CN113023730B - Preparation method of silicon-containing layered double hydroxide - Google Patents

Preparation method of silicon-containing layered double hydroxide Download PDF

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CN113023730B
CN113023730B CN202110348675.5A CN202110348675A CN113023730B CN 113023730 B CN113023730 B CN 113023730B CN 202110348675 A CN202110348675 A CN 202110348675A CN 113023730 B CN113023730 B CN 113023730B
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侯万国
田震
杜娜
李海平
宋淑娥
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Abstract

The invention provides a preparation method of silicon-containing layered double hydroxide, which comprises the following steps: mixing divalent metal ion hydroxide and trivalent metal ion hydroxide, and performing ball milling to obtain a hydroxide mixture; then dispersing the obtained hydroxide mixture in a solvent to obtain hydroxide mixture dispersion liquid; adding SiCl to the hydroxide mixture dispersion4Fully stirring to obtain a suspension, and then standing and aging; and after the reaction is finished, filtering, washing and drying to obtain the silicon-containing layered double hydroxide powder. The method has the advantages of mild experimental conditions, simple operation, low energy consumption, less sewage discharge, high yield, easy industrialization and the like. The prepared product has high specific surface area and crystallinity, and has great application value in the fields of catalysis, energy storage, flame retardants, composite materials and the like.

