CN104445411A - Preparation method of large granular molybdic acid - Google Patents
Preparation method of large granular molybdic acid Download PDFInfo
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- CN104445411A CN104445411A CN201410811547.XA CN201410811547A CN104445411A CN 104445411 A CN104445411 A CN 104445411A CN 201410811547 A CN201410811547 A CN 201410811547A CN 104445411 A CN104445411 A CN 104445411A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a preparation method of large granular molybdic acid. The preparation method comprises the following steps: 1, adding sodium carbonate into commercial molybdenum oxide washing wastewater while stirring, performing heat preservation stirring reaction, and then filtering to obtain a filtrate and filter residues; 2, mixing oxydol, a sodium carbonate liquid and the filter residues, boiling, standing to cool the materials after boiling to room temperature, and then filtering to obtain alkaline leaching residues and an alkaline leaching liquid; and 3, performing acid precipitation on the filtrate by using nitric acid, filtering to obtain an acid precipitation mother liquid and a filter cake, drying the filter cake, and sieving the filter cake to obtain molybdic acid of which the Fisher particle size is 20-50 microns and the loose density is 1.2-1.5g/cm<3>. According to the preparation method disclosed by the invention, the commercial molybdenum oxide washing wastewater is adopted as a raw material, the sodium carbonate liquid is used for precipitating foreign ions in the commercial molybdenum oxide washing wastewater and can be used for dissolving tiny molybdic acid in the commercial molybdenum oxide washing wastewater at the same time, and molybdic acid ions in the nitric acid acid-precipitation filtrate are adopted to crystallize and grow up at a high temperature to generate large granular molybdic acid.
Description
Technical field
The invention belongs to molybdic acid preparing technical field, be specifically related to a kind of preparation method of macrobead molybdic acid.
Background technology
Molybdic acid, outward appearance is white or light yellow crystalline powder.Technical pure molybdic acid is mainly used as the raw material manufacturing molybdenum class catalyzer and molybdenum salt.For developer, precipitation agent, Metal plating tinting material, the blue pigments of ceramic glaze, oil painting and moist colours, coating etc.For measuring phosphorus, phosphoric acid salt, silicate, lead, aluminium etc.At medicine, electronic industry, analytical chemistry, there is widespread use.Conventional production methods mainly contains:
1, molybdenum glance is crushed to 60 ~ 80 orders, oxidizing roasting 6h ~ 8h is carried out in 500 DEG C ~ 550 DEG C in stoving oven, leach with ammoniacal liquor, obtain ammonium molybdate solution, after purification removing impurity, heavy with nitric acid acid, separate out precipitate molybdic acid, with warm water washing, centrifuge dehydration, drying, pulverizing, obtain molybdic acid finished product.The method adopts the heavy technique of ammonium molybdate acid, has acid ion to be mixed into unavoidably and causes product contamination, and easily produce ammonia nitrogen waste water in production process in the fine-grain precipitate molybdic acid thing of generation.
2, by molybdic oxide MoO
3hydrochloric acid soln 40 DEG C ~ 60 DEG C heating, molybdic acid H
2moO
4.The method needs to prepare MoO
3hydrochloric acid soln, operation is numerous and diverse, and the molybdic acid formed is comparatively thin, sad filter.
3, ammonium molybdate solution content being about 15% is added to (relative density 1.16) in the salpeter solution of same volume, add a certain amount of ammonium nitrate and a small amount of molybdic acid crystal (as crystal seed) again, after stirring, leave standstill to crystallization complete, filter the washing of gained precipitation frozen water to qualified, dry after suction filtration, be anhydrous molybdic acid.Although the molybdic acid that the method is formed is containing assorted lower, crystal be mingled with liquid containing nitrate radical and ammonium root higher, be restricted in catalyst field application.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind of preparation method of macrobead molybdic acid.The method adopts molybdenum calcining washing waste water to be raw material, add sodium carbonate solution wherein, sodium carbonate solution is utilized to precipitate the foreign ions such as copper, iron, calcium and magnesium in molybdenum calcining washing waste water, sodium carbonate solution can dissolve molybdic acid tiny in molybdenum calcining washing waste water simultaneously, after making filtration, filtrate is limpid, then adopt the molybdic acid ion in the heavy filtrate of nitric acid acid, at high temperature crystal growth generates macrobead molybdic acid.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of macrobead molybdic acid, is characterized in that, comprise the following steps:
Step one, under the agitation condition of 60 DEG C ~ 80 DEG C, in molybdenum calcining washing waste water, add sodium carbonate to the pH value of molybdenum calcining washing waste water is 5.5 ~ 6.5, filters, obtain filtrate and filter residue after insulated and stirred reaction 10min ~ 45min;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 0.5% ~ 2.0% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain alkali leaching slag and alkali immersion liquid, alkali immersion liquid is returned in step one sodium carbonate replaced in step one; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:(0.05 ~ 0.2): (2.5 ~ 4.0); The mass concentration of described hydrogen peroxide is 27% ~ 40%;
Step 3, employing nitric acid carry out acid to filtrate described in step one and sink, the temperature that acid is sunk is 75 DEG C ~ 95 DEG C, the pH value of filtrate is kept to be 0.5 ~ 1.0 in the heavy process of acid, filter after reaction 10min ~ 45min, obtain the heavy mother liquor of acid and filter cake, screening after being dried by described filter cake, obtaining Fisher particle size is 20 μm ~ 50 μm, and pine is than being 1.2g/cm
3~ 1.5g/cm
3macrobead molybdic acid.
