CN107043129A - A kind of preparation method of ammonium dimolybdate - Google Patents

A kind of preparation method of ammonium dimolybdate Download PDF

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CN107043129A
CN107043129A CN201710422587.9A CN201710422587A CN107043129A CN 107043129 A CN107043129 A CN 107043129A CN 201710422587 A CN201710422587 A CN 201710422587A CN 107043129 A CN107043129 A CN 107043129A
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ammonium
source
carbonate
product
preparation
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CN107043129B (en
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周秋生
杨利群
李小斌
彭志宏
刘桂华
齐天贵
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Central South University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00Compounds of molybdenum
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention provides a kind of preparation method of ammonium dimolybdate:Molybdenum source and source of ammonium are subjected to metathesis reaction, ammonium dimolybdate is obtained.The present invention is using ammonium tetramolybdate and/or molybdic acid as molybdenum source, using one or more of as source of ammonium in ammoniacal liquor, ammonium hydrogen carbonate and ammonium carbonate, without adding substantial amounts of solvent and water, environmental protection and saving.From the result of embodiment, the preparation method that the application is provided can be successfully obtained ammonium dimolybdate, and the equal > 99% of its purity.

Description

A kind of preparation method of ammonium dimolybdate
Technical field
The present invention relates to ammonium molybdate technical field, more particularly to a kind of preparation method of ammonium dimolybdate.
Background technology
Ammonium dimolybdate is a kind of conventional ammonium molybdate, and molecular formula is (NH4)2Mo2O7.At present, ammonium dimolybdate is widely used In the raw material of dyestuff, pigment, catalyst, fireproof agent, trace-element fertilizer, ceramic pigment and the other compounds of synthesis.
At present, the method for production ammonium dimolybdate is generally required for being reacted in aqueous in the prior art, through peracid The series of processes such as heavy, the molten, evaporative crystallization of ammonia obtain target product.However, the use of a large amount of water not only results in water resource Shortage, production terminates rear ammonia-containing water and directly outer can not arranged, can only evaporative crystallization, cause higher energy expenditure;And two molybdenums Sour ammonium product purity control is difficult, and impurity is easy to be mixed into wherein.
The content of the invention
It is an object of the invention to provide a kind of method that ammonium dimolybdate is prepared in the case of without a large amount of water, this hair The method flow of bright offer is short, energy consumption is low, pollution is low, cost is low and easy to operate.
In order to realize foregoing invention purpose, the present invention provides following technical scheme:
The invention provides a kind of preparation method of ammonium dimolybdate, comprise the following steps:
Molybdenum source and source of ammonium are subjected to metathesis reaction, ammonium dimolybdate is obtained;
The molybdenum source is ammonium tetramolybdate and/or molybdic acid;
The source of ammonium is the one or more in ammoniacal liquor, ammonium hydrogen carbonate and ammonium carbonate.
It is preferred that, the mol ratio of the molybdenum source and source of ammonium is (0.8~2.5):(0.8~2.5).
It is preferred that, the mol ratio of the ammonium tetramolybdate and ammonium hydrogen carbonate is 1:(1.5~2.5).
It is preferred that, the mol ratio of the ammonium tetramolybdate and ammonium carbonate is 1:(0.8~1.5).
It is preferred that, the mol ratio of the ammonium tetramolybdate and ammoniacal liquor is 1:(1.5~2.5).
It is preferred that, the mol ratio of the molybdic acid and ammonium hydrogen carbonate is 1:(0.8~1.5).
It is preferred that, the mol ratio of the molybdic acid and ammonium carbonate is (1.8~2.5):1.
It is preferred that, NH in the molybdic acid and ammoniacal liquor3·H2O mol ratio is 1:(0.8~1.5).
It is preferred that, the temperature of the metathesis reaction is 60~90 DEG C;
The time of the metathesis reaction is 0.5~3h.
It is preferred that, the pressure of the metathesis reaction is 0.1~0.15MPa.
