CN107188229B - A kind of preparation method of ten ammonium molybdates - Google Patents
A kind of preparation method of ten ammonium molybdates Download PDFInfo
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- CN107188229B CN107188229B CN201710422834.5A CN201710422834A CN107188229B CN 107188229 B CN107188229 B CN 107188229B CN 201710422834 A CN201710422834 A CN 201710422834A CN 107188229 B CN107188229 B CN 107188229B
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Abstract
The present invention provides a kind of preparation methods of ten ammonium molybdates：Molybdenum source and source of ammonium are subjected to metathesis reaction, obtain ten ammonium molybdates.The present invention is using ammonium tetramolybdate and/or molybdic acid as molybdenum source, using one or more of ammonium hydroxide, ammonium hydrogen carbonate and ammonium carbonate as source of ammonium, without adding a large amount of solvent and water, environmental protection and saving.By the result of embodiment it is found that preparation method provided by the present application can be successfully obtained ten ammonium molybdates, and the equal ＞ of its purity 99%.
Description
Technical field
The present invention relates to ammonium molybdate technical field more particularly to a kind of preparation methods of ten ammonium molybdates.
Background technology
Ten ammonium molybdates are a kind of common ammonium molybdates, and molecular formula is (NH4)8Mo10O34.Currently, ten ammonium molybdates are by widely
For dyestuff, the raw material of pigment, catalyst, fireproof agent, trace-element fertilizer, ceramic pigment and the other compounds of synthesis.
Currently, the method for producing ten ammonium molybdates in the prior art is generally required for being reacted in aqueous solution, 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, after production ammonia-containing water can not directly outer row, can only evaporative crystallization, cause higher energy expenditure；And ten molybdenum
Sour ammonium product purity control is difficult, and impurity is easy to be mixed into wherein.
Invention content
The method that the purpose of the present invention is to provide a kind of to prepare ten ammonium molybdates in the case where not adding a large amount of water, this hair
The method flow of bright offer is short, low energy consumption, pollution is low, at low cost and easy to operate.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of preparation methods of ten ammonium molybdates, comprise the following steps：
Molybdenum source and source of ammonium are subjected to metathesis reaction, obtain ten ammonium molybdates；
The molybdenum source is ammonium tetramolybdate and/or molybdic acid；
The source of ammonium is one or more of ammonium hydroxide, ammonium hydrogen carbonate and ammonium carbonate.
Preferably, the molar ratio of the molybdenum source and source of ammonium is 10:(2~14).
Preferably, the molar ratio of the ammonium tetramolybdate and ammonium hydrogen carbonate is 10:(10~14).
Preferably, the molar ratio of the ammonium tetramolybdate and ammonium carbonate is 10:(4~8).
Preferably, NH in the ammonium tetramolybdate and ammonium hydroxide3·H2The molar ratio of O is 10:(10~14).
Preferably, the molar ratio of the molybdic acid and ammonium hydrogen carbonate is 10:(6~10).
Preferably, the molar ratio of the molybdic acid and ammonium carbonate is 10:(2~6).
Preferably, NH in the molybdic acid and ammonium hydroxide3·H2The molar ratio of O is 10:(6~10).
Preferably, the temperature of the metathesis reaction is 100~130 DEG C；
The time of the metathesis reaction is 0.5~3h.
Preferably, the pressure of the metathesis reaction is 0.1~0.15MPa.
The present invention provides a kind of preparation methods of ten ammonium molybdates：Molybdenum source and source of ammonium are subjected to metathesis reaction, obtain ten
Ammonium molybdate.The present invention is using ammonium tetramolybdate and/or molybdic acid as molybdenum source, with one kind in ammonium hydroxide, ammonium hydrogen carbonate and ammonium carbonate or several
Kind is used as source of ammonium, without adding a large amount of solvent and water, environmental protection and saving.By the result of embodiment it is found that provided by the present application
Preparation method can be successfully obtained ten ammonium molybdates, and the equal ＞ of its purity 99%.
Description of the drawings
Fig. 1 is the X-ray diffraction spectrogram for ten ammonium molybdates that embodiment 1 obtains.
