CN109046357A - A kind of preparation method of metal oxide-LDH loaded catalyst - Google Patents
A kind of preparation method of metal oxide-LDH loaded catalyst Download PDFInfo
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Abstract
本发明提供了一种金属氧化物‑LDH负载型催化剂的制备方法。本发明利用LDH对于金属元素阴离子前驱体(金属含氧酸根离子)的高容量吸附特征，首先将金属含氧酸根吸附在LDH层间，然后通过还原处理将金属含氧酸根还原成金属阳离子，由于LDH层间对阳离子的排斥作用，将金属阳离子排斥出LDH层间，阳离子进一步水解形成水合金属氧化物，水合金属氧化物带有负电性，可以重新吸附到LDH外表面。本发明的制备方法在水中进行，制备过程依靠LDH材料的性质，无需高温煅烧，能耗小，流程简单，且无需进行金属氧化物颗粒尺寸调控，能够实现金属氧化物‑LDH负载型催化剂的大规模合成。
The invention provides a method for preparing a metal oxide-LDH supported catalyst. The present invention utilizes the high-capacity adsorption characteristics of LDH for metal element anion precursors (metal oxyacid ions), firstly adsorbs metal oxyacids between LDH layers, and then reduces metal oxyacids to metal cations through reduction treatment. The repulsion of cations between the LDH layers will repel the metal cations out of the LDH layers, and the cations will be further hydrolyzed to form hydrated metal oxides. The hydrated metal oxides are negatively charged and can be re-adsorbed to the outer surface of LDH. The preparation method of the present invention is carried out in water, the preparation process relies on the properties of the LDH material, does not require high-temperature calcination, has low energy consumption, simple process, and does not need to control the particle size of the metal oxide, and can realize the large-scale production of the metal oxide-LDH-supported catalyst. Scale synthesis.
Description
Technical field
The present invention relates to catalyst technical field more particularly to a kind of preparations of metal oxide-LDH loaded catalyst
Method.
Background technique
LDH (Layered double hydroxides) is layered double hydroxide, and layer structure possesses huge
Specific surface area, be capable of providing a large amount of absorption, catalytic site.Material itself has " memory effect ", is being lower than 400 DEG C of temperature
Lower calcined dehydration can form metal composite oxide, after absorbing water into the water, can be re-converted to layer structure.In higher temperature
The lower calcining of degree can be changed into spinelle, be used as electrode material, catalyst etc..
Using LDH as substrate, metal oxide-loaded (Fe2O3, Cr2O3, MnO2) composite catalyst be widely used
In Industrial Catalysis, the fields such as environmental improvement.For example, α-Fe2O3/ NiCoAl-LDH can be used as electrocatalysis material oxidation water, γ-
Fe2O3/ NiFe-LDH is used for Degradation of Organo-pollutants in Water with Photo-catalysis, Fe2O3/ CuMgAl-LDH is hydrocracked for glycerine,
Fe3O4/WO4 2-- LDH and H2O2Selective oxidation sulfurous organic compound, Cr2O3Sulfuric acid decomposition is anti-in/LDH catalytic water/syngas conversion reactor
It answers, MnO2/ LDH catalysis oxidation VOCs etc..Therefore, before this metal oxide-LDH loaded catalyst has a wide range of applications
Scape.