The invention provides a kind of preparation method of ammonium dimolybdate:Molybdenum source and source of ammonium are subjected to metathesis reaction, two are obtained Ammonium molybdate.The present invention is using ammonium tetramolybdate and/or molybdic acid as molybdenum source, with one kind in ammoniacal liquor, ammonium hydrogen carbonate and ammonium carbonate or several Plant as source of ammonium, without adding substantial amounts of solvent and water, environmental protection and saving.From the result of embodiment, what the application was provided Preparation method can be successfully obtained ammonium dimolybdate, and the equal > 99% of its purity.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram for the ammonium dimolybdate that embodiment 1 is obtained.
Embodiment
The invention provides a kind of preparation method of ammonium dimolybdate, comprise the following steps:
Molybdenum source and source of ammonium are subjected to metathesis reaction, ammonium dimolybdate is obtained;
The molybdenum source is ammonium tetramolybdate and/or molybdic acid;
The source of ammonium is the one or more in ammoniacal liquor, ammonium hydrogen carbonate and ammonium carbonate.
Molybdenum source and source of ammonium are carried out metathesis reaction by the present invention, obtain ammonium dimolybdate.In the present invention, the molybdenum source is four Ammonium molybdate and/or molybdic acid;The source of ammonium is the one or more in ammoniacal liquor, ammonium hydrogen carbonate and ammonium carbonate.The present invention is to the molybdenum Source and the source of source of ammonium are using commercially available molybdenum source well-known to those skilled in the art and source of ammonium without any particular/special requirement Can, specifically ammonium tetramolybdate can be two commercially available hydration ammonium tetramolybdates as described.The present invention does not have any to the ammoniacal liquor Particular/special requirement, using the ammoniacal liquor of commercial concentration well-known to those skilled in the art, preferably 25~28wt%.
In the present invention, the mol ratio of the molybdenum source and source of ammonium is preferably (0.8~2.5):(0.8~2.5), more preferably (1~2):(1~2).
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, and the source of ammonium is ammonium hydrogen carbonate, described four The mol ratio of ammonium molybdate and ammonium hydrogen carbonate is preferably 1:(1.5~2.5), more preferably 1:(1.9~2.3), most preferably 1:2. In the present invention, the equation of ammonium tetramolybdate and the ammonium hydrogen carbonate reaction is specifically:
(NH4)2Mo4O13+2NH4HCO3=2 (NH4)2Mo2O7+2CO2↑+H2O。
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, and the source of ammonium is ammonium carbonate, four molybdenum The mol ratio of sour ammonium and ammonium carbonate is preferably 1:(0.8~1.5), more preferably 1:(0.9~1.3), most preferably 1:1.At this In invention, the equation of ammonium tetramolybdate and the ammonium carbonate reaction is specifically:
(NH4)2Mo4O13+(NH4)2CO3=2 (NH4)2Mo2O7+CO2↑。
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, and the source of ammonium is ammoniacal liquor, four molybdic acid NH in ammonium and ammoniacal liquor3·H2O mol ratio is preferably 1:(1.5~2.5), more preferably 1:(1.9~2.3), most preferably 1:2. In the present invention, the equation of ammonium tetramolybdate and the ammoniacal liquor reaction is specifically:
(NH4)2Mo4O13+2NH3·H2O=2 (NH4)2Mo2O7+H2O。
In the specific embodiment of the invention, when the molybdenum source be molybdic acid, the source of ammonium be ammonium hydrogen carbonate when, the molybdic acid and The mol ratio of ammonium hydrogen carbonate is preferably 1:(0.8~1.5), more preferably 1:(0.9~1.3), most preferably 1:1.In the present invention In, the equation of molybdic acid and the ammonium hydrogen carbonate reaction is specifically:
2H2MoO4+2NH4HCO3=(NH4)2Mo2O7+2CO2↑+3H2O。
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, and the source of ammonium is ammonium carbonate, the molybdic acid and carbon The mol ratio of sour ammonium is preferably (1.8~2.5):1, more preferably (1.9~2.3):1, most preferably 2:1.In the present invention, institute State molybdic acid and ammonium carbonate reaction equation be specifically:
2H2MoO4+(NH4)2CO3=(NH4)2Mo2O7+CO2↑+2H2O。
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, and the source of ammonium is ammoniacal liquor, the molybdic acid and ammoniacal liquor Middle NH3·H2O mol ratio is preferably 1:(0.8~1.5), more preferably 1:(0.9~1.3), most preferably 1:1.In the present invention In, the equation of molybdic acid and the ammoniacal liquor reaction is specifically:
2H2MoO4+2NH3·H2O=(NH4)2Mo2O7+3H2O。
In the present invention, when the mixture that the molybdenum source is ammonium tetramolybdate and molybdic acid, the source of ammonium is ammoniacal liquor, ammonium hydrogen carbonate During with two or three in ammonium carbonate, the metathesis reaction is actually that the recombination reaction that carries out of above-mentioned each independent raw material is same Shi Jinhang, is no longer repeated herein.