Specific implementation mode
The present invention provides a kind of preparation methods of ten ammonium molybdates, comprise the following steps：
Molybdenum source and source of ammonium are subjected to metathesis reaction, obtain ten ammonium molybdates；
The molybdenum source is ammonium tetramolybdate and/or molybdic acid；
The source of ammonium is one or more of ammonium hydroxide, ammonium hydrogen carbonate and ammonium carbonate.
Molybdenum source and source of ammonium are carried out metathesis reaction by the present invention, obtain ten ammonium molybdates.In the present invention, the molybdenum source is four
Ammonium molybdate and/or molybdic acid；The source of ammonium is one or more of ammonium hydroxide, ammonium hydrogen carbonate and ammonium carbonate.The present invention is to the molybdenum
Source and the source of source of ammonium do not have any particular/special requirement, are using commercially available molybdenum source well-known to those skilled in the art and source of ammonium
Can, it is specific if the ammonium tetramolybdate can be commercially available two hydrations ammonium tetramolybdate.The present invention does not have the ammonium hydroxide any
Particular/special requirement, using the ammonium hydroxide of commercial concentration well-known to those skilled in the art, preferably 25~28wt%.
In the present invention, the molar ratio of the molybdenum source and source of ammonium is preferably 10:(2~14), more preferably 10:(6~10).
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 molar ratio of ammonium molybdate and ammonium hydrogen carbonate is preferably 10:(10~14), more preferably 10:(11~13), most preferably 10:12.
In the present invention, the ammonium tetramolybdate and the equation of ammonium hydrogen carbonate reaction are specifically：
5(NH4)2Mo4O13+6NH4HCO3=2 (NH4)8Mo10O34+6CO2↑+3H2O。
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 molar ratio of sour ammonium and ammonium carbonate is preferably 10:(4~8), more preferably 10:(5~7), most preferably 10:6.In the present invention
In, the equation of the ammonium tetramolybdate and ammonium carbonate reaction is specifically：
5(NH4)2Mo4O13+3(NH4)2CO3=2 (NH4)8Mo10O34+3CO2↑。
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, and the source of ammonium is ammonium hydroxide, four molybdic acid
NH in ammonium and ammonium hydroxide3·H2The molar ratio of O is preferably 10:(10~14), more preferably 10:(11~13), most preferably 10:12.
In the present invention, the ammonium tetramolybdate and the equation of ammonium hydroxide reaction are specifically：
5(NH4)2Mo4O13+6NH3·H2O=2 (NH4)8Mo10O34+3H2O。
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 molar ratio of ammonium hydrogen carbonate is preferably 10:(6~10), more preferably 10:(7~9), most preferably 10:8.In the present invention, institute
Stating the equation that molybdic acid and ammonium hydrogen carbonate react is specifically：
10H2MoO4+8NH4HCO3=(NH4)8Mo10O34+8CO2↑+14H2O。
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 molar ratio of sour ammonium is preferably 10:(2~6), more preferably 10:(3~5), most preferably 10:4.In the present invention, the molybdenum
Acid and the equation of ammonium carbonate reaction are specifically：
10H2MoO4+4(NH4)2CO3=(NH4)8Mo10O34+4CO2↑+10H2O。
In the specific embodiment of the invention, when the molybdenum source is molybdic acid, and the source of ammonium is ammonium hydroxide, the molybdic acid and ammonium hydroxide
Middle NH3·H2The molar ratio of O is preferably 10:(6~10), more preferably 10:(7~9), most preferably 10:8.In the present invention,
The molybdic acid and the equation of ammonium hydroxide reaction are specifically：
10H2MoO4+8NH3·H2O=(NH4)8Mo10O34+14H2O。
In the present invention, when the mixture that the molybdenum source is ammonium tetramolybdate and molybdic acid, the source of ammonium is ammonium hydroxide, ammonium hydrogen carbonate
When 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, the molar ratio of the ammonium tetramolybdate and ammonium carbonate, ammonium hydrogen carbonate is preferably 10：(2~4)：(5~7), more preferably
It is 10：3：6.
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 ammonium hydroxide
When closing object, NH in the ammonium tetramolybdate and ammonium carbonate, ammonium hydroxide3·H2The molar ratio of O is preferably 10：(2~4)：(5~7), more
Preferably 10：3：6.
