CN104789983A - Method for preparing aluminum molybdate with cationic membrane electrolysis method - Google Patents
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Abstract
The invention discloses a method for preparing aluminum molybdate with a cationic membrane electrolysis method. An aluminum sheet is taken as an anode, an inert electrode is taken as a cathode, an aqueous solution containing a depolarizer and sodium molybdate is taken as an anolyte, an acid solution, an alkaline solution or a salt solution is taken as a catholyte, and the aqueous solution containing the depolarizer and the sodium molybdate is electrolyzed in a double-chamber electrolytic cell with a cationic membrane serving as a diaphragm with the temperature controlled to range from the room temperature to 90 DEG C in a constant-current electrolysis or constant-voltage electrolysis manner until all Na<+> ions are transferred to a cathode chamber; a product obtained in an anode chamber is washed and filtered with deionized water, an obtained filter cake is dried at the temperature of 300-400 DEG C for 1-4 h, and the aluminum molybdate which is high in purity and free of impurity phases is obtained. According to the method, the effect of cationic membrane electrolysis is used, the Na<+> ions are transferred to the cathode chamber, the effect caused by the Na<+> ions is eliminated, the reaction time is short, and the finally obtained aluminum molybdate product is high in purity and free of the impurity phases.
Description
Technical field
The present invention relates to a kind of method molybdic acid aluminium utilizing cationic membrane electrolytic preparation molybdic acid aluminium, belong to field of inorganic materials.
Technical background
Al
2(MoO
4)
3belong to A
2(MO
4)
3the compound of structure type, wherein A=Y, Sc, In, Al and the rare earth metal from Ho to Lu, M=W, Mo, belong to orthohormbic structure crystallographic system, has negative isolator CTE, due to A
2(MO
4)
3structure has larger consistency, can hold+3 valency positively charged ions of ionic radius at 67.5-107.5pm, therefore can by changing the kind of A ion or forming different A
2(MO
4)
3the sosoloid of the compound of structure type, can change the temperature that crystal structure types changes from orthogonal phase transformation monoclinic phase, thus to prepare thermal expansivity be positive and negative, zero material.Potential using value can be had in fields such as electronics, optics and micromechanicss.
Commercial conventional nontoxic corrosion inhibitor has three kinds of main Types: borate, phosphoric acid salt, molybdate pigment.Over more than 20 year for commercial applications, and its resistance to corrosion is equivalent to exceed chromic salt and lead base pigment even under certain condition molybdate always.Molybdate pigment is the secure replacement product of lead base and chromic acid base corrosion-inhibiting pigment.
At Ag
2moO
4synthesis aspect, applies more method and mainly comprises: sol-gel method, spray pyrolysis, solid state synthesis, molten-salt growth method, mechanochemical synthesis, supersonic method, masterplate method, hydrothermal method etc.But solid state synthesis method has evenly caused a lot of metal oxide impurities due to raw material mixing cloth; The shortcoming of sol-gel method, aqueous phase precipitation method, hydrothermal method, microwave method etc. has the existence of additive or reaction times longer (reach several hours even several days time).
Cationic membrane has certain selective penetrated property, can to make in anode by the cation permeable ionic membrane selected in cathode compartment, and perfluorinated sulfonic acid cationic exchange membrane can allow the Na in anolyte compartment
+ion permeable ionic membrane enters cathode compartment, thus cancellation Na
+the impact of ionic impurity.
Summary of the invention
Object of the present invention is in order to solve long reaction time in above-mentioned molybdic acid aluminium preparation process, technical problems such as impurity is many in the product of final gained and a kind of method adopting cationic membrane electrolytic process to prepare molybdic acid aluminium is provided, it is short that the method has the reaction times, the molybdic acid aluminium inclusion-free of final gained.
Technical scheme of the present invention
Utilize cationic membrane electrolytic process to prepare a method for molybdic acid aluminium, specifically comprise the steps:
(1), take aluminium flake as anode, take noble electrode as negative electrode, with the aqueous solution containing depolarizer and Sodium orthomolybdate for anolyte, with acid solution, alkaline solution or salts solution for catholyte, be in the two-compartment cell of barrier film at cationic membrane, adopt the mode of constant-current electrolysis or constant-potential electrolysis, control temperature scope is room temperature to 90 DEG C, preferably carry out the aqueous solution that electrolysis contains depolarizer and Sodium orthomolybdate, until Na from room temperature to 50 DEG C
+ion all transfers to cathode compartment;
Described noble electrode is glass-carbon electrode, Graphite Electrodes, titanium net or platinum guaze;
Described containing in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of Sodium orthomolybdate is 0.005-2.5mol/L, and be preferably 0.01-0.5mol/L, be more preferably 0.1mol/L, the concentration of depolarizer is 0.01-0.1mol/L;
Described depolarizer is nitric acid or SODIUMNITRATE;
Aqueous hydrochloric acid or the concentration of described acid solution to be concentration be 0.001-1mol/L are the aqueous sulfuric acid of 0.001-1mol/L;
Aqueous sodium hydroxide solution or the concentration of described alkaline solution to be concentration be 0.001-1mol/L are the potassium hydroxide aqueous solution of 0.001-1mol/L;
Sodium chloride aqueous solution or the concentration of described salts solution to be concentration be 0.001-1mol/L are the aqueous sodium carbonate of 0.001-1mol/L;
Described cationic membrane is perfluorinated sulfonic acid cationic exchange membrane; Be preferably the Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane that du pont company produces;
The electric current of described constant-current electrolysis is 0.08-0.8A, and be preferably 0.4-0.8A, be more preferably 0.6A, current density is 1-100mA/cm
2, be preferably 50-100mA/cm
2, be more preferably 75mA/cm
2;
The voltage of described constant-potential electrolysis is 10-300V, is preferably 20-150V, is more preferably 20V;
(2), electrolysis complete after, the cleaning limit, product deionized water limit that obtains in anolyte compartment is filtered, so that by Na
+and depolarizer cleans up, the filter cake control temperature obtained is 300-400 DEG C of dry 1-4h, obtains molybdic acid aluminium.
Beneficial effect of the present invention
A kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium of the present invention, because the cationic membrane adopted in preparation process has certain selective penetrated property, particularly Nafion series perfluorinated sulfonic acid cationic exchange membrane can allow the Na in anolyte compartment
+ion permeable ionic membrane enters cathode compartment, thus cancellation Na
+ionic impurity is on the impact of the finished product molybdic acid aluminium purity, and therefore to have the molybdic acid aluminium product purity of final gained high for preparation method of the present invention, without the feature of dephasign.
Further, a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium of the present invention, its reaction times is short, as can be seen from specific embodiment, its electrolytic preparation deficiency of time 0.5h, can obtain pure molybdic acid aluminium, therefore subsequent disposal is simple, thus preparation cost reduces.
Further, a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium of the present invention, catholyte scope used is wide, acid solution, alkali lye and saline solution are all passable, in addition, no matter electrolytic process is the mode of constant-current electrolysis or constant-potential electrolysis, can obtain pure molybdic acid aluminium.
Further, a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium of the present invention, owing to only needing one-step electrolysis can prepare molybdic acid aluminium, therefore its preparation process technique is simple, easily operates, invests little, and resultant quantity is large, can directly apply to suitability for industrialized production.
Accompanying drawing explanation
The EDS figure of the molybdic acid aluminium obtained in Fig. 1 a, embodiment 1;
The XRD figure of the molybdic acid aluminium obtained in Fig. 1 b, embodiment 1;
The EDS figure of the molybdic acid aluminium obtained in Fig. 2 a, embodiment 2;
The XRD figure of the molybdic acid aluminium obtained in Fig. 2 b, embodiment 2;
The EDS figure of the molybdic acid aluminium obtained in Fig. 3 a, embodiment 3;
The XRD figure of the molybdic acid aluminium obtained in Fig. 3 b, embodiment 3;
The EDS figure of the molybdic acid aluminium obtained in Fig. 4 a, embodiment 4;
The XRD figure of the molybdic acid aluminium obtained in Fig. 4 b, embodiment 4.
Embodiment
Also by reference to the accompanying drawings the present invention is set forth further below by specific embodiment, but do not limit the present invention.
Perfluorinated sulfonic acid cationic exchange membrane used in various embodiments of the present invention is the Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane that du pont company produces.
embodiment 1
Utilize cationic membrane electrolytic process to prepare a method for molybdic acid aluminium, specifically comprise the steps:
(1), take aluminium flake as anode, take noble electrode as negative electrode, the aqueous solution of depolarizer and Sodium orthomolybdate is contained for anolyte with 95ml, with 90ml acid solution for catholyte, be in the two-compartment cell of barrier film at cationic membrane, adopt the mode of constant-potential electrolysis, control temperature scope is the aqueous solution 10min that room temperature to 50 DEG C constant-potential electrolysis contains depolarizer and Sodium orthomolybdate;
Described noble electrode is titanium net;
Described containing in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of Sodium orthomolybdate is 0.1mol/L, and the concentration of depolarizer is 0.01mol/L, and described depolarizer is nitric acid;
The aqueous hydrochloric acid of described acid solution to be concentration be 0.1mol/L;
Described cationic membrane is Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane;
The voltage of described constant-potential electrolysis is 20V;
(2), electrolysis complete after, the cleaning limit, product deionized water limit that obtains in anolyte compartment is filtered, so that by Na
+and depolarizer cleans up, the filter cake control temperature obtained is 300 DEG C of dry 2h, obtains pure molybdic acid aluminium crystal.