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, the source of ammonium is ammonium carbonate and ammonium hydrogen carbonate Mixture when, ammonium tetramolybdate and ammonium carbonate, the mol ratio of ammonium hydrogen carbonate are preferably 1:(0.4~0.75):(0.75~1.25), More preferably 1:(0.5~0.6):(0.9~1.1).
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, the source of ammonium is the mixed of ammonium carbonate and ammoniacal liquor During compound, NH in the ammonium tetramolybdate and ammonium carbonate, ammoniacal liquor3·H2O mol ratio is preferably 1:(0.4~0.75):(0.75~ 1.25), more preferably 1:(0.5~0.6):(0.9~1.1).
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, the source of ammonium is ammonium hydrogen carbonate and ammoniacal liquor During mixture, NH in the ammonium tetramolybdate and ammonium hydrogen carbonate, ammoniacal liquor3·H2O mol ratio is preferably 1:(0.4~0.75): (0.75~1.25), more preferably 1:(0.5~0.6):(0.9~1.1).
In the specific embodiment of the invention, when the molybdenum source be ammonium tetramolybdate, the source of ammonium be ammonium carbonate, ammonium hydrogen carbonate and During the mixture of ammoniacal liquor, NH in the ammonium tetramolybdate and ammonium carbonate, ammonium hydrogen carbonate, ammoniacal liquor3·H2O mol ratio is preferably 1: (0.27~0.5):(1~1.6):(1~1.6), more preferably 1:(0.3~0.4):(1.2~1.4):(1.2~1.4).
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, the source of ammonium is the mixed of ammonium carbonate and ammonium hydrogen carbonate During compound, the molybdic acid and ammonium carbonate, the mol ratio of ammonium hydrogen carbonate are preferably 1:(0.1~0.35):(0.4~0.74), it is more excellent Elect 1 as:(0.2~0.3):(0.5~0.6).
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, the source of ammonium is the mixture of ammonium carbonate and ammoniacal liquor When, NH in the molybdic acid and ammonium carbonate, ammoniacal liquor3·H2O mol ratio is preferably 1:(0.1~0.35):(0.4~0.74), it is more excellent Elect 1 as:(0.2~0.3):(0.5~0.6).
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, the source of ammonium is the mixing of ammonium hydrogen carbonate and ammoniacal liquor During thing, NH in the molybdic acid and ammonium hydrogen carbonate, ammoniacal liquor3·H2O mol ratio is preferably 1:(0.4~0.75):(0.4~0.75), More preferably 1:(0.5~0.6):(0.5~0.6).
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, the source of ammonium is ammonium carbonate, ammonium hydrogen carbonate and ammoniacal liquor Mixture when, NH in the molybdic acid and ammonium carbonate, ammonium hydrogen carbonate, ammoniacal liquor3·H2O mol ratio is preferably 1:(0.1~0.6): (0.5~1.2):(0.5~1.2), more preferably 1:(0.2~0.4):(0.7~1.0):(0.7~0.9).