In the specific embodiment of the invention, when the molybdenum source is ammonium tetramolybdate, the source of ammonium is ammonium hydrogen carbonate and ammonium hydroxide
When mixture, NH in the ammonium tetramolybdate and ammonium hydrogen carbonate, ammonium hydroxide3·H2The molar ratio of O is preferably 10：(5~7)：(5~7),
More preferably 10：6：6.
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
When the mixture of ammonium hydroxide, NH in the ammonium tetramolybdate and ammonium carbonate, ammonium hydrogen carbonate, ammonium hydroxide3·H2The molar ratio of O is preferably 10：(1
~4)：(3~7)：(3~7), more preferably 10：(2~3)：(4~5)：(5~6).
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
When closing object, the molar ratio of the molybdic acid and ammonium carbonate, ammonium hydrogen carbonate is preferably 10：(2~5)：(3~7), more preferably 10：(3
~4)：(4~5).
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 ammonium hydroxide
When, NH in the molybdic acid and ammonium carbonate, ammonium hydroxide3·H2The molar ratio of O is preferably 10：(2~5)：(3~7), more preferably 10：(3
~4)：(4~5).
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 ammonium hydroxide
When object, NH in the molybdic acid and ammonium hydrogen carbonate, ammonium hydroxide3·H2The molar ratio of O is preferably 10：(3~7)：(3~7), more preferably
10：(4~5)：(5~6).
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 ammonium hydroxide
Mixture when, NH in the molybdic acid and ammonium carbonate, ammonium hydrogen carbonate, ammonium hydroxide3·H2The molar ratio of O is preferably 10：(0.5~4)：
(1.5~5)：(1.5~5), more preferably 10：(1~3)：(2~3)：(2~3).
In the present invention, the metathesis reaction carries out preferably in closed container；The pressure of the metathesis reaction is excellent
It is selected as 0.1~0.15MPa, more preferably 0.11~0.14MPa, most preferably 0.12~0.13MPa；The metathesis reaction
Temperature is preferably 100~130 DEG C, more preferably 110~120 DEG C, most preferably 115 DEG C；The time of the metathesis reaction is excellent
It is selected as 0.5~3h, more preferably 1~2.5h, most preferably 1.5~2h.
Processing is dried in the product system that the present invention preferably obtains the metathesis reaction, obtains ten 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 the present invention preferably generates the metathesis reaction process2Gas is recycled.Of the invention specific
In embodiment, present invention preferably uses alkaline absorption solutions to CO2Gas is absorbed；The alkaline absorption solution be preferably ammonium hydroxide or
Sal volatile, CO2Gas obtains neutralization reaction solution after being reacted with alkaline absorption solution, anti-for double decomposition after being further processed
The raw material answered.The present invention does not have any particular/special requirement to the concentration and dosage of the alkaline absorption solution, can specifically make
The CO that must be generated2Gas is all absorbed.
In the present invention, described to be further processed preferably to CO2The neutralization that gas obtains after being reacted with alkaline absorption solution
Reactant is added in reaction solution, is then evaporated crystallization again, obtains ammonium hydrogen carbonate solid.In the present invention, the reaction
Agent be preferably one kind in ammonium hydrogen carbonate, ammonium carbonate and ammonium hydroxide, two or three；The additive amount of the reactant does not have any
Particular/special requirement enables to include only a kind of solute of ammonium hydrogen carbonate in neutralization reaction solution.The present invention ties the evaporation
Brilliant mode and parameter does not have any particular/special requirement, and the evaporation of the solvent of the neutralization reaction solution after capable of being further processed is done
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:(0.1~1), more preferably 15:
(0.5~0.75).
The preparation method of ten ammonium molybdate provided by the invention is described in detail with reference to embodiment, but cannot
They are interpreted as limiting the scope of the present invention.
Embodiment 1
The mass ratio of ammonium tetramolybdate, ammonium carbonate and water is 15:1.95:0.5, it is uniformly mixed, 110 DEG C of temperature, pressure is
0.13MPa, reaction time 1h obtain ten ammonium molybdate products.X-ray detection is carried out to ten ammonium molybdates that the present embodiment obtains,
The results are shown in Figure 1.Its X-ray diffraction analysis the result shows that, object present in product is mutually single, ten ammonium molybdate product purities>
99%.