Description

Preparation method of silicon-containing layered double hydroxide
Technical Field
The invention relates to a preparation method of a silicon-containing layered double hydroxide, belonging to the technical field of functional materials and preparation thereof.
Background
Layered Double Hydroxides (LDHs), also known as hydrotalcite-like compounds, are hydroxides having a hydrotalcite crystal structure composed of two or more metal elements. LDHs have a layered structure, the layered plate has a positive charge due to isomorphous substitution, and exchangeable anions exist between layers, so that the LDHs are layered materials which are attracted by attention in recent years. The LDHs has the advantages of high specific surface area, good metal ion dispersibility, small crystal grain size, adjustable composition (such as anion and cation types), easy realization of functionalization by compounding with other materials, simple synthesis method, low price and the like, thereby showing wide application prospect in the fields of adsorbents, energy storage materials, electromagnetic materials, flame retardants, catalysts, organic-inorganic hybrid materials and the like.
The preparation method of the LDHs mainly comprises a coprecipitation method, a hydrothermal method, a mechanical method and the like. The coprecipitation method is a method for generating LDHs by using a metal ion salt mixed solution forming an LDHs laminate under the action of a coprecipitator (alkali). The LDHs prepared by the method has high crystallinity and good dispersibility, but has the defects of high polluted water yield, long washing time and the like. The synthesis of LDHs by the hydrothermal method also has the advantages of high crystallinity, good dispersibility and the like, but the reaction temperature is high (above 140 ℃), the reaction time is long and the energy consumption is high. The mechanical method is a method of inducing a chemical change by changing the form, crystal structure, and the like of a solid substance under the action of a mechanical force. The method uses the high-speed vibration and rotation of the ball mill to make the hard balls strongly impact, grind and stir hydroxides or oxides, so that powder particles generate plastic deformation and a large number of defects, the diffusion activation energy of elements is reduced, and further chemical reaction is induced to synthesize LDHs.
In recent years, researches on doping of tetravalent cations into LDHs are receiving wide attention, and synthesis of silicon-containing LDHs (Si-LDHs) is a research hotspot. As the quadrivalent cations are doped, the adsorption performance of the composite material is obviously improved, and the composite material is expected to play an important role in the fields of wastewater purification, organic matter recycling, pharmaceutical carriers and the like. However, the reported Si-LDHs are mainly prepared by a coprecipitation method or a hydrothermal method, and have a single synthesis method, which causes environmental pollution and energy waste.
Therefore, the development of a green, simple and economical preparation method of the Si-LDHs still has necessity and urgency. The invention is therefore proposed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a silicon-containing layered double hydroxide. The invention uses metal hydroxide and SiCl4The method has the advantages of mild conditions, low energy consumption, less sewage discharge, environmental friendliness, simple and convenient preparation process, high yield and easy industrialization.
The technical scheme of the invention is as follows:
a preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) mixing divalent metal ion hydroxide and trivalent metal ion hydroxide, and performing ball milling to obtain a hydroxide mixture; then dispersing the obtained hydroxide mixture in a solvent to obtain hydroxide mixture dispersion liquid;
(2) adding SiCl to the hydroxide mixture dispersion obtained in step (1)4Fully stirring to obtain a suspension, and then standing and aging; and after the reaction is finished, filtering, washing and drying to obtain the silicon-containing layered double hydroxide powder.
Preferably according to the invention, the divalent metal ion in step (1) is Mg2+、Mn2+、Fe2+、Co2+、Ni2+、Cu2 +、Zn2+Or Ca2+One or two, more preferably Mg2+(ii) a The trivalent metal ion is Al3+、Cr3+、Mn3+、Fe3+、Co3+Or La3+One or two kinds of them, more preferably Al3+。
According to the present invention, the molar ratio of the divalent metal ions to the trivalent metal ions in the hydroxide mixture in step (1) is preferably 2 to 4:1, and more preferably 3 to 3.5: 1.
According to the invention, the ball-to-material ratio of the ball milling in the step (1) is preferably 1-60: 1, more preferably 40-60: 1, and even more preferably 49: 1.
According to the invention, the rotation speed of the ball milling in the step (1) is preferably 200-2000 rpm, more preferably 1200-1800 rpm, and even more preferably 1500 rpm; the ball milling time is 0.5-12 h, preferably 3-6 h, and more preferably 4 h.
According to the invention, the solvent in the step (1) is water or a salt solution, and the salt solution is NaNO3、NaCl、KNO3Or KCl aqueous solution, wherein the concentration of the salt solution is 0.1-0.5 mol/L; preferably, the solvent is water.