In the present invention, the metathesis reaction is carried out preferably in closed container;The pressure of the metathesis reaction is excellent Elect 0.1~0.15MPa, most preferably more preferably 0.11~0.14MPa, 0.12~0.13MPa as;The metathesis reaction Temperature is preferably 60~90 DEG C, more preferably 70~80 DEG C, most preferably 75 DEG C;The time of the metathesis reaction is preferably 0.5~3h, more preferably 1~2.5h, most preferably 1.5~2h.
Processing is dried in the product system that metathesis reaction described in preferred pair of the present invention is obtained, and obtains two pure molybdic acids Ammonium.In the present invention, the temperature of the drying process is preferably 50~70 DEG C, more preferably 55~65 DEG C, most preferably 60 DEG C; The time of the drying process is preferably 5~7h, more preferably 6h.
The CO that metathesis reaction process described in preferred pair of the present invention is generated2Gas is recycled.Of the invention specific In embodiment, present invention preferably uses alkaline absorption solution to CO2Gas is absorbed;The alkaline absorption solution be preferably ammoniacal liquor or Sal volatile, CO2It is anti-that gas is used for double decomposition with obtaining neutralization reaction solution after alkaline absorption solution reaction, further after processing The raw material answered.The present invention does not have any particular/special requirement to the concentration and consumption of the alkaline absorption solution, can specifically make The CO that must be generated2Gas is all absorbed.
In the present invention, the further processing is preferably to CO2The neutralization that gas is obtained after being reacted with alkaline absorption solution Reactant is added in reaction solution, crystallization is then evaporated again, ammonium hydrogen carbonate solid is obtained.In the present invention, the reaction Agent be preferably one kind in ammonium hydrogen carbonate, ammonium carbonate and ammoniacal liquor, two or three;The addition of the reactant does not have any Particular/special requirement, enables to only include a kind of solute of ammonium hydrogen carbonate in neutralization reaction solution.The present invention is tied to the evaporation Brilliant mode and parameter does not have any particular/special requirement, the solvent of the neutralization reaction solution after further processing can be evaporated into dry Only, ammonium hydrogen carbonate solid is obtained.
In the present invention, the metathesis reaction process can add micro water, and a wetting state is provided to reaction, Promote the progress of reaction.In the present invention, the mass ratio of the molybdenum source and water is preferably 15:(0.25~1), more preferably 15: (0.5~0.75).
The preparation method of the ammonium dimolybdate provided with reference to embodiment the present invention is described in detail, but can not They are interpreted as limiting the scope of the present invention.
In all embodiments of the invention, the water added can provide a kind of wetting state to reaction, promote reaction Carry out.
Embodiment 1
The mass ratio of ammonium tetramolybdate, ammonium hydrogen carbonate and water is 15:3.9:0.25, it is well mixed, 80 DEG C of temperature, pressure is 0.13MPa, reaction time 2h, obtain ammonium dimolybdate product.The ammonium dimolybdate obtained to the present embodiment carries out X-ray detection, its As a result it is as shown in Figure 1.Its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate product purity> 99%.
Embodiment 2
The mass ratio of ammonium tetramolybdate, ammonium hydrogen carbonate and water is 15:4.2:0.5, it is well mixed, temperature 60 C, pressure is 0.12MPa, reaction time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, two molybdenums Sour ammonium product purity>99%.
Embodiment 3
The mass ratio of ammonium tetramolybdate, ammonium hydrogen carbonate and water is 15:4.5:1, it is well mixed, 90 DEG C of temperature, pressure is 0.15MPa, reaction time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, two molybdenums Sour ammonium product purity>99%.
Embodiment 4
The mass ratio of ammonium tetramolybdate, ammonium hydrogen carbonate and water is 15:4.7:0.25, it is well mixed, temperature 70 C, pressure is 0.14MPa, reaction time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, two molybdenums Sour ammonium product purity>99%.
