CN112978791B - Preparation method of titanium-containing layered double hydroxides - Google Patents
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Abstract
The invention provides a preparation method of titanium-containing layered double hydroxides, 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 TiCl to the hydroxide mixture dispersion4Fully stirring to obtain a suspension, and then standing and aging; after the reaction is finished, filtering, washing and drying to obtain the titanium-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
Technical Field
The invention relates to a preparation method of titanium-containing layered double hydroxides, belonging to the technical field of functional materials and preparation thereof.
Background
Layered Double Hydroxides (LDHs) are a class of anionic clays whose structure is based on brucite, in which part of the divalent cations are replaced by trivalent or tetravalent cations, forming positively charged platelets, with anions inserted between the layers maintaining the charge balance. The species of the metal ions and the interlayer anions are different, so that LDHs with different properties can be formed. 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, medical carriers, 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 utilizes the high-speed vibration and rotation of a ball mill to enable hard balls to 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 chemical reaction is induced to synthesize LDHs. For example: chinese patent document CN109179338A provides a method for preparing layered double hydroxides by one-step mechanical ball milling, comprising the steps of: putting divalent metal salt and trivalent metal salt into a ball milling tank of a planetary ball mill, adding ammonia water and grinding balls, carrying out ball milling for 2-3 h at the rotating speed of 470r/min, taking out slurry obtained after ball milling, adding distilled water, carrying out ultrasonic treatment and centrifugation, carrying out vacuum drying at 120 ℃ until the weight of a sample is constant, and grinding to obtain the target product, namely the nano layered double hydroxide.
In recent years, titanium-containing inorganic materials have attracted much attention, and the synthesis of titanium-containing LDHs (Ti-LDHs) is also a research hotspot. The Ti-LDHs has the advantages of high specific surface area, strong recoverability and the like, and is expected to play an important role in the fields of photocatalysis, pesticide slow release, adsorption and the like. However, the reported Ti-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. For example: chinese patent document CN102784614A provides a method for preparing layered double hydroxide containing tetravalent metal ions, which adopts a coprecipitation method, comprising the steps of: dropwise adding the metal mixed salt solution and the alkali solution into a reaction container by using a peristaltic pump, fully reacting under stirring, controlling the reaction pH to be about 10, aging the mixed solution at a certain temperature after the reaction is finished, carrying out centrifugal solid-liquid separation, washing the solid, drying at constant temperature and grinding. However, the coprecipitation method has the disadvantages of high yield of polluted water, long washing time and the like.
Therefore, the development of a green, simple and economical preparation method of titanium-containing layered double hydroxides (Ti-LDHs) is still necessary and urgent. The invention is therefore proposed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of titanium-containing layered double hydroxide. The invention uses metal hydroxide and TiCl4The 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 method for preparing titanium-containing layered double hydroxides 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 TiCl 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 the titanium-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 invention, the TiCl in step (2)4The molar ratio of the metal ion to the trivalent metal ion in the hydroxide mixture dispersion liquid is 0.15 to 0.5:1, and more preferably 0.2 to 0.4: 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 titanium-containing layered double hydroxides (Ti-LDHs) with good crystallinity and high dispersibility, which is a novel method for synthesizing LDHs materialsTrap, reduce the diffusion activation energy of the elements, and further react with TiCl during aging4Reacting to generate titanium-containing layered double hydroxides (Ti-LDHs); the method of the invention requires strict control of TiCl4The molar ratio of the metal ion hydroxide to the trivalent metal ion hydroxide in the hydroxide mixture is too small, which results in incomplete reaction, and the molar ratio is too large, which results in the generation of impurities of divalent metal ion-titanium oxide, and the product is not pure. The method has the advantages of mild preparation conditions, low energy consumption, less sewage discharge, environmental friendliness, simple preparation process operation, high yield and easy industrialization.
2. The titanium-containing layered double hydroxide (Ti-LDHs) prepared by the invention has large specific surface area which can reach 160.9m2More than g.
3. The titanium-containing layered double hydroxide (Ti-LDHs) prepared by the invention 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-Ti LDHs prepared in example 1.
FIG. 2 is a TEM image of Mg-Al-Ti LDHs prepared in example 1.
FIG. 3 is an SEM photograph of Mg-Al-Ti LDHs prepared in example 1.
FIG. 4 is a nitrogen desorption isotherm plot of the Mg-Al-Ti 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-Ti 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 method for preparing titanium-containing layered double hydroxides 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) Adding 24. mu.L TiCl to the hydroxide mixture dispersion obtained in 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-TiLDHs powder, namely the titanium-containing layered double hydroxide powder.