According to the present invention, the concentration of the hydroxide mixture dispersion in the step (1) is preferably 0.05 to 0.30mol/L, and more preferably 0.08 to 0.10 mol/L; the concentration refers to the total concentration of divalent metal ion hydroxide and trivalent metal ion hydroxide.
Preferably, according to the present invention, the SiCl in the step (2)4The molar ratio of the metal ion to the trivalent metal ion in the hydroxide mixture dispersion liquid is 0.10 to 0.3:1, and more preferably 0.2 to 0.25: 1.
According to the invention, the aging temperature in the step (2) is preferably 60-100 ℃, and more preferably 80 ℃; the aging time is 6-48 h, more preferably 12-30 h, and still more preferably 24 h.
Preferably, the washing in the step (2) is washing with water for 2-3 times; the drying temperature is 25-80 ℃, and the preferable temperature is 60 ℃; the drying time is 3-48 h, and more preferably 24 h.
The invention has the following technical characteristics and beneficial effects:
1. the invention adopts a mechanical-low temperature hydrothermal method to synthesize the silicon-containing layered double hydroxides (Si-LDHs) with good crystallinity and high dispersibility, and is a novel method for synthesizing LDHs materials.
2. The method of the invention leads the metal hydroxide particles to generate plastic deformation and a large number of defects by ball milling, reduces the diffusion activation energy of elements and further leads the elements to react with SiCl in the aging process4Reacting to generate silicon-containing layered double hydroxides (Si-LDHs); the method of the invention requires strict control of SiCl4Too low a molar ratio to the trivalent metal ion hydroxide in the hydroxide mixture results in incomplete reaction with the remainder of the divalent metal ion hydroxide and the trivalent metal ion hydroxide, and too high a molar ratio results in the remainder of the divalent metal ion hydroxide with impure product.
3. The silicon-containing layered double hydroxide (Si-LDHs) prepared by the invention has large specific surface area and can be used for preparingUp to 116.9m2The polymer has important application value in the fields of catalysis, energy storage, flame retardants, composite materials and the like.
Drawings
FIG. 1 is an XRD pattern of Mg-Al-Si LDHs prepared in example 1.
FIG. 2 is a TEM image of Mg-Al-Si LDHs prepared in example 1.
FIG. 3 is an SEM photograph of Mg-Al-Si LDHs prepared in example 1.
FIG. 4 is a nitrogen desorption isotherm plot of Mg-Al-Si LDHs prepared in example 1.
FIG. 5 is an XRD pattern of Mg-Al LDHs prepared in comparative example 1.
FIG. 6 is a nitrogen desorption isotherm diagram of Mg-Al LDHs prepared in comparative example 1.
FIG. 7 is an XRD pattern of Mg-Al LDHs prepared in comparative example 2.
Detailed Description
The present invention is further illustrated by the following specific examples, which are set forth to provide a further description and explanation of the invention, but are not intended to limit the invention to the precise form set forth.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1
A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) 2.864g of magnesium hydroxide, 1.136g of aluminum hydroxide and 196g of agate balls (ball-to-material ratio 49:1) are weighed and added into a 100mL ball-milling tank, and ball milling is carried out at 1500rpm for 4 hours to obtain a hydroxide mixture; 0.178g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) To the hydroxide mixture dispersion obtained in step (1), 17. mu.L of SiCl was added4Stirring thoroughly to obtain suspension, transferring the suspension into a glass bottle, placing in an oven at 80 deg.C, standing and aging for 24 hr, naturally cooling to room temperature, filtering, and precipitatingWashing with water for 3 times, and drying at 60 deg.C for 24 hr to obtain Mg-Al-Si LDHs powder, i.e. silicon-containing layered double hydroxide powder.
The XRD pattern of the Mg-Al-Si LDHs prepared in this example is shown in FIG. 1, and the interlayer spacing d003Similar to the traditional Mg-Al LDHs and has no impurity peak, and as can be seen from figure 1, the LDHs are formed in the invention; the molar ratio of Mg to Al to Si in the prepared powder was 3.10:1.20:0.0.26, as measured by ICP-OES, which was close to the molar ratio of Mg, Al, Si in the reactants, thus demonstrating the successful incorporation of Si into the LDHs. TEM and SEM images of the Mg-Al-Si LDHs prepared by the embodiment are respectively shown in FIG. 2 and FIG. 3, and it can be seen that the Mg-Al-Si LDHs nanosheet prepared by the invention has a transverse dimension of 50-500 nm and a thickness of 5-10 nm. The nitrogen desorption isotherms of the Mg-Al-Si LDHs prepared in the present example are shown in FIG. 4, and it can be seen from FIG. 4 that the obtained Mg-Al-Si LDHs contain a large amount of mesopores, have a large specific surface area, and can reach 116.9m2The specific surface area (about 10 m) of the particles is larger than that of the conventional LDHs2/g)。
Example 2