Above-mentioned metal oxide-LDH loaded catalyst is matched frequently with Co deposited synthesis first, in accordance with the ion of LDH
LDO (metal composite oxide) is prepared than configuring mixed salt solution, then by co-precipitation and high-temperature calcination, then by LDO
It is immersed in metal salt solution, LDO obtains hydroxyl in the solution and is changed into LDH, while Hydrolysis Reactions of Metal-ions forms hydration gold
Belong to oxide nano particles and be supported on the surface LDH, hydrated metal oxide is dehydrated after drying, and it is negative to obtain metal oxide-LDH
Supported catalyst.But this preparation method needs high-temperature calcination, energy consumption is larger, and the nanotopography of metal oxide can not
Control is easy to reunite.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of metal oxide-LDH loaded catalyst.The present invention mentions
The preparation method of confession does not need high-temperature calcination, can be completed at normal temperature, and the metal oxide nanoparticles on the surface LDH are not easy
Reunite.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
A kind of preparation method of metal oxide-LDH loaded catalyst, comprising the following steps:
(1) metal matrix reagent and water are mixed, obtains the first solution；The metal matrix reagent is that divalent metal is solvable
The mixture of property salt and trivalent metal soluble-salt；
(2) metal oxyacid salts are dissolved in alkaline solution, obtain the second solution；
(3) first solution is added in the second solution and carries out coprecipitation reaction, obtain suspension；
(4) suspension is separated by solid-liquid separation, obtains solid product；
(5) solid product and reducing agent aqueous solution are mixed and carries out reduction treatment, it is dry after reduzate is separated,
Obtain metal oxide-LDH loaded catalyst；
Step (1)~(4) carry out under nitrogen protection；
The limitation of the not no time sequencing in the step (1) and (2).
Preferably, the divalent metal soluble-salt includes CaCl2、MgCl2、Ca(NO3)2With Mg (NO3)2One of or
It is several；The trivalent metal soluble-salt includes AlCl3And/or Al (NO3)3。
Preferably, in the metal matrix reagent molar ratio of bivalent metal ion and trivalent metal ion be 1.5~
4.0:1。
Preferably, the metal oxyacid salts include one of ferrate, permanganate, bichromate and chromate
Or it is several.
Preferably, the molar ratio of metal ion total amount is 0.5~3:5 in the metal oxyacid salts and matrix agent.
Preferably, the alkaline solution is sodium hydroxide solution or ammonia spirit.
Preferably, the time of the coprecipitation reaction is 1~16h, and temperature is 7~25 DEG C.
Preferably, the reducing agent includes ascorbic acid and/or sodium sulfite.
Preferably, the molar ratio of the reducing agent and metal oxyacid salts is 1~3:1.
Preferably, the time of the reduction treatment is 0.3~5h, and temperature is 7~25 DEG C.
The present invention provides a kind of preparation methods of metal oxide-LDH loaded catalyst.The present invention utilizes LDH pairs
In the high capacity adsorpting characteristic of the element anions such as Fe, Cr, Mn presoma (metal oxygen-containing acid group), first by metal oxygen-containing acid group
It is adsorbed on LDH interlayer, metal oxygen-containing acid group is then reduced into metal cation by restoring, since LDH interlayer is to cation
Repulsive interaction, metal cation is ejected from into LDH interlayer, cation further hydrolyzes to form hydrated metal oxide, is hydrated
Metal oxide has elecrtonegativity, can be adsorbed onto the outer surface LDH again.Preparation method of the invention carries out in water, preparation
Process relies on the property of LDH material, is not necessarily to high-temperature calcination, and energy consumption is small；The present invention be added reducing agent after metal oxoanions also
Originally it was that metal ion is synchronous with the process that Hydrolysis Reactions of Metal-ions is hydrated metal oxide nano particle to carry out, gained catalyst
Performance is only related with metal ion ratio, and process is simple；Preparation method of the invention is without carrying out metal oxide particle size
Regulation, and metal oxide particle is not easy to reunite, can be realized the extensive synthesis of metal oxide-LDH loaded catalyst.
Detailed description of the invention
Fig. 1 is that the SEM of 1 step of embodiment (3) obtained solid product schemes；
Fig. 2 is Fe prepared by embodiment 12O3@Ca2The SEM of Al-LDH loaded catalyst schemes.
Specific embodiment
The present invention provides a kind of preparation methods of metal oxide-LDH loaded catalyst, comprising the following steps:
(1) metal matrix reagent and water are mixed, obtains the first solution；The metal matrix reagent is divalent metal oxidation
The mixture of object and trivalent metal oxide, or the mixture for divalent metal soluble-salt and trivalent metal soluble-salt；
(2) metal oxyacid salts are dissolved in alkaline solution, obtain the second solution；
(3) first solution is added in the second solution and carries out coprecipitation reaction, obtain suspension；
(4) suspension is separated by solid-liquid separation, obtains solid product；
(5) solid product and reducing agent aqueous solution are mixed and carries out reduction treatment, it is dry after reduzate is separated,
Obtain metal oxide-LDH loaded catalyst；
Step (1)~(4) carry out under nitrogen protection；
The limitation of the not no time sequencing in the step (1) and (2).