Embodiment 5
The mass ratio of ammonium tetramolybdate, ammonium hydrogen carbonate and water is 15:4.7:0.5, it is well mixed, 75 DEG C of temperature, pressure is 0.11MPa, reaction time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, two molybdenums Sour ammonium product purity>99%.
Embodiment 6
The mass ratio of ammonium tetramolybdate, ammonium hydrogen carbonate and water is 15:4.5:0.5, it is well mixed, 80 DEG C of temperature, pressure is 0.12MPa, reaction time 1.5h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, and two Ammonium molybdate product purity>99%.
Embodiment 7
The mass ratio of molybdic acid, ammonium carbonate and water is 15:5:0.25, it is well mixed, 80 DEG C of temperature, pressure is 0.15MPa, instead 1h between seasonable, obtains product, its X-ray diffraction analysis result shows that thing present in product is mutually single, and ammonium dimolybdate product is pure Degree>99%.
Embodiment 8
The mass ratio of molybdic acid, ammonium carbonate and water is 15:5.4:0.25, it is well mixed, 90 DEG C of temperature, pressure is 0.14MPa, Reaction time 0.5h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate production Product purity>99%.
Embodiment 9
The mass ratio of molybdic acid, ammonium carbonate and water is 15:6:0.25, it is well mixed, temperature 70 C, pressure is 0.12MPa, instead 2h between seasonable, obtains product, its X-ray diffraction analysis result shows that thing present in product is mutually single, and ammonium dimolybdate product is pure Degree>99%.
Embodiment 10
The mass ratio of molybdic acid, ammonium carbonate and water is 15:5.4:1, it is well mixed, temperature 60 C, pressure is 0.14MPa, instead 2h between seasonable, obtains product, its X-ray diffraction analysis result shows that thing present in product is mutually single, and ammonium dimolybdate product is pure Degree>99%.
Embodiment 11
The mass ratio of molybdic acid, ammonium carbonate and water is 15:6:0.25, it is well mixed, temperature 60 C, pressure is 10.11MPa, Reaction time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate product Purity>99%.
Embodiment 12
The mass ratio of molybdic acid, ammonium carbonate and water is 15:4.6:1, it is well mixed, 90 DEG C of temperature, pressure is 0.12MPa, instead 2h between seasonable, obtains product, its X-ray diffraction analysis result shows that thing present in product is mutually single, and ammonium dimolybdate product is pure Degree>99%.
Embodiment 13
The mol ratio of molybdic acid and ammonium hydrogen carbonate is 1:1, it is well mixed, 80 DEG C of temperature, pressure is 0.13MPa, reaction time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate product purity> 99%.
Embodiment 14
NH in molybdic acid and ammoniacal liquor3·H2O mol ratio is 1:1, it is well mixed, temperature 70 C, pressure is 0.14MPa, reaction Time 2h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate product purity >99%.
Embodiment 15
NH in ammonium tetramolybdate and ammoniacal liquor3·H2O mol ratio is 1:2, it is well mixed, 80 DEG C of temperature, pressure is 0.11MPa, Reaction time 1.5h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate production Product purity>99%.
Embodiment 16
The mol ratio of ammonium tetramolybdate and ammonium carbonate is 1:1, it is well mixed, temperature 60 C, pressure is 0.12MPa, during reaction Between 1h, obtain product, its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate product purity> 99%.
Embodiment 17
Ammonium tetramolybdate and ammonium carbonate, ammonium hydrogen carbonate mol ratio are 1:0.5:0.9, it is well mixed, temperature 60 C, pressure is 0.12Mpa, reaction time 1h, obtains product, and its X-ray diffraction analysis result shows that thing present in product is mutually single, two molybdenums Sour ammonium product purity>99%.