The molybdic acid aluminium of 4010 type X-ray detection instrument to above-mentioned gained of German Brooker ALX company is adopted to measure, its EDS schemes as shown in Figure 1a, as can be seen from Fig. 1 a, obtain in product, only having Al, Mo, O tri-kinds of elements, indicating the molybdic acid aluminium that the present invention adopts cationic membrane electrolytic process to prepare the method gained of molybdic acid aluminium is thus pure phase, inclusion-free.
Adopt the molybdic acid aluminium of D8 Advance type x-ray diffractometer to above-mentioned gained of German Brooker AXS company to measure, as shown in Figure 1 b, as can be seen from Fig. 1 b, the product obtained is Al to its XRD figure
2(MoO
4)
3.
embodiment 2
Utilize cationic membrane electrolytic process to prepare a method for molybdic acid aluminium, concrete steps are as follows:
(1), take aluminium flake as anode, take noble electrode as negative electrode, the aqueous solution of depolarizer and Sodium orthomolybdate is contained for anolyte with 95ml, with 90ml acid solution for catholyte, be in the two-compartment cell of barrier film at cationic membrane, adopt the mode of constant-current electrolysis, control temperature scope is the aqueous solution 10min that room temperature to 50 DEG C electrolysis contains depolarizer and Sodium orthomolybdate;
Described noble electrode is titanium net;
Described containing in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of Sodium orthomolybdate is 0.1mol/L, and the concentration of depolarizer is 0.01mol/L, and described depolarizer is nitric acid;
The aqueous hydrochloric acid of described acid solution to be concentration be 0.1mol/L;
Described cationic membrane is Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane;
The electric current of described constant-current electrolysis is 0.6A, and current density is 75mA/cm
2;
(2), electrolysis complete after, the cleaning limit, product deionized water limit that obtains in anolyte compartment is filtered, so that by Na
+and depolarizer cleans up, the filter cake control temperature obtained is 300 DEG C of dry 2h, obtains pure molybdic acid aluminium crystal.
The molybdic acid aluminium of 4010 type X-ray detection instrument to above-mentioned gained of German Brooker ALX company is adopted to measure, its EDS schemes as shown in Figure 2 a, as can be seen from Fig. 2 a, obtain in product, only having Al, Mo, O tri-kinds of elements, indicating the molybdic acid aluminium that the present invention adopts cationic membrane electrolytic process to prepare the method gained of molybdic acid aluminium is thus pure phase, inclusion-free;
Adopt the molybdic acid aluminium of D8 Advance type x-ray diffractometer to above-mentioned gained of German Brooker AXS company to measure, as shown in Figure 2 b, as can be seen from Fig. 2 b, the product obtained is Al to its XRD figure
2(MoO
4)
3.
embodiment 3
Utilize cationic membrane electrolytic process to prepare a method for molybdic acid aluminium, specifically comprise the steps:
(1), take aluminium flake as anode, take noble electrode as negative electrode, the aqueous solution of depolarizer and Sodium orthomolybdate is contained for anolyte with 95ml, with 90ml alkaline solution for catholyte, be in the two-compartment cell of barrier film at cationic membrane, adopt the mode of constant-current electrolysis, control temperature scope is the aqueous solution 10min that room temperature to 50 DEG C is carried out electrolysis and contained depolarizer and Sodium orthomolybdate;
Described noble electrode is titanium net;
Described containing in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration range of Sodium orthomolybdate is at 0.1mol/L, and the concentration of depolarizer is 0.01mol/L, and described depolarizer is SODIUMNITRATE;
The aqueous sodium hydroxide solution of described alkaline solution to be concentration be 0.1mol/L;
Described cationic membrane is Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane;
The electric current of described constant-current electrolysis is 0.6A, and current density is 75mA/cm
2;
(2), electrolysis complete after, the cleaning limit, product deionized water limit that obtains in anolyte compartment is filtered, so that by Na
+and depolarizer cleans up, the filter cake control temperature obtained is 300 DEG C of dry 2h, obtains pure molybdic acid aluminium crystal.
