reinforcing of the whisker, has adjustable and denatured pore diameter, and is an environment-friendly multifunctional inorganic material. The preparation process of the compound forms LDH-Cl with special appearance, composition and crystal structure by controlling the charge ratio, the pH value of a reaction system, the reaction temperature and the reaction time4The preparation method of the whisker is simple, environment-friendly, efficient and energy-saving, and the obtained LDH-Cl4The whisker can be widely applied to toughening and reinforcing materials, catalytic materials, flame retardant materials and adsorption materials.
Drawings
Fig. 1 is a schematic view of the layered structure of HTLc.
FIG. 2 is a diagram showing the preparation of layered double hydroxides LDH-Cl4A roadmap of whiskers.
FIG. 3 is the layered double hydroxide LDH-Cl prepared in example 14XRD pattern of whiskers.
FIG. 4 is the layered double hydroxide LDH-Cl of example 14SEM image of whiskers.
FIG. 5 is a diagram of layered double hydroxide LDH-Cl prepared in comparative example 14SEM image of whiskers.
Detailed Description
The present invention will be further described with reference to the following examples. These examples are merely representative descriptions of the present invention, but the present invention is not limited thereto. The test methods used in the following examples are all conventional methods unless otherwise specified; the raw materials and reagents used, etc., are all commercially available from conventional sources unless otherwise specified.
Example 1
Layered double metal hydroxide LDH-Cl4Whisker of the formula Mg6Al2(OH)14Cl4·4H2And O. The preparation method comprises the following flow chart of figure 2The method comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2Solution from AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.40mol/L, and Al is in3+The concentration is 0.80 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: firstly measuring the pH value of the current system, then adding alkali to increase the pH value by 0.05 unit, filtering, washing and precipitating to obtain the layered double metal hydroxide LDH-Cl4A whisker.
The evaporation process is carried out under the conditions that the temperature of the solution is 40 ℃ and the surface wind speed of the solution is 4 m/s.
Example 2
Layered double metal hydroxide LDH-Cl4The whisker has a chemical formula shown in figure 1, and the preparation method comprises the following steps:
s1, preparing MgCl from Qinghai salt lake bittern2Solution with AlCl3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.20mol/L, and Al is in3+The concentration is 0.90 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: firstly measuring the pH value of the current system, then adding alkali to increase the pH value by 0.05 unit, filtering, washing and precipitating to obtain the layered double metal hydroxide LDH-Cl4A whisker.
The evaporation process is carried out under the conditions that the temperature of the solution is 10 ℃ and the surface wind speed of the solution is 5 m/s.
Example 3
Layered double metal hydroxide LDH-Cl4A whisker having the chemical formulaThe preparation method has the flow shown in figure 1 and comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2Solution from AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.60mol/L, and Al is in3+The concentration is 0.90 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: firstly measuring the pH value of the current system, then adding alkali to increase the pH value by 0.05 unit, filtering, washing and precipitating to obtain the layered double metal hydroxide LDH-Cl4A whisker.
Example 4
Layered double metal hydroxide LDH-Cl4The whisker has a chemical formula shown in figure 1, and the preparation method comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2Solution from AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.10mol/L, and Al is in3+The concentration is 0.80 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: firstly measuring the pH value of the current system, then adding alkali to increase the pH value by 0.05 unit, filtering, washing and precipitating to obtain the layered double metal hydroxide LDH-Cl4A whisker.
Comparative example 1
Layered double metal hydroxide LDH-Cl4The whisker has a chemical formula shown in figure 1, and the preparation method comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2The solution is prepared by mixing a solvent and a solvent,using AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.00mol/L, and Al is in3+The concentration is 0.80 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: the pH value of the current system is measured, then alkali is added to increase the pH value by 0.05 unit, and the precipitate is filtered and washed.
Comparative example 2
Layered double metal hydroxide LDH-Cl4The whisker has a chemical formula shown in figure 1, and the preparation method comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2Solution from AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.80mol/L, and Al is in3+The concentration is 0.80 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: the pH value of the current system is measured, then alkali is added to increase the pH value by 0.05 unit, and the precipitate is filtered and washed.
Comparative example 3
Layered double metal hydroxide LDH-Cl4The whisker has a chemical formula shown in figure 1, and the preparation method comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2Solution from AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.40mol/L, and Al is in3+Has a concentration of 0.70 mol-L；
S2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: the pH value of the current system is measured, then alkali is added to increase the pH value by 0.05 unit, and the precipitate is filtered and washed.