A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) 2.760g of magnesium hydroxide, 1.240g of aluminum hydroxide and 196g of agate balls (ball-to-material ratio 49:1) are weighed and added into a 100mL ball-milling pot, and ball milling is carried out at 1500rpm for 4h to obtain a hydroxide mixture; 0.163g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) Adding 8.5 mu LSiCl into the hydroxide mixture dispersion obtained in the step (1)4Fully stirring to obtain a suspension, transferring the suspension into a glass bottle, placing the glass bottle in an oven at 80 ℃, standing and aging for 24h, then naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24h to obtain Mg-Al-Si LDHs powder, namely the silicon-containing layered double hydroxide powder.
Example 3
A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) weighing 2.890g of nickel hydroxide, 1.110g of ferric hydroxide and 196g of agate balls (the ball-to-material ratio is 49:1), adding into a 100mL ball-milling tank, and carrying out ball milling at 1500rpm for 4 hours to obtain a hydroxide mixture; 0.288g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) To the hydroxide mixture dispersion obtained in step (1), 17. mu.L of SiCl was added4Fully stirring to obtain a suspension, transferring the suspension into a glass bottle, placing the glass bottle in an oven at 80 ℃, standing and aging for 24h, then naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24h to obtain Ni-Fe-Si LDHs powder, namely the silicon-containing layered double metal hydroxide powder.
Example 4
A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) 2.891g of cobalt hydroxide, 1.109g of ferric hydroxide and 196g of agate balls (ball-to-material ratio 49:1) are weighed and added into a 100mL ball-milling tank, and ball milling is carried out at 1500rpm for 4 hours to obtain a hydroxide mixture; 0.290g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) To the hydroxide mixture dispersion obtained in step (1), 17. mu.L of SiCl was added4Fully stirring to obtain a suspension, transferring the suspension into a glass bottle, placing the glass bottle in an oven at 80 ℃, standing and aging for 24h, then naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24h to obtain Co-Fe-Si LDHs powder, namely the silicon-containing layered double metal hydroxide powder.
Example 5
A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) weighing 3.158g of copper hydroxide, 0.842g of aluminum hydroxide and 196g of agate balls (ball-to-material ratio 49:1), adding into a 100mL ball-milling tank, and carrying out ball milling at 1500rpm for 4h to obtain a hydroxide mixture; 0.278g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) To the hydroxide mixture dispersion obtained in step (1), 17. mu.L of SiCl was added4Fully stirring to obtain a suspension, transferring the suspension into a glass bottle, placing the glass bottle in an oven at 80 ℃, standing and aging for 24h, then naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24h to obtain Cu-Al-Si LDHs powder, namely the silicon-containing layered double metal hydroxide powder.
Comparative example 1
A method for preparing a layered double hydroxide, comprising the steps of:
(1) 2.864g of magnesium hydroxide, 1.136g of aluminum hydroxide and 196g of agate balls (ball-to-material ratio 49:1) are weighed and added into a 100mL ball-milling tank, and ball milling is carried out at 1500rpm for 4 hours to obtain a hydroxide mixture; 0.178g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) And (2) transferring the hydroxide mixture dispersion liquid obtained in the step (1) into a glass bottle, placing the glass bottle in an oven at 80 ℃, standing and aging for 24h, naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24h to obtain Mg-Al LDHs powder.
The XRD pattern of the product prepared in this comparative example is shown in FIG. 5, and from FIG. 5 it can be seen that the product contains magnesium hydroxide and aluminum hydroxide, indicating no SiCl4When present, the reaction did not proceed completely, since no SiCl was added4The pH of the hydroxide mixture dispersion is higher. The nitrogen adsorption-desorption isotherm of the product prepared in this comparative example is shown in FIG. 6, and the specific surface area thereof is 74.23m2(ii)/g, much smaller than in inventive example 1.
Comparative example 2
A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) 2.864g of magnesium hydroxide, 1.136g of aluminum hydroxide and 196g of agate balls (ball-to-material ratio 49:1) are weighed and added into a 100mL ball-milling tank, and ball milling is carried out at 1500rpm for 4 hours to obtain a hydroxide mixture; 0.178g of the obtained hydroxide mixture was weighed and dispersed in 30mL of water with stirring to obtain a hydroxide mixture dispersion.
(2) To the hydroxide mixture dispersion obtained in step (1), 34. mu.L of SiCl was added4Fully stirring to obtain a suspension, transferring the suspension into a glass bottle, placing the glass bottle in an oven at 80 ℃, standing and aging for 24h, naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24h to obtain Mg-Al-Si LDHs powder.
The XRD pattern of the product obtained in this comparative example is shown in FIG. 7, and it can be seen from FIG. 7 that most of Mg (OH)2Unreacted, when SiCl is present4When the molar ratio of the metal ions to the trivalent metal ions is 0.46:1, pure Mg-Al-Si LDHs cannot be generated.