The molybdic acid aluminium of 4010 type X-ray detection instrument to above-mentioned gained of German Brooker ALX company is adopted to measure, its EDS schemes as shown in Figure 3 a, as can be seen from Fig. 3 a, obtain in product, only having Al, Mo, O tri-kinds of elements, indicating the molybdic acid aluminium that the present invention adopts cationic membrane electrolytic process to prepare the method gained of molybdic acid aluminium is thus pure phase, inclusion-free;
Adopt the molybdic acid aluminium of D8 Advance type x-ray diffractometer to above-mentioned gained of German Brooker AXS company to measure, as shown in Figure 3 b, as can be seen from Fig. 3 b, the product obtained is Al to its XRD figure
2(MoO
4)
3.
embodiment 4
Utilize cationic membrane electrolytic process to prepare a method for molybdic acid aluminium, specifically comprise the steps:
(1), take aluminium flake as anode, take noble electrode as negative electrode, the aqueous solution of the Sodium orthomolybdate of depolarizer is contained for anolyte with 95ml, with 90ml salts solution for catholyte, be in the two-compartment cell of barrier film at cationic membrane, adopt the mode of constant-current electrolysis, control temperature scope is the aqueous solution 10min that room temperature to 50 DEG C is carried out electrolysis and contained depolarizer and Sodium orthomolybdate;
Described noble electrode is titanium net;
Described containing in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of Sodium orthomolybdate is 0.1mol/L, and the concentration of depolarizer is 0.01mol/L, and described depolarizer is SODIUMNITRATE;
The sodium chloride aqueous solution of described salts solution to be concentration be 0.1mol/L;
Described cationic membrane is Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane;
The electric current of described constant-current electrolysis is 0.6A, and current density is 75mA/cm
2;
(2), electrolysis complete after, the cleaning limit, product deionized water limit that obtains in anolyte compartment is filtered, so that by Na
+and depolarizer cleans up, the filter cake control temperature obtained is 300 DEG C of dry 2h, obtains pure molybdic acid aluminium crystal.
The molybdic acid aluminium of 4010 type X-ray detection instrument to above-mentioned gained of German Brooker ALX company is adopted to measure, its EDS schemes as shown in fig. 4 a, as can be seen from Fig. 4 a, obtain in product, only having Al, Mo, O tri-kinds of elements, indicating the molybdic acid aluminium that the present invention adopts cationic membrane electrolytic process to prepare the method gained of molybdic acid aluminium is thus pure phase, inclusion-free;
Adopt the molybdic acid aluminium of D8 Advance type x-ray diffractometer to above-mentioned gained of German Brooker AXS company to measure, as shown in Figure 4 b, as can be seen from Fig. 4 b, the product obtained is Al to its XRD figure
2(MoO
4)
3.
In sum, a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium of the present invention, owing to adopting cationic exchange membrane electrolysis, no matter be therefore constant-potential electrolysis, or constant-current electrolysis; No matter catholyte is acid solution, alkali lye or saline solution, no matter depolarizer is nitric acid or SODIUMNITRATE, all can obtain molybdic acid aluminium, and the electrolytic preparation time is less than 0.5h, the molybdic acid aluminium of final gained is pure phase, without dephasign.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (7)
1. utilize cationic membrane electrolytic process to prepare a method for molybdic acid aluminium, it is characterized in that specifically comprising the steps:
(1), take aluminium flake as anode, take noble electrode as negative electrode, with the aqueous solution containing depolarizer and Sodium orthomolybdate for anolyte, with acid solution, alkaline solution or salts solution for catholyte, be in the two-compartment cell of barrier film at cationic membrane, adopt the mode of constant-current electrolysis or constant-potential electrolysis, control temperature scope is the aqueous solution that room temperature to 90 DEG C is carried out electrolysis and contained depolarizer and Sodium orthomolybdate, until Na
+ion all transfers to cathode compartment;
Described noble electrode is glass-carbon electrode, Graphite Electrodes, titanium net or platinum guaze;
Described containing in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of Sodium orthomolybdate is 0.005-2.5mol/L, and the concentration of depolarizer is 0.01-0.1mol/L, and wherein said depolarizer is nitric acid or SODIUMNITRATE;
Aqueous hydrochloric acid or the concentration of described acid solution to be concentration be 0.001-1mol/L are the aqueous sulfuric acid of 0.001-1mol/L;
Aqueous sodium hydroxide solution or the concentration of described alkaline solution to be concentration be 0.001-1mol/L are the potassium hydroxide aqueous solution of 0.001-1mol/L;
Sodium chloride aqueous solution or the concentration of described salts solution to be concentration be 0.001-1mol/L are the aqueous sodium carbonate of 0.001-1mol/L;
Described cationic membrane is perfluorinated sulfonic acid cationic exchange membrane;
The electric current of described constant-current electrolysis is 0.08-0.8A, and current density is 1-100mA/cm
2;
The voltage of described constant-potential electrolysis is 10-300V;
(2), electrolysis complete after, the cleaning limit, product deionized water limit that obtains in anolyte compartment filtered, the filter cake control temperature obtained is 300-400 DEG C of dry 1-4h, obtains molybdic acid aluminium.
2. a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium as claimed in claim 1, is characterized in that the noble electrode described in step (1) is titanium net;
Described contains in the aqueous solution of depolarizer and Sodium orthomolybdate, and the concentration of Sodium orthomolybdate is 0.01-0.5mol/L;
The aqueous hydrochloric acid of described acid solution to be concentration be 0.001-1mol/L;
The aqueous sodium hydroxide solution of described alkaline solution to be concentration be 0.001-1mol/L;
The sodium chloride aqueous solution of described salts solution to be concentration be 0.001-1mol/L;
Described cationic membrane is the Nafion perfluorinated sulfonic acid 212 type cationic exchange membrane that du pont company produces;
In constant-current electrolysis or constant-potential electrolysis process, control temperature scope is room temperature to 50 DEG C;
The electric current of described constant-current electrolysis is 0.4-0.8A, and current density is 50-100mA/cm
2;
The voltage of described constant-potential electrolysis is 20-100V.
3. a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium as claimed in claim 2, is characterized in that the concentration of Sodium orthomolybdate is 0.1mol/L containing in the aqueous solution of depolarizer and Sodium orthomolybdate described in step (1);
The filter cake control temperature that step (2) obtains after filtering is 300-400 DEG C of dry 2h.
4. a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium as claimed in claim 3, it is characterized in that containing described in step (1) in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of depolarizer is 0.01mol/L, and described depolarizer is nitric acid;
Take acid solution as catholyte, the aqueous hydrochloric acid of described acid solution to be concentration be 0.1mol/L;
Adopt the mode of constant-potential electrolysis to carry out electrolysis, the voltage of constant-potential electrolysis is 20V.
5. a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium as claimed in claim 3, it is characterized in that containing described in step (1) in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of depolarizer is 0.01mol/L, and described depolarizer is nitric acid;
Take acid solution as catholyte, the aqueous hydrochloric acid of described acid solution to be concentration be 0.1mol/L;
Adopt the mode of constant-current electrolysis to carry out electrolysis, the current density of constant-current electrolysis is 75mA/cm
2, electric current is 0.6A.
6. a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium as claimed in claim 3, it is characterized in that containing described in step (1) in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of depolarizer is 0.01mol/L, and described depolarizer is SODIUMNITRATE;
Take alkaline solution as catholyte, the aqueous sodium hydroxide solution of described alkaline solution to be concentration be 0.1mol/L;
Adopt the mode of constant-current electrolysis to carry out electrolysis, the current density of constant-current electrolysis is 75mA/cm
2, electric current is 0.6A.
7. a kind of method utilizing cationic membrane electrolytic process to prepare molybdic acid aluminium as claimed in claim 3, it is characterized in that containing described in step (1) in the aqueous solution of depolarizer and Sodium orthomolybdate, the concentration of depolarizer is 0.01mol/L, and described depolarizer is SODIUMNITRATE;
Take salts solution as catholyte, the sodium-chlor of described salts solution to be concentration be 0.1mol/L;
Adopt the mode of constant-current electrolysis to carry out electrolysis, the current density of constant-current electrolysis is 75mA/cm
2, electric current is 0.6A.
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| CN105355899A (en) * | 2015-11-10 | 2016-02-24 | 上海应用技术学院 | Preparation method for molybdenum dioxide-active carbon composite material |
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| CN106367773A (en) * | 2016-09-23 | 2017-02-01 | 上海应用技术大学 | Preparation method of vanadic acid copper |
| CN106367772A (en) * | 2016-09-23 | 2017-02-01 | 上海应用技术大学 | Preparation method of 3D flower-like spherical zinc vanadium oxide hydroxide hydrate photocatalyst |
| CN106367773B (en) * | 2016-09-23 | 2018-08-17 | 上海应用技术大学 | A kind of preparation method of copper vanadate |
| CN106367772B (en) * | 2016-09-23 | 2018-08-24 | 上海应用技术大学 | A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst |
| CN106191903B (en) * | 2016-09-23 | 2018-12-04 | 上海应用技术大学 | A kind of preparation method of silver vanadate photochemical catalyst |
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