The preparation method of above-mentioned a kind of macrobead molybdic acid, is characterized in that, the mass percent concentration of nitric acid described in step 3 is 40% ~ 60%.
The preparation method of above-mentioned a kind of macrobead molybdic acid, is characterized in that, keeps the pH value of filtrate to be 0.5 ~ 0.7 in step 3 in the heavy process of acid.
The preparation method of above-mentioned a kind of macrobead molybdic acid, is characterized in that, keeps the pH value of filtrate to be 0.6 in the heavy process of acid.
The preparation method of above-mentioned a kind of macrobead molybdic acid, is characterized in that, the temperature that described in step 3, acid is heavy is 80 DEG C ~ 90 DEG C.
The preparation method of above-mentioned a kind of macrobead molybdic acid, is characterized in that, the temperature that described acid is sunk is 85 DEG C.
The preparation method of above-mentioned a kind of macrobead molybdic acid, is characterized in that, the screen cloth sieving employing described in step 3 is 40 eye mesh screens.
The present invention compared with prior art has the following advantages:
1, the inventive method is unique, simple to operate and molybdenum utilization ratio is high.
2, the present invention adopts molybdenum calcining washing waste water to be raw material, add sodium carbonate solution wherein, sodium carbonate solution is utilized to precipitate the foreign ions such as copper, iron, calcium and magnesium in molybdenum calcining washing waste water, sodium carbonate solution can dissolve molybdic acid tiny in molybdenum calcining washing waste water simultaneously, after making filtration, filtrate is limpid, then adopt the molybdic acid ion in the heavy filtrate of nitric acid acid, at high temperature crystal growth generates macrobead molybdic acid.
The Fisher particle size of the molybdic acid 3, adopting method of the present invention to prepare is 20 μm ~ 50 μm, and pine is than being 1.2g/cm
3~ 1.5g/cm
3.
Below in conjunction with drawings and Examples, technical solution of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of molybdic acid prepared by the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of the molybdic acid of the heavy preparation of the direct acid of ammonium molybdate solution.
Fig. 3 is the scanning electron microscope (SEM) photograph that ammonium molybdate solution adds the molybdic acid of ammonium nitrate and the heavy preparation of molybdic acid crystal seed acid.
Fig. 4 is the scanning electron microscope (SEM) photograph that molybdic oxide hydrochloric acid soln adds the molybdic acid of hot preparation.
Embodiment
Embodiment 1
The present embodiment comprises the following steps:
Step one, under the agitation condition of 70 DEG C, in molybdenum calcining washing waste water, add sodium carbonate to the pH value of molybdenum calcining washing waste water is 6.5, filters, obtain filtrate and filter residue after insulated and stirred reaction 10min; In described molybdenum calcining washing waste water, the concentration of primary metal ion is: molybdenum 35g/L, copper 0.96g/L, iron 0.029g/L, potassium 0.68g/L, sodium 0.027g/L, calcium 0.026g/L, magnesium 0.03g/L; Containing molybdenum 24.63wt%, the insoluble molybdenum 1.26wt% of alkali in described filter residue; In described filtrate, the concentration of primary metal ion is: molybdenum 34.48g/L, copper 0.002g/L, iron 0.0078g/L, potassium 0.25g/L, sodium 1.06/L, calcium 0.076g/L, magnesium 0.243g/L;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 1.5% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain molybdenum content be less than the alkali leaching slag of 1wt% and contain molybdenum 15.4g/L, pH value is the alkali immersion liquid of 12.5; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:0.1:3.0; The mass concentration of described hydrogen peroxide is 32%;
The nitric acid that step 3, employing mass percent concentration are 40% carries out acid to filtrate described in step one and sinks, the temperature that acid is sunk is 85 DEG C, the pH value of filtrate is kept to be 0.6 in the heavy process of acid, filter after reaction 25min, obtain the heavy mother liquor of acid and filter cake, with 40 eye mesh screen screenings after being dried by described filter cake, obtaining Fisher particle size is 50 μm, and pine is than being 1.2g/cm
3macrobead molybdic acid.