Comparative example 4
Layered double metal hydroxide LDH-Cl4The whisker has a chemical formula shown in figure 1, and the preparation method comprises the following steps:
s1, using MgCl2·6H2O preparation of MgCl2Solution from AlCl3·6H2Preparation of AlCl from O3Mixing the two solutions in a beaker under stirring, and adjusting pH of the mixed system to 7.50 with 0.01mol/L NaOH solution, wherein Mg is added2+The concentration is 2.40mol/L, and Al is in3+The concentration is 1.10 mol/L;
s2, preparing 0.02mol/L NaOH solution, adding the NaOH solution into the mixed system in batches, and adding the NaOH solution once every 8 hours, wherein the adding amount of each time is as follows: the pH value of the current system is measured, then alkali is added to increase the pH value by 0.05 unit, and the precipitate is filtered and washed.
Result detection
(1) Whisker structure detection
The whisker junction prepared in example 1 was examined by X-ray diffraction (XRD) examination.
From the XRD test, it was found that the layered double hydroxide LDH-Cl prepared in example 1 was4The XRD results of the whiskers are shown in fig. 3. Examples 2 to 5 of the obtained layered double hydroxide LDH-Cl4The XRD results of the whiskers were the same as in example 1.
As shown in FIG. 3, the layered double hydroxide LDH-Cl prepared in example 14XRD pattern of whiskers. The diffraction characteristic peak shows that the sample has sharp peak shape, and the position and the intensity of each main diffraction peak show that the substance is LDH-Cl with a layered structure4As can be seen from the XRD diffraction pattern of the layered double hydroxide LDH-Cl4The compounds having LDHThe layered structure (LDH of the layered structure diffracts the intensity in the (003) plane maximally, followed by the (006) plane, and the smallest being (009) due to the "extinction" effect of the layered compound on XRD.
(2) Topography detection
The layered double hydroxide LDH-Cl prepared in example 1 was examined by Scanning Electron Microscopy (SEM)4The appearance of the whiskers is calculated by biological microscope observation4Aspect ratio of the whisker. The aspect ratio structure of the whiskers is shown in Table 3 below, LDH-Cl prepared in example 14FIG. 4 shows a scanning electron micrograph of whiskers, the sample having whisker-like shape, LDH-Cl prepared in comparative example 14The sem image of the whiskers is shown in fig. 5, and do not have the whisker shape.
TABLE 3
Figure GDA0002208074910000071
(3) Composition detection
The results of elemental analysis of the samples are shown in Table 4, and the data in Table 4 show that the samples substantially satisfy nMg:nAl:nS:nCWhen oxygen (oxygen content obtained by subtraction) and hydrogen are combined together, the chemical formula is assumed to be Mg6Al2(OH)14Cl4·4H2O。
TABLE 4 LDH-Cl4Results of elemental analysis
ω(Mg)％ ω(Al)％ ω(Cl)％ ω(H)％ Mg/Al/Cl
22.21 8.38 21.79 3.39 0.925:0.310:0.614

Claims (7)

1. Layered double metal hydroxide LDH-Cl4The preparation method of the whisker is characterized by comprising the following steps:
s1, preparing MgCl2Solution with AlCl3Mixing the solutions, adding base to adjust pH of the mixed solution to 7.50, wherein Mg2+Al with a concentration of 2.1-2.7 mol/L3+The concentration is 0.8-1.0 mol/L;
s2, evaporating and crystallizing the mixed solution in the S1 until the precipitate is complete, wherein the evaporation is carried out under the condition of wind blowing and sun drying, and the evaporation condition is as follows: the temperature of the solution is 5-45 ℃, the surface air speed of the solution is 3-5 m/s, the pH value of the system is detected every 7.7-8.3 h in the evaporation process, 0.02mol/L NaOH solution is added to increase the pH value of the system by 0.05, and the layered double hydroxide LDH-Cl is obtained by filtering, washing and precipitating4Whisker of the chemical formula Mg6Al2(OH)14Cl4·4H2O。
2. The layered double hydroxide LDH-Cl as claimed in claim 14The preparation method of the whisker is characterized in that S1 Mg2 +Concentration of 2.40mol/L, Al3+The concentration was 0.80 mol/L.
3. The layered double hydroxide LDH-Cl as claimed in claim 14The preparation method of the whisker is characterized in that the alkali for adjusting the pH in S1 is 0.01mol/L sodium hydroxide solution.
4. The layered double hydroxide LDH-Cl as claimed in claim 14A process for the preparation of whiskers, characterized in that the MgCl described in S12Solution with AlCl3The mixed solution of the solution is prepared from salt lake bittern.
5. The layered double hydroxide LDH-Cl as claimed in claim 44The preparation method of the crystal whisker is characterized in that the salt lake bittern is Qinghai salt lake bittern.
6. Layered double hydroxide LDH-Cl prepared by the method of any one of claims 1 to 54Whisker of the chemical formula Mg6Al2(OH)14Cl4·4H2O。
7. The layered double hydroxide LDH-Cl as set forth in claim 64The crystal whisker is applied to preparing toughening and reinforcing materials, catalytic materials, flame-retardant materials or adsorbing materials.
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