Embodiment 18
Ammonium tetramolybdate and ammonium carbonate, ammoniacal liquor mol ratio are 1:0.6:1, it is well mixed, 80 DEG C of temperature, pressure is 0.14Mpa, 1h is reacted, product is obtained, its X-ray diffraction analysis result shows that thing present in product is mutually single, ammonium dimolybdate product purity >99%.
Embodiment 19
Molybdic acid and ammonium hydrogen carbonate, ammoniacal liquor mol ratio are 1:0.5:0.5, it is well mixed, temperature 70 C, pressure 0.11Mpa, instead 2h is answered, product is obtained, its X-ray diffraction analysis result shows that thing present in product is mutually single, the purity of ammonium dimolybdate product >99%.
Embodiment 20
Molybdic acid and ammonium carbonate, ammonium hydrogen carbonate, ammoniacal liquor mol ratio are 1:0.14:0.3:0.5, it is well mixed, temperature 60 C, pressure Power 0.15Mpa, reacts 1.2h, obtains product, its X-ray diffraction analysis result shows that thing present in product is mutually single, two molybdenums Sour ammonium product purity>99%.
As seen from the above embodiment, the invention provides a kind of preparation method of ammonium dimolybdate:Molybdenum source and source of ammonium are carried out Metathesis reaction, obtains ammonium dimolybdate.The present invention is using ammonium tetramolybdate and/or molybdic acid as molybdenum source, with ammoniacal liquor, ammonium hydrogen carbonate and carbon It is one or more of as source of ammonium in sour ammonium, without adding substantial amounts of solvent and water, environmental protection and saving.Can by the result of embodiment Know, the preparation method that the application is provided can be successfully obtained ammonium dimolybdate, and the equal > 99% of its purity.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (10)

1. a kind of preparation method of ammonium dimolybdate, is comprised the following steps:
Molybdenum source and source of ammonium are subjected to metathesis reaction, ammonium dimolybdate is obtained;
The molybdenum source is ammonium tetramolybdate and/or molybdic acid;
The source of ammonium is the one or more in ammoniacal liquor, ammonium hydrogen carbonate and ammonium carbonate.
2. preparation method according to claim 1, it is characterised in that the mol ratio of the molybdenum source and source of ammonium for (0.8~ 2.5):(0.8~2.5).
3. preparation method according to claim 1, it is characterised in that the mol ratio of the ammonium tetramolybdate and ammonium hydrogen carbonate is 1:(1.5~2.5).
4. preparation method according to claim 1, it is characterised in that the mol ratio of the ammonium tetramolybdate and ammonium carbonate is 1: (0.8~1.5).
5. preparation method according to claim 1, it is characterised in that NH in the ammonium tetramolybdate and ammoniacal liquor3·H2O's rubs You are than being 1:(1.5~2.5).
6. preparation method according to claim 1, it is characterised in that the mol ratio of the molybdic acid and ammonium hydrogen carbonate is 1: (0.8~1.5).
7. preparation method according to claim 1, it is characterised in that the mol ratio of the molybdic acid and ammonium carbonate for (1.8~ 2.5):1。
8. preparation method according to claim 1, it is characterised in that NH in the molybdic acid and ammoniacal liquor3·H2O mol ratio For 1:(0.8~1.5).
9. the preparation method according to claim 1~8 any one, it is characterised in that the temperature of the metathesis reaction For 60~90 DEG C;
The time of the metathesis reaction is 0.5~3h.
10. the preparation method according to claim 1~8 any one, it is characterised in that the pressure of the metathesis reaction For 0.1~0.15MPa.
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CN107601565A (en) * 2017-08-30 2018-01-19 金堆城钼业股份有限公司 A kind of preparation method of ammonium molybdate
CN108622938A (en) * 2018-07-23 2018-10-09 安徽华西稀有金属材料有限公司 A method of preparing ammonium dimolybdate from containing molybdenum solution
CN109665562A (en) * 2019-01-31 2019-04-23 成都虹波钼业有限责任公司 A kind of device and method preparing ammonium molybdate using molybdic acid

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