The present invention mixes metal matrix reagent and water, obtains the first solution.In the present invention, the metal matrix reagent
For the mixture of divalent metal soluble-salt and trivalent metal soluble-salt；The divalent metal soluble-salt preferably includes
CaCl2、MgCl2、Ca(NO3)2With Mg (NO3)2One or more of；The trivalent metal soluble-salt preferably includes AlCl3
And/or Al (NO3)3；The molar ratio of bivalent metal ion and trivalent metal ion is preferably 1.5~4.0 in the matrix agent:
1, more preferably 2~3:1.It include simultaneously bivalent metal ion and trivalent metal ion in the first solution of the invention, subsequent
Coprecipitation process in, bivalent metal ion and trivalent metal ion form layered double hydroxide.
The present invention does not have particular/special requirement to the matrix agent and water hybrid mode, can completely dissolve in water matrix
?.In the present invention, the total concentration of the first solution mesostroma reagent preferably (0,100) g/L, more preferably 20~
50g/L。
Metal oxyacid salts are dissolved in alkaline solution, the second solution is obtained.In the present invention, the metal oxyacid salts
Including one or more of ferrate, permanganate, bichromate and chromate；The metal oxyacid salts and matrix examination
The molar ratio of metal ion total amount is preferably 0.5~3:5 in agent, more preferably 1~2:5, further preferably 2:5；The alkali
Property solution is preferably sodium hydroxide solution or ammonia spirit；The concentration of solute is preferably the first GOLD FROM PLATING SOLUTION in the alkaline solution
Belong to 2~3 times, more preferably 2.5 times of total ion concentration.
After obtaining the first solution and the second solution, first solution is added in the second solution and is co-precipitated by the present invention
Reaction, obtains suspension.In the present invention, the time of the coprecipitation reaction is preferably 1~16h, more preferably 3~10h, into
One step is preferably 4h, and temperature is preferably 7~25 DEG C, and more preferably 10~20 DEG C.The second solution is added in first solution by the present invention
In, it is excessively high to avoid local basicity.
During coprecipitation reaction, bivalent metal ion and trivalent metal ion react under alkaline condition, raw
At layered double hydroxide, the characteristic that layered double hydroxide has high capacity to adsorb anion, thus by metal oxygen-containing
Acid ion is adsorbed on interlayer.
After obtaining suspension, the suspension is separated by solid-liquid separation by the present invention, obtains solid product.In the present invention,
The separation of solid and liquid is preferably centrifugated, and the revolving speed of the centrifugation is preferably 4000~5000rpm, more preferably 4500rpm；
The present invention does not have particular/special requirement to the time of the centrifuge separation, can be kept completely separate solid product.
After the completion of centrifuge separation, the present invention is preferably successively washed and is freeze-dried to centrifugation product, obtains solid phase production
Object.In the present invention, the washing is preferably washed, and the number of the washing is preferably 2 times；The present invention is to the freeze-drying
Temperature and time there is no particular/special requirement, can make be centrifuged product be completely dried.
The present invention mixes reducing agent and water, obtains reducing agent solution.In the present invention, the reducing agent preferably includes to resist
Bad hematic acid and/or sodium sulfite；The molar ratio of the reducing agent and metal oxyacid salts is preferably 1~3:1, and more preferably 1.5
~2.5:1；The concentration of the reducing agent solution is preferably that the first metal ion in solution total concentration is 2~3 times, and the present invention is preferred
The volume of water is determined according to the quality of the total concentration of the first metal ion in solution and required reducing agent.The present invention is gone back to described
The hybrid mode of former agent and water does not have particular/special requirement, can completely dissolve in water reducing agent.