Embodiment 2
The mass ratio of ammonium tetramolybdate, ammonium carbonate and water is 15:1.72:1, it is uniformly mixed, 120 DEG C of temperature, pressure is
0.12MPa, reaction time 2h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten molybdenums
Sour ammonium product purity>99%.
Embodiment 3
The mass ratio of molybdic acid, ammonium hydrogen carbonate and water is 15:6.2:0.1, it is uniformly mixed, 110 DEG C of temperature, pressure is
0.15MPa, reaction time 1h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten molybdenums
Sour ammonium product purity>99%.
Embodiment 4
The mass ratio of molybdic acid, ammonium hydrogen carbonate and water is 15:5.87:0.25, it is uniformly mixed, 120 DEG C of temperature, pressure is
0.14MPa, reaction time 0.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 5
The mass ratio of molybdic acid, ammonium carbonate and water is 15:6:0.25, it is uniformly mixed, temperature 70 C, pressure 0.12MPa, instead
2h between seasonable, obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single, and ten ammonium molybdate products are pure
Degree>99%.
Embodiment 6
The mass ratio of molybdic acid, ammonium hydrogen carbonate and water is 15:6:1, it is uniformly mixed, 130 DEG C, pressure 0.14MPa of temperature, instead
2h between seasonable, obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single, and ten ammonium molybdate products are pure
Degree>99%.
Embodiment 7
The molar ratio of molybdic acid and ammonium carbonate is 10:4, it is uniformly mixed, 100 DEG C, pressure 0.13MPa of temperature, the reaction time
2h obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten ammonium molybdate product purities>
99%.
Embodiment 8
NH in molybdic acid and ammonium hydroxide3·H2The molar ratio of O is 10:8, it is uniformly mixed, 110 DEG C, pressure 0.14MPa of temperature, instead
2h between seasonable, obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single, and ten ammonium molybdate products are pure
Degree>99%.
Embodiment 9
NH in ammonium tetramolybdate and ammonium hydroxide3·H2The molar ratio of O is 5:6, it is uniformly mixed, 120 DEG C of temperature, pressure is
0.11MPa, reaction time 1.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 10
The molar ratio of ammonium tetramolybdate and ammonium hydrogen carbonate is 5:6, it is uniformly mixed, 130 DEG C, pressure 0.12MPa of temperature, reaction
Time 1h obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten ammonium molybdate product purities
>99%.
Embodiment 11
Ammonium tetramolybdate and ammonium carbonate, ammonium hydrogen carbonate molar ratio are 10:2.7:6.2, it is uniformly mixed, 110 DEG C of temperature, pressure is
0.14MPa, reaction time 0.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 12
Ammonium tetramolybdate and ammonium carbonate, ammonium hydroxide molar ratio are 10:3.3:5.9, it is uniformly mixed, 130 DEG C of temperature, pressure is
0.12MPa, reaction time 0.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 13
Ammonium tetramolybdate and ammonium hydrogen carbonate, ammonium hydroxide molar ratio are 10:6.1:5.5, it is uniformly mixed, 110 DEG C of temperature, pressure is
0.12MPa, reaction time 0.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 14
Ammonium tetramolybdate and ammonium carbonate, ammonium hydrogen carbonate, ammonium hydroxide molar ratio are 10:2:5:5, it is uniformly mixed, 130 DEG C of temperature, pressure
Power is 0.13MPa, and reaction time 0.5h obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single
One, ten ammonium molybdate product purities>99%.
Embodiment 15
Molybdic acid and ammonium carbonate, ammonium hydrogen carbonate molar ratio are 10:3.6:4.3, it is uniformly mixed, 130 DEG C of temperature, pressure is
0.14MPa, reaction time 0.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 16
Molybdic acid and ammonium carbonate, ammonium hydroxide molar ratio are 10:2.8:4, it is uniformly mixed, 110 DEG C, pressure 0.12MPa of temperature, instead
0.5h between seasonable, obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten ammonium molybdate products
Purity>99%.
Embodiment 17
Molybdic acid and ammonium hydrogen carbonate, ammonium hydroxide molar ratio are 10:5.6:6.8, it is uniformly mixed, 120 DEG C of temperature, pressure is
0.12MPa, reaction time 0.5h obtain product, X-ray diffraction analysis the result shows that, object present in product is mutually single, ten
Ammonium molybdate product purity>99%.
Embodiment 18
Molybdