CN108486657B - Layered double metal hydroxide LDH- (NO)3)2-SO4Preparation method of whisker - Google Patents

Layered double metal hydroxide LDH- (NO)3)2-SO4Preparation method of whisker Download PDF

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CN108486657B
CN108486657B CN201810278537.2A CN201810278537A CN108486657B CN 108486657 B CN108486657 B CN 108486657B CN 201810278537 A CN201810278537 A CN 201810278537A CN 108486657 B CN108486657 B CN 108486657B
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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
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    • 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
    • C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
    • C30B7/04—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents
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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
    • 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 invention discloses a layered double metal hydroxide LDH- (NO)3)2‑SO4The preparation method of the whisker comprises the following steps: s1, preparing Mg (NO)3)2·6H2O and Al2(SO4)3·18H2S3, placing the mixed system of S2 at the temperature of 5 ~ ℃ to evaporate water for 101 ~ h, adding second strong base solution every 9h in the process of evaporating water, and adding the second strong base solution every time to increase the pH value of the mixed system by 0.05 to obtain the layered double-metal hydroxide LDH- (NO)3)2‑SO4A whisker. The preparation method does not use the crystal whisker as a precursor, and has simple and easy operation, simple and reasonable technical route and low cost; prepared layered double hydroxide LDH- (NO)3)2‑SO4The whisker not only has all functions of LDH, such as catalysis, adsorption, flame retardance and the like, but also has the toughening and reinforcing functions of the whisker, is an environment-friendly multifunctional inorganic material, and has wide application prospect.

Description

Layered double metal hydroxide LDH- (NO)3)2-SO4Preparation method of whisker
Technical Field
The invention relates to the technical field of layered double hydroxides, and in particular relates to layered double hydroxide LDH- (NO)3)2-SO4A preparation method of the whisker.
Background
Layered Double Hydroxides (LDHs) are a general term for Hydrotalcite (HT) and Hydrotalcite-Like Compounds (HTLc), and are important inorganic functional 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:
Figure RE-GDA0001648269160000011
(M-0, 1,2 … N) (wherein M is2+Is twoValent metal ions, e.g. 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 RE-GDA0001648269160000012
The sheet layers formed are called metal sheet layers and are composed of
Figure RE-GDA0001648269160000013
The composed layer is referred to as an anionic layer. Such a layered structure may be as shown in fig. 4.
Much work has been done on LDH compounds at home and abroad to conduct this research, and promising results have been achieved in the respective fields. The research at home and abroad mainly focuses on the replacement of divalent cations of metal plate layers, such as the replacement of magnesium ions by copper ions or cobalt ions, and the replacement of anions by organic biomolecules such as amino acids is also designed. In China, great achievements are made on the research of LDH by Beijing university of chemical industry. They have made great research results in the field of designing intercalated LDH composite materials containing copper, cobalt, nickel, organic acid, polyacid and the like. In foreign countries, many scholars have enjoyed a lot of results in the preparation of LDH, the synthesis of many important organic and inorganic compounds using LDH as a catalyst, the research of flame retardants and adsorbents, and the like, and provide a lot of useful experimental data. Reports on the preparation of LDHs in the form of whiskers are also rare, and most of the preparation routes use certain whiskers (such as magnesium hydroxide whiskers) as precursors, or the preparation technical routes are long and high in cost. Furthermore, the chemical formula of Mg has not been prepared in the prior art6Al2(OH)14(NO3)2SO4·5H2LDH whiskers of O.
In addition, solar energy, as a new energy source, is equivalent to about 130 trillion tons of coal of solar radiation energy reaching the earth's surface every year, and the total amount thereof is the largest energy source that can be developed in the world today. Compared with conventional energy sources such as electric energy and the like, the energy-saving device has three characteristics: firstly, the method comprises the following steps: it is the most abundant energy source available to humans. It is estimated that in the past 11 billion years, the sun has consumed 2% of its own energy. The product is enough for global human to use for billions of years in the future, and can be used inexhaustibly. Secondly, the method comprises the following steps: solar energy is available anywhere on the earth, can be developed and utilized on site, and is particularly significant for remote areas such as Qinghai salt lakes, islands and the like where traffic is not available. Thirdly, the method comprises the following steps: solar energy is a clean energy source. When in use, the utility model does not produce waste residue, waste water and waste gas, has no noise and does not influence ecological balance. Absolutely does not cause pollution and public nuisance. The method is highly consistent with the low-energy-consumption clean and environment-friendly utilization of salt lake resources, and has important scientific significance for developing and utilizing the salt lake resources at low cost and high value and protecting the ecological environment of the salt lake.