The chemical index (wt%) of macrobead molybdic acid prepared by the present embodiment is: molybdenum 60.2%, copper 0.0001%, iron 0.029%, potassium 0.25%, sodium 0.23%, calcium 0.075%, magnesium 0.019%.The acid of the present embodiment is sunk primary metal ion concentration in mother liquor and is: molybdenum 0.91g/L, copper 0.0002g/L, iron 0.033g/L, potassium 0.16g/L, sodium 1.11g/L, calcium 0.056g/L, magnesium 0.015g/L.
Fig. 1 is the scanning electron microscope (SEM) photograph of molybdic acid prepared by the present embodiment, and magnification is 3000 times, and as can be seen from the figure, molybdic acid granularity prepared by the present embodiment is six prisms, octahedra shape, and size is homogeneous, and interface is clear, is uniformly dispersed.Fig. 2 is the first traditional method in background technology---the scanning electron microscope (SEM) photograph of the direct molybdic acid of the heavy preparation of acid of ammonium molybdate solution, under 3000 times of mirror images, crystal is tiny, reunites, interface is fuzzy.Fig. 3 is that the second traditional method in background technology---molybdic oxide hydrochloric acid soln adds the scanning electron microscope (SEM) photograph of the molybdic acid of hot preparation, and under 3000 times of mirror images, crystal diameter is little, more elongated, but interfacial phase is to clear.Fig. 4 is the third traditional method in background technology---ammonium molybdate solution adds the scanning electron microscope (SEM) photograph of the molybdic acid of ammonium nitrate and the heavy preparation of molybdic acid crystal seed acid, and under 3000 times of mirror images, crystal comparatively Fig. 2 is grown up to some extent, interface is more clear, have six prisms, octahedra crystal formation occurs, but crystal is little.As can be seen from the contrast of four figure, the molybdic acid size adopting method of the present invention to prepare is homogeneous, and interface is clear, is uniformly dispersed, and is significantly better than molybdic acid prepared by existing method.
Embodiment 2
The present embodiment comprises the following steps:
Step one, under the agitation condition of 60 DEG C, the alkali immersion liquid adding embodiment 1 in molybdenum calcining washing waste water is 6.0 to the pH value of molybdenum calcining washing waste water, filters, obtain filtrate and filter residue after insulated and stirred reaction 30min; In described molybdenum calcining washing waste water, the concentration of primary metal ion is: molybdenum 24.29g/L, copper 0.5g/L, iron 0.74g/L, potassium 0.8g/L, sodium 0.028g/L, calcium 0.21g/L, magnesium 0.35g/L; Containing molybdenum 25.99wt%, the insoluble molybdenum 1.34wt% of alkali in described filter residue; In described filtrate, the concentration of primary metal ion is: molybdenum 23.48g/L, copper 0.006g/L, iron 0.0098g/L, potassium 0.26g/L, sodium 0.36/L, calcium 0.086g/L, magnesium 0.333g/L;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 0.5% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain molybdenum content be less than the alkali leaching slag of 1wt% and contain molybdenum 10.2g/L, pH value is the alkali immersion liquid of 13.8; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:0.05:4.0; The mass concentration of described hydrogen peroxide is 27%;
The nitric acid that step 3, employing mass percent concentration are 60% carries out acid to filtrate described in step one and sinks, the temperature that acid is sunk is 75 DEG C, the pH value of filtrate is kept to be 0.5 in the heavy process of acid, filter after reaction 10min, obtain the heavy mother liquor of acid and filter cake, with 40 eye mesh screen screenings after being dried by described filter cake, obtaining Fisher particle size is 20 μm, and pine is than being 1.5g/cm
3macrobead molybdic acid.
The chemical index (wt%) of macrobead molybdic acid prepared by the present embodiment is: molybdenum 59.2%, copper 0.016%, iron 0.055%, potassium 0.29%, sodium 0.18%, calcium 0.065%, magnesium 0.018%.The acid of the present embodiment is sunk primary metal ion concentration in mother liquor and is: molybdenum 0.93g/L, copper 0.002g/L, iron 0.023g/L, potassium 0.16g/L, sodium 0.11g/L, calcium 0.086g/L, magnesium 0.014g/L.