The XRD pattern of the Mg-Al-TiLDHs 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 the metals in the prepared powder, Mg: Al: Ti 3.70:1.20:0.38, was determined by ICP-OES and was close to the molar ratio of the metals in the reactants, thus demonstrating the successful incorporation of Ti into the LDHs. TEM and SEM images of the Mg-Al-Ti LDHs prepared by the embodiment are respectively shown in FIG. 2 and FIG. 3, and it can be seen that the Mg-Al-Ti LDHs nanosheet prepared by the invention has a transverse dimension of 50-500 nm and a thickness of 5-20 nm. The nitrogen adsorption and desorption isotherms of the Mg-Al-Ti LDHs prepared in the example are shown in FIG. 4, and it can be seen from FIG. 4 that the obtained Mg-Al-Ti LDHs contain a large number of mesopores, have a large specific surface area, and can reach 160.9m2The specific surface area (about 10 m) of the particles is larger than that of the conventional LDHs2/g)。
Example 2
A method for preparing titanium-containing layered double hydroxides 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 16. mu.L TiCl to the hydroxide mixture dispersion obtained in 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-Ti LDHs powder, namely the titanium-containing layered double hydroxide powder.
Example 3
A method for preparing titanium-containing layered double hydroxides 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) Adding 16. mu.L TiCl to the hydroxide mixture dispersion obtained in 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 Ni-Fe-Ti LDHs powder, namely the titanium-containing layered double hydroxide powder.
Example 4
A method for preparing titanium-containing layered double hydroxides 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) Adding 16. mu.L TiCl to the hydroxide mixture dispersion obtained in 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 Co-Fe-Ti LDHs powder, namely the titanium-containing layered double hydroxide powder.
Example 5
A method for preparing titanium-containing layered double hydroxides 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) Adding 16. mu.L TiCl to the hydroxide mixture dispersion obtained in 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 Cu-Al-Ti LDHs powder, namely the titanium-containing layered double 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 it can be seen from FIG. 5 that the product contains hydrogenMagnesium oxide and aluminum hydroxide, indicating absence of TiCl4When present, the reaction does not proceed completely, since no TiCl is 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 75.4m2(ii)/g, much smaller than in inventive example 1.
Comparative example 2
A method for preparing titanium-containing layered double hydroxides 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) Adding 48. mu.L of TiCl to the hydroxide mixture dispersion obtained in step (1)4And fully 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 24 hours, naturally cooling to room temperature, filtering, washing the obtained precipitate with water for 3 times, and drying at 60 ℃ for 24 hours to obtain Mg-Al-Ti 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 the product obtained contains MgTiO3Impurities, description when TiCl4When the molar ratio of the metal hydroxide to the trivalent metal hydroxide is more than 0.5:1, pure Mg-Al-Ti LDHs cannot be generated.
Claims (12)
1. A method for preparing titanium-containing layered double hydroxides 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; what is needed isThe 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, and the ball milling time is 0.5-12 h;
(2) adding TiCl 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 titanium-containing layered double hydroxide powder; the TiCl4The molar ratio of the metal ions to the trivalent metal ions in the hydroxide mixture dispersion liquid is 0.15-0.5: 1; the aging temperature is 60-100 ℃, and the aging time is 6-48 h.
2. The method for preparing layered double hydroxide containing titanium according to claim 1, wherein the divalent metal ion in step (1) is Mg2+(ii) a The trivalent metal ion is Al3+。
3. The method for preparing layered double hydroxide containing titanium 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 layered double hydroxide containing titanium 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 titanium-containing layered double hydroxide according to claim 1, wherein the ball-milling in step (1) has a ball-to-material ratio of 40 to 60: 1.
6. The method for preparing layered double hydroxide containing titanium according to claim 1, wherein the rotation speed of the ball mill in step (1) is 1200-1800 rpm; the ball milling time is 3-6 h.
7. The process 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 the 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 the step (1) is 0.08 to 0.10 mol/L.
10. The method of claim 1, wherein the TiCl in step (2) is added to the titanium-containing layered double hydroxide4The molar ratio of the metal ions to the trivalent metal ions in the hydroxide mixture dispersion liquid is 0.2-0.4: 1.
11. The method for producing a layered double hydroxide containing titanium 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 titanium according to claim 1, wherein the washing in the step (2) is washing with water 2 to 3 times; the drying temperature is 25-80 ℃; the drying time is 3-48 h.
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| CN102553660A (en) * | 2012-01-17 | 2012-07-11 | 山东大学 | Composite of lamellar bimetal hydroxide and magnetic substrate and preparation thereof |
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| CN102553660A (en) * | 2012-01-17 | 2012-07-11 | 山东大学 | Composite of lamellar bimetal hydroxide and magnetic substrate and preparation thereof |
| CN108554439A (en) * | 2018-05-11 | 2018-09-21 | 北京化工大学 | A kind of photo-reduction CO2 ultra-thin Ti bases LDHs composite photo-catalysts and preparation method thereof |
| WO2019220081A1 (en) * | 2018-05-14 | 2019-11-21 | Scg Chemicals Co., Ltd. | Surface modified layered double hydroxide |
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