Claims (12)

1. A preparation method of silicon-containing layered double hydroxide comprises the following steps:
(1) mixing divalent metal ion hydroxide and trivalent metal ion hydroxide, and performing ball milling to obtain a hydroxide mixture; then dispersing the obtained hydroxide mixture in a solvent to obtain hydroxide mixture dispersion liquid; the divalent metal ion is Mg2+、Mn2+、Fe2+、Co2+、Ni2+、Cu2+、Zn2+Or Ca2+One or two of them; the trivalent metal ion is Al3+、Cr3+、Mn3+、Fe3+、Co3+Or La3+One or two of them; the ball-material ratio of the ball milling is 1-60: 1; the rotation speed of the ball milling is 200-2000 rpm; the ball milling time is 0.5-12 h;
(2) adding SiCl to the hydroxide mixture dispersion obtained in step (1)4Fully stirring to obtain a suspension, and then standing and aging; after the reaction is finished, filtering, washing and drying to obtain silicon-containing layered double hydroxide powder; the SiCl4The molar ratio of the metal ions to the trivalent metal ions in the hydroxide mixture dispersion liquid is 0.10-0.3: 1; the aging temperature is 60-100 ℃; the aging time is 6-48 h.
2. According to the claimsThe method for preparing a layered double hydroxide containing silicon according to claim 1, wherein the divalent metal ion in the step (1) is Mg2+(ii) a The trivalent metal ion is Al3+。
3. The method for preparing a layered double hydroxide containing silicon according to claim 1, wherein the molar ratio of the divalent metal ions to the trivalent metal ions in the hydroxide mixture in step (1) is 2 to 4: 1.
4. The method for preparing a layered double hydroxide containing silicon according to claim 3, wherein the molar ratio of the divalent metal ions to the trivalent metal ions in the hydroxide mixture in step (1) is 3 to 3.5: 1.
5. The method for preparing the silicon-containing layered double hydroxide according to claim 1, wherein the ball-to-material ratio of the ball milling in the step (1) is 40-60: 1.
6. The method for preparing the silicon-containing layered double hydroxide according to claim 1, wherein the rotation speed of the ball mill in the step (1) is 1200-1800 rpm; the ball milling time is 3-6 h.
7. The method for preparing a layered double hydroxide containing silicon according to claim 1, wherein the solvent in step (1) is water or a salt solution, and the salt solution is NaNO3、NaCl、KNO3Or KCl aqueous solution, wherein the concentration of the salt solution is 0.1-0.5 mol/L.
8. The method according to claim 1, wherein the concentration of the hydroxide mixture dispersion in step (1) is 0.05 to 0.30 mol/L.
9. The method according to claim 8, wherein the concentration of the hydroxide mixture dispersion in step (1) is 0.08 to 0.10 mol/L.
10. The method for preparing a layered double hydroxide containing silicon according to claim 1, wherein the SiCl is used in the step (2)4The molar ratio of the metal ions to the trivalent metal ions in the hydroxide mixture dispersion liquid is 0.2-0.25: 1.
11. The method for preparing a layered double hydroxide containing silicon according to claim 1, wherein the aging temperature in the step (2) is 80 ℃; the aging time is 12-30 h.
12. The method for preparing a layered double hydroxide containing silicon according to claim 1, wherein the washing in the step (2) is washing with water for 2 to 3 times; the drying temperature is 25-80 ℃; the drying time is 3-48 h.
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CN106241893A (en) * 2015-06-06 2016-12-21 青岛科技大学 A kind of flower ball-shaped nickel aluminum layered double hydroxide and its preparation method and application
CN111545055A (en) * 2020-06-18 2020-08-18 中国科学院大学 Application of hydrotalcite-like compound derived composite oxide material
CN111659339A (en) * 2020-06-23 2020-09-15 华东交通大学 Preparation method and application of LDHs-loaded layered nano hollow microsphere NiSiO @ NiAlFe adsorbent

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CN106241893A (en) * 2015-06-06 2016-12-21 青岛科技大学 A kind of flower ball-shaped nickel aluminum layered double hydroxide and its preparation method and application
CN111545055A (en) * 2020-06-18 2020-08-18 中国科学院大学 Application of hydrotalcite-like compound derived composite oxide material
CN111659339A (en) * 2020-06-23 2020-09-15 华东交通大学 Preparation method and application of LDHs-loaded layered nano hollow microsphere NiSiO @ NiAlFe adsorbent

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