Embodiment 3
The present embodiment comprises the following steps:
Step one, under the agitation condition of 80 DEG C, the alkali immersion liquid adding embodiment 2 in molybdenum calcining washing waste water is 5.5 to the pH value of molybdenum calcining washing waste water, filters, obtain filtrate and filter residue after insulated and stirred reaction 45min; In described molybdenum calcining washing waste water, the concentration of primary metal ion is: molybdenum 37.63g/L, copper 0.6g/L, iron 2.08mg/L, potassium 0.20g/L, sodium 0.052mg/L, calcium 0.46mg/L; Containing molybdenum 22.51wt%, the insoluble molybdenum 1.04wt% of alkali in described filter residue; In described filtrate, the concentration of primary metal ion is: molybdenum 36.38g/L, copper 0.0002g/L, iron 0.0048g/L, potassium 0.23g/L, sodium 2.06/L, calcium 0.046g/L, magnesium 0.193g/L;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 2.0% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain molybdenum content be less than the alkali leaching slag of 1wt% and contain molybdenum 17.4g/L, pH value is the alkali immersion liquid of 14.0; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:0.2:2.5; The mass concentration of described hydrogen peroxide is 40%;
The nitric acid that step 3, employing mass percent concentration are 50% carries out acid to filtrate described in step one and sinks, the temperature that acid is sunk is 95 DEG C, the pH value of filtrate is kept to be 1.0 in the heavy process of acid, filter after reaction 45min, obtain the heavy mother liquor of acid and filter cake, with 40 eye mesh screen screenings after being dried by described filter cake, obtaining Fisher particle size is 30 μm, and pine is than being 1.4g/cm
3macrobead molybdic acid.
The chemical index (wt%) of macrobead molybdic acid prepared by the present embodiment is: molybdenum 60.5%, copper 0.0001%, iron 0.0029%, potassium 0.18%, sodium 0.23%, calcium 0.085%, magnesium 0.013%.The acid of the present embodiment is sunk primary metal ion concentration in mother liquor and is: molybdenum 0.79g/L, copper 0.0002g/L, iron 0.043g/L, potassium 0.17g/L, sodium 2.01g/L, calcium 0.047g/L, magnesium 0.012g/L.
Embodiment 4
The present embodiment comprises the following steps:
Step one, under the agitation condition of 65 DEG C, the alkali immersion liquid adding embodiment 3 in molybdenum calcining washing waste water is 6.0 to the pH value of molybdenum calcining washing waste water, filters, obtain filtrate and filter residue after insulated and stirred reaction 20min; In described molybdenum calcining washing waste water, the concentration of primary metal ion is: molybdenum 57.43g/L, copper 0.42g/L, iron 2.23mg/L, potassium 0.18g/L, sodium 0.062mg/L, calcium 0.43mg/L; Containing molybdenum 27.61wt%, the insoluble molybdenum 1.12wt% of alkali in described filter residue; In described filtrate, the concentration of primary metal ion is: molybdenum 56.17g/L, copper 0.0001g/L, iron 0.0053g/L, potassium 0.24g/L, sodium 2.16/L, calcium 0.052g/L, magnesium 0.174g/L;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 1.0% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain molybdenum content be less than the alkali leaching slag of 1wt% and contain molybdenum 21.2g/L, pH value is the alkali immersion liquid of 14; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:0.05:2.5; The mass concentration of described hydrogen peroxide is 30%;
The nitric acid that step 3, employing mass percent concentration are 40% carries out acid to filtrate described in step one and sinks, the temperature that acid is sunk is 80 DEG C, the pH value of filtrate is kept to be 0.7 in the heavy process of acid, filter after reaction 30min, obtain the heavy mother liquor of acid and filter cake, with 40 eye mesh screen screenings after being dried by described filter cake, obtaining Fisher particle size is 40 μm, and pine is than being 1.2g/cm
3macrobead molybdic acid.
The chemical index (wt%) of macrobead molybdic acid prepared by the present embodiment is: molybdenum 60.2%, copper 0.0001%, iron 0.0019%, potassium 0.17%, sodium 0.22%, calcium 0.075%, magnesium 0.010%.The acid of the present embodiment is sunk primary metal ion concentration in mother liquor and is: molybdenum 0.92g/L, copper 0.0003g/L, iron 0.053g/L, potassium 0.16g/L, sodium 2.31g/L, calcium 0.057g/L, magnesium 0.013g/L.