After obtaining reducing agent solution, the reducing agent and water are mixed and carry out reduction treatment by the present invention.In the present invention, institute
The temperature for stating reduction treatment is preferably 7~25 DEG C, and more preferably 10~20 DEG C, the time of reduction treatment is preferably 0.3~5h, more
Preferably 2~3h, more preferably 2.5h.
In the present invention, step (1)~(4) are in N2It is carried out under protective condition, to prevent the CO in air2It is dissolved in
Replace the metal oxygen-containing acid group of intercalation in solution.
In reduction treatment process, the metal oxygen-containing acid group of absorption LDH interlayer is reduced to metal cation, metal sun from
Son ejects from interlayer by LDH and enters in water, is then hydrolyzed to hydrated metal oxide nano particle, hydrated metal oxide in water
Object has elecrtonegativity, is attracted to the surface LDH.In the present invention, above-mentioned reaction occurs simultaneously in reduction treatment process, this hair
It is bright by LDH interlayer to the suction-operated of anion and to cation repulsive interaction based on, whole preparation process in water into
Row is not necessarily to high-temperature calcination, and metal oxide particle is not easy to reunite.In the present invention, the partial size of the metal oxide is 30
~150nm.
After the completion of reduction treatment, the present invention preferably filters the reaction solution of step (6), and gained solid product is dry,
In drying process, hydrated metal oxide dehydration forms metal oxide nanoparticles, obtains metal oxide-LDH support type
Catalyst.The present invention does not have particular/special requirement to the filtering and dry specific method, can be realized separation of solid and liquid and by solid-state
Product is completely dried.
It is carried out below with reference to preparation method of the embodiment to metal oxide-LDH loaded catalyst provided by the invention
Detailed description, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) 0.888g CaCl is weighed respectively2And 0.966gAlCl3·6H2O is dissolved in 50mL deionized water and forms first
Solution；
(2) 2.3g NaOH is dissolved in 150mL deionized water, and 0.794g potassium ferrate is added into above-mentioned NaOH solution,
It stirs evenly, forms the second solution.
(3) the first solution is quickly poured into the second solution, is stirred 4 hours under 25 degrees Celsius, form suspension.
(4) suspension is centrifugated at 4500rpm using supercentrifuge, and cleans two with 150mL deionized water
It is secondary to obtain solid product；
(5) using ascorbic acid as reducing agent, configuration concentration is the ascorbic acid solution of 50mg/L；Solid product is added to
It is reacted 2 hours in ascorbic acid solution；Solid product drying is arrived di-iron trioxide supported catalyst by reaction solution filtering
Agent (Fe2O3@Ca2Al-LDH loaded catalyst)
Step (1)~(4) keep N2Atmosphere reduces CO2Introducing.
To step (3) obtained solid product be scanned Electronic Speculum detection, acquired results as shown in Figure 1, wherein Fig. 1 (a) and
Fig. 1 (b) is respectively SEM figure of solid product different parts under the conditions of 100000 times of amplification factors；According to Fig. 1 as can be seen that
The solid product has apparent layer structure, illustrates that coprecipitation reaction generates layered double hydroxide.
To gained Fe2O3@Ca2Al-LDH loaded catalyst be scanned Electronic Speculum detection, acquired results as shown in Fig. 2, its
Middle Fig. 2 (a) is Fe2O3@Ca2SEM figure of Al-LDH loaded catalyst under the conditions of 100000 times of amplification factors, Fig. 2 (b) are
Fe2O3@Ca2SEM figure of Al-LDH loaded catalyst under the conditions of 50000 times of amplification factors.According to fig. 2 as can be seen that three oxygen
Change two iron nano-particles and is dispersed in layered double hydroxide surface, and soilless sticking phenomenon.
Embodiment 2
(1) 0.768g Mg (NO is weighed respectively3)2·6H2O and 0.375gAl (NO3)3·9H2O is dissolved in 50mL deionization
The first solution is formed in water；
(2) 0.794g potassium permanganate is added into above-mentioned ammonia spirit in 150mL deionized water for 2.0g ammonia solvent,
It stirs evenly, forms the second solution.