Disclosure of Invention
The present invention overcomes the above-mentioned drawbacks of the prior art by providing a layered double hydroxide LDH- (NO)3)2-SO4A preparation method of the whisker.
Another object of the present invention is to provide a layered double hydroxide LDH- (NO)3)2-SO4And (5) crystal whiskers.
In order to solve the technical problems, the invention adopts the technical scheme that:
layered double metal hydroxide LDH- (NO)3)2-SO4The preparation method of the whisker comprises the following steps:
s1, preparing Mg (NO)3)2·6H2O and Al2(SO4)3·18H2Mixed solution of O, said Mg (NO)3)2·6H2The concentration of O is 2.1-2.7 mol/L, and the Al is2(SO4)3·18H2The concentration of O is 0.35-0.45 mol/L;
s2, adjusting the pH value of the mixed solution prepared in the S1 to 7.95-8.05 by adopting a first strong alkali solution to obtain a mixed system;
s3, placing the mixed system of the S2 at the temperature of 5-45 ℃ to evaporate water for 101-111 h to obtain the layered double hydroxide LDH- (NO)3)2-SO4Whisker; and adding a second strong alkali solution every 9 hours in the process of evaporating water, wherein the pH value of the mixed system is increased by 0.05 by adding the second strong alkali solution every time, and the concentration of the second strong alkali solution is 0.01 mol/L.
Said layered double hydroxide LDH- (NO)3)2-SO4The chemical formula of the whisker is Mg6Al2(OH)14(NO3)2SO4·5H2O。
During the research process of the inventor, the inventor occasionally finds that Mg (NO) is controlled3)2·6H2O and Al2(SO4)3·18H2The dosage ratio and the concentration of O, the addition amount of strong base, the pH value, the temperature and the time for evaporating water are in the specific ranges, and the layered double hydroxide LDH- (NO) can be prepared3)2-SO4A whisker. The preparation method does not use the crystal whisker as a precursor, and has simple and easy operation, simple and reasonable technical route and low cost.
Layered double hydroxide LDH- (NO) prepared by the invention3)2-SO4The whisker not only has all functions of LDH, but also has adjustable pore diameter, larger specific surface area and interlaminar ion exchangeability, such as catalysis, adsorption, flame retardance and the like, and also has the toughening and reinforcing functions of the whisker, thereby being an environment-friendly multifunctional inorganic material and having wide application prospect.
The method can scientifically and high-value utilize the huge amount of bittern in the Qinghai salt lake, avoid the idling and waste of bittern resources in the Qinghai salt lake, is favorable for improving the ecological environment of the salt lake while utilizing the bittern, relieves the salinization of soil around the salt lake and reduces the difficulty in mining the salt field resources. In addition, in the preparation process, solar energy can be utilized, energy can be saved, and green chemical industry is realized.
Preferably, said Mg (NO)3)2·6H2O concentration of 2.40mol/L, Al2(SO4)3·18H2The concentration of O was 0.40 mol/L.
Preferably, the evaporative moisture is wind-blown sunlight.
In the Qinghai salt lake region, the solar energy and the wind energy are fully utilized by blowing and sunning the wind, so that the energy is effectively saved, and the green chemical industry is realized.
In the process of blowing and drying by the sun, the temperature of the mixed system is 5-45 ℃, the place is Qinghai Guelder, the air humidity is 10-50%, the air pressure is 72kPa, and the air speed is 1-12 m/s.
Preferably, the first strong base solution is a NaOH solution or a KOH solution.
More preferably, the first strong base solution is a NaOH solution.
NaOH is less costly than KOH. The use of NaOH solution as the first strong alkaline solution can save costs.
Preferably, the concentration of the first strong alkali solution is 0.01-0.02 mol/L.
More preferably, the concentration of the first strong base solution is 0.01 mol/L. The pH of the mixed solution can be more conveniently adjusted using a low concentration of the first strong alkaline solution.
Preferably, in S2, the pH of the mixed solution prepared in S1 is adjusted to 7.45-7.55 by using a first strong alkali solution, and after 60min, the pH is adjusted to 7.95-8.05. Can prevent the crystal whisker generation from being influenced by too fast alkali adding speed.
Preferably, the second strong alkali solution is a NaOH solution or a KOH solution.
More preferably, the second strong alkaline solution is a NaOH solution.
Preferably, S3. further comprises reacting said layered double hydroxide LDH- (NO)3)2-SO4Filtering, washing and drying whiskerThe step (2).
Preferably, the washing is performed with distilled water.
Preferably, the drying temperature is 60-80 ℃, and the drying time is 36-48 h.
The invention also protects the layered double hydroxide LDH- (NO) prepared by the preparation method3)2-SO4A whisker.
The layered double hydroxide LDH- (NO) described above3)2-SO4The application of the whisker in the flame-retardant material is also within the protection scope of the invention.
Compared with the prior art, the invention has the beneficial effects that:
the invention controls Mg (NO)3)2·6H2O and Al2(SO4)3·18H2The dosage ratio and concentration of O, the addition amount of strong base, the pH value, the temperature and the time for evaporating water are in the specific range of the invention, and the layered double hydroxide LDH- (NO) can be prepared3)2-SO4A whisker. The preparation method does not use crystal whiskers as a precursor, and has the advantages of simple and easy operation, simple and reasonable technical route and low cost; prepared layered double hydroxide LDH- (NO)3)2-SO4The whisker has adjustable pore diameter, larger specific surface area and interlaminar ion exchangeability, not only has all functions of LDH, such as catalysis, adsorption, flame retardance and the like, but also has the toughening and reinforcing functions of the whisker, is an environment-friendly multifunctional inorganic material, and has wide application prospect.
Drawings
FIG. 1 is the layered double hydroxide LDH- (NO) of example 13)2-SO4SEM image of whiskers.
FIG. 2 is a layered double hydroxide LDH- (NO) of comparative example 13)2-SO4SEM image of whiskers.
FIG. 3 is the layered double hydroxide LDH- (NO) of example 13)2-SO4XRD pattern of whiskers.
Fig. 4 is a schematic view of the layered structure of hydrotalcite-like compound HTLc.
Detailed Description
The present invention will be further described with reference to the following embodiments. The raw materials in the examples are all commercially available;
in the embodiment, the whisker ratio is estimated by observing through a scanning microscope, and the result is the mass fraction; the length-diameter ratio of the crystal whisker is also observed by a scanning microscope.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. The wind blowing and sun drying in the invention are carried out in the Qinghai salt lake area.
Example 1
The preparation method of this example is as follows:
(1) 4.80mol/L Mg (NO) is prepared3)2·6H2O and 0.80mol/LAl2(SO4)3·18H2And (3) taking the two solutions, mixing the two solutions in a beaker in an equal volume under stirring, wherein the volume is 4.00L, and adjusting the pH value of a mixed system to be 7.50 by using 0.01mol/L NaOH solution to obtain a mixed solution, wherein in the mixed solution, Al is used as the raw material3+Hydrolysis of the ions renders the solution cloudy, but this does not affect the subsequent LDH- (NO)3)2-SO4And (5) growing the whisker.
(2) And (2) adding 0.010mol/L NaOH solution into the mixed solution obtained in the step (1) while stirring until the pH value of the system is 8.0, then placing the system in a sunny place, allowing the system to be exposed to wind for 106 hours, wherein the temperature of the system in the process of exposure to wind is 5-45 ℃, filtering, washing, precipitating and drying to obtain the sample. During the 106h period, 0.010mol/L NaOH solution is added every 9 hours, and the adding amount is as follows: the pH value of the current system is measured, and then 0.010mol/L NaOH solution is added to increase the pH value by 0.05 unit.
Examples 2 to 4
The concentrations of the reaction materials and the reaction conditions in examples 2 to 4 are shown in Table 1, and the other operation steps are the same as those in example 1.
TABLE 1 concentrations of reaction raw materials and reaction conditions of examples 1 to 4
Figure BDA0001614116460000051
Comparative examples 1 to 7
The concentrations of the reaction materials and the reaction conditions in comparative examples 1 to 7 are shown in Table 2, and the other operation steps are the same as those in example 1.
TABLE 2 reaction raw material concentrations and reaction conditions of comparative examples 1 to 7
Figure BDA0001614116460000061
Carry out the test
(1) SEM test, scanning electron microscope of PHILIPS-SL-30 type; RM2000 type microscopic confocal Raman spectrometer.
(2) XRD test, X-ray diffraction (XRD): x-ray diffractometer model D/Max-3C (Riguka, japan, copper target,graphite curved crystal monochromator), the scanning speed is 0.02 degree/s, the scanning range is: 10 to 70 degrees.
(3) Performing elemental analysis, wherein an ULTIMA type plasma emission spectrometer, a French JY company, is adopted for measuring magnesium and aluminum elements; and a PE2400Series II CHNS/O element analyzer is adopted for measuring the carbon, nitrogen, hydrogen and sulfur elements.
TABLE 3 aspect ratio and whisker proportion of examples 1 to 4
Example 1 Example 2 Example 3 Example 4
Whisker proportion 97％ 96％ 96％ 97％
Aspect ratio 26:1 25:1 25:1 22:1
Table 4 elemental analysis results of example 1
Figure BDA0001614116460000062
The results of the SEM test of example 1 are shown in FIG. 1, and it can be seen that the sample had a whisker shape, good dispersibility, good crystal form, aspect ratio and whisker proportion as shown in Table 3. While the layered double metal hydroxide LDH- (NO) was not obtained in comparative examples 1 to 73)2-SO4The SEM test result shows that the product is in an amorphous whisker shape; wherein the SEM test results of the product of comparative example 1 are shown in fig. 2.
FIG. 3 is the layered double hydroxide LDH- (NO) prepared in example 13)2-SO4XRD pattern of whiskers. The diffraction characteristic peak shows that the sample has a sharp peak shape, and the position and the intensity of each main diffraction peak indicate that the substance has a layered structure of LDH. LDH with layered structure diffracts the intensity in the (003) plane most, followed by the (006) plane and the smallest (009), due to the "extinction" of the layered compound to XRD "The effect is caused. The diffraction peaks corresponding to the (003), (006), and (009) planes are shown in FIG. 3. Examples 2 to 4 of the prepared layered double hydroxides LDH- (NO)3)2-SO4The XRD results of the whiskers were the same as in example 1.
The elemental analysis results of example 1 are shown in Table 4, and the product substantially conforms to nMg:nAl:nS:nNWhen oxygen (oxygen content obtained by the subtraction method) and hydrogen are combined together, the chemical formula is assumed to be Mg6Al2(OH)14(NO3)2SO4·5H2And O. The test results of examples 2 to 4 were the same as those of example 1, and basically satisfied with the formula Mg6Al2(OH)14(NO3)2SO4·5H2O。
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. It will be apparent to those skilled in the art that other variations and modifications can be made on the basis of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (8)

1. Layered double metal hydroxide LDH- (NO)3)2-SO4A whisker, which is characterized in that,
said layered double hydroxide LDH- (NO)3)2-SO4The chemical formula of the whisker is Mg6Al2(OH)14(NO3)2SO4·5H2O；
Layered double hydroxide LDH- (NO)3)2-SO4The preparation method of the whisker comprises the following steps:
s1, preparing Mg (NO)3)2·6H2O and Al2(SO4)3·18H2Mixed solution of O, said Mg (NO)3)2·6H2The concentration of O is 2.1-2.7 mol/L, and the Al is2(SO4)3·18H2The concentration of O is 0.35-0.45 mol/L;
s2, adjusting the pH value of the mixed solution prepared in the S1 to 7.95-8.05 by adopting a first strong alkali solution to obtain a mixed system;
s3, placing the mixed system of the S2 at the temperature of 5-45 ℃ to evaporate water for 101-111 h to obtain the layered double hydroxide LDH- (NO)3)2-SO4Whisker; and adding a second strong alkali solution every 9 hours in the process of evaporating water, wherein the pH value of the mixed system is increased by 0.05 by adding the second strong alkali solution every time, and the concentration of the second strong alkali solution is 0.01 mol/L.
2. Layered double hydroxide LDH- (NO) according to claim 13)2-SO4Whisker, characterized in that said Mg (NO)3)2·6H2O concentration of 2.40mol/L, Al2(SO4)3·18H2The concentration of O was 0.40 mol/L.
3. Layered double hydroxide LDH- (NO) according to claim 13)2-SO4The whisker is characterized in that the first strong alkali solution is NaOH solution or KOH solution.
4. Layered double hydroxide LDH- (NO) according to claim 1 or 33)2-SO4The whisker is characterized in that the concentration of the first strong alkali solution is 0.01-0.02 mol/L.
5. Layered double hydroxide LDH- (NO) according to claim 1 or 33)2-SO4The whisker is characterized in that in S2, the pH of the mixed solution prepared in S1 is adjusted to 7.45-7.55 by using a first strong alkali solution, and after 60min, the pH is adjusted to 7.95-8.05.
6. Layered double hydroxide LDH- (NO) according to claim 13)2-SO4The whisker is characterized in that the second strong alkali solution is NaOH solution or KOH solution.
7. Layered double hydroxide LDH- (NO) according to claim 13)2-SO4A whisker, characterized in that S3. further comprises subjecting the layered double hydroxide LDH- (NO)3)2-SO4And filtering, washing and drying the crystal whisker.
8. Layered double hydroxide LDH- (NO) as claimed in any one of claims 1 to 73)2-SO4The application of the whisker in flame retardant materials.
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