Embodiment 5
The present embodiment comprises the following steps:
Step one, under the agitation condition of 75 DEG C, the alkali immersion liquid adding embodiment 4 in molybdenum calcining washing waste water is 6.5 to the pH value of molybdenum calcining washing waste water, filters, obtain filtrate and filter residue after insulated and stirred reaction 40min; In described molybdenum calcining washing waste water, the concentration of primary metal ion is: molybdenum 45g/L, copper 1.06g/L, iron 0.032g/L, potassium 0.73g/L, sodium 0.031g/L, calcium 0.023g/L, magnesium 0.023g/L; Containing molybdenum 26.41wt%, the insoluble molybdenum 1.04wt% of alkali in described filter residue; In described filtrate, the concentration of primary metal ion is: molybdenum 44.36g/L, copper 0.001g/L, iron 0.0068g/L, potassium 0.24g/L, sodium 1.26/L, calcium 0.069g/L, magnesium 0.198g/L;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 1.0% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain molybdenum content be less than the alkali leaching slag of 1wt% and contain molybdenum 18.5g/L, pH value is the alkali immersion liquid of 10; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:0.2:4.0; The mass concentration of described hydrogen peroxide is 27%;
The nitric acid that step 3, employing mass percent concentration are 50% carries out acid to filtrate described in step one and sinks, the temperature that acid is sunk is 90 DEG C, the pH value of filtrate is kept to be 0.5 in the heavy process of acid, filter after reaction 20min, obtain the heavy mother liquor of acid and filter cake, with 40 eye mesh screen screenings after being dried by described filter cake, obtaining Fisher particle size is 30 μm, and pine is than being 1.3g/cm
3macrobead molybdic acid.
The chemical index (wt%) of macrobead molybdic acid prepared by the present embodiment is: molybdenum 60.2%, copper 0.006%, iron 0.015%, potassium 0.24%, sodium 0.15%, calcium 0.063%, magnesium 0.021%.The acid of the present embodiment is sunk primary metal ion concentration in mother liquor and is: molybdenum 0.53g/L, copper 0.002g/L, iron 0.033g/L, potassium 0.21g/L, sodium 0.14g/L, calcium 0.068g/L, magnesium 0.031g/L.
The above; it is only preferred embodiment of the present invention; not any restriction is done to the present invention, every above embodiment is done according to invention technical spirit any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (7)
1. a preparation method for macrobead molybdic acid, is characterized in that, comprises the following steps:
Step one, under the agitation condition of 60 DEG C ~ 80 DEG C, in molybdenum calcining washing waste water, add sodium carbonate to the pH value of molybdenum calcining washing waste water is 5.5 ~ 6.5, filters, obtain filtrate and filter residue after insulated and stirred reaction 10min ~ 45min;
Boil after filter residue mixing described in step 2, the sodium carbonate solution that is 0.5% ~ 2.0% by hydrogen peroxide, mass concentration and step one, then the material after boiling is left standstill after being cooled to room temperature and filter, obtain alkali leaching slag and alkali immersion liquid, alkali immersion liquid is returned in step one sodium carbonate replaced in step one; The mass ratio of described filter residue, hydrogen peroxide and sodium carbonate solution is 1:(0.05 ~ 0.2): (2.5 ~ 4.0); The mass concentration of described hydrogen peroxide is 27% ~ 40%;
Step 3, employing nitric acid carry out acid to filtrate described in step one and sink, the temperature that acid is sunk is 75 DEG C ~ 95 DEG C, the pH value of filtrate is kept to be 0.5 ~ 1.0 in the heavy process of acid, filter after reaction 10min ~ 45min, obtain the heavy mother liquor of acid and filter cake, screening after being dried by described filter cake, obtaining Fisher particle size is 20 μm ~ 50 μm, and pine is than being 1.2g/cm
3~ 1.5g/cm
3macrobead molybdic acid.
2. the preparation method of a kind of macrobead molybdic acid according to claim 1, is characterized in that, the mass percent concentration of nitric acid described in step 3 is 40% ~ 60%.
3. the preparation method of a kind of macrobead molybdic acid according to claim 1, is characterized in that, keeps the pH value of filtrate to be 0.5 ~ 0.7 in step 3 in the heavy process of acid.
4. the preparation method of a kind of macrobead molybdic acid according to claim 3, is characterized in that, keeps the pH value of filtrate to be 0.6 in the heavy process of acid.
5. the preparation method of a kind of macrobead molybdic acid according to claim 1, is characterized in that, the temperature that described in step 3, acid is heavy is 80 DEG C ~ 90 DEG C.
6. the preparation method of a kind of macrobead molybdic acid according to claim 5, is characterized in that, the temperature that described acid is sunk is 85 DEG C.
7. the preparation method of a kind of macrobead molybdic acid according to claim 1, is characterized in that, the screen cloth sieving employing described in step 3 is 40 eye mesh screens.
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