(3) the first solution is quickly poured into the second solution, is stirred 4 hours under 20 degrees Celsius, form suspension.
(4) suspension is centrifugated at 4500rpm using supercentrifuge, and cleans two with 150mL deionized water
It is secondary to obtain solid product；
(5) using sodium sulfite as reducing agent, configuration concentration is the sodium sulfite solution of 50mg/L；Solid product is added to
It is reacted 2 hours in sodium sulfite solution；Solid product drying is arrived manganese sesquioxide managnic oxide supported catalyst by reaction solution filtering
Agent (Mn2O3@Mg2Al-LDH loaded catalyst)
Step (1)~(4) keep N2Atmosphere reduces CO2Introducing.
Electronic Speculum detection is scanned to step (3) obtained solid product, acquired results and embodiment 1 are similar.
To gained Mn2O3@Mg2Al-LDH loaded catalyst is scanned Electronic Speculum detection, 1 phase of acquired results and embodiment
Seemingly.
As seen from the above embodiment, preparation method step provided by the invention is simple, metal oxide particle uniform particle sizes,
And uniform adsorption is less prone to agglomeration on two layer metal oxide surface, the present invention carries out gold using the property of LDH material
Belong to the preparation of oxide-LDH loaded catalyst, whole preparation process is simple, quick, is easy to be mass produced.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of metal oxide-LDH loaded catalyst, comprising the following steps:
(1) metal matrix reagent and water are mixed, obtains the first solution；The metal matrix reagent is divalent metal soluble-salt
With the mixture of trivalent metal soluble-salt；
(2) metal oxyacid salts are dissolved in alkaline solution, obtain the second solution；
(3) first solution is added in the second solution and carries out coprecipitation reaction, obtain suspension；
(4) suspension is separated by solid-liquid separation, obtains solid product；
(5) solid product and reducing agent aqueous solution are mixed and carries out reduction treatment, it is dry after reduzate is separated, it obtains
Metal oxide-LDH loaded catalyst；
Step (1)~(4) carry out under nitrogen protection；
The limitation of the not no time sequencing in the step (1) and (2).
2. preparation method according to claim 1, which is characterized in that the divalent metal soluble-salt includes CaCl2、
MgCl2、Ca(NO3)2With Mg (NO3)2One or more of；The trivalent metal soluble-salt includes AlCl3And/or Al
(NO3)3。
3. preparation method according to claim 1 or 2, which is characterized in that in the metal matrix reagent divalent metal from
The molar ratio of son and trivalent metal ion is 1.5~4.0:1.
4. preparation method according to claim 1, which is characterized in that the metal oxyacid salts include ferrate, height
One or more of manganate, bichromate and chromate.
5. preparation method according to claim 1, which is characterized in that in the metal oxyacid salts and metal matrix reagent
The molar ratio of metal ion total amount is 0.5~2:5.
6. preparation method according to claim 1, which is characterized in that the alkaline solution is sodium hydroxide solution or ammonium hydroxide
Solution.
7. preparation method according to claim 1, which is characterized in that the time of the coprecipitation reaction is 1~16h, temperature
Degree is 7~25 DEG C.
8. preparation method according to claim 1, which is characterized in that the reducing agent includes ascorbic acid and/or sulfurous
Sour sodium.
9. preparation method according to claim 1 or 5, which is characterized in that the reducing agent and metal oxyacid salts rub
You are than being 1~3:1.
10. preparation method according to claim 1 or 8, which is characterized in that the time of the reduction treatment is 0.3~5h,
Temperature is 7~25 DEG C.
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| CN114931954A (en) * | 2022-04-26 | 2022-08-23 | 浙江工业大学 | Two-stage photocatalyst of ferrate composite titanium-zinc layered double hydroxide, and preparation method and application thereof |
| CN115305481A (en) * | 2022-08-26 | 2022-11-08 | 青岛科技大学 | Chromium oxide functionalized nickel-iron hydrotalcite nanosheet and preparation method and electrocatalysis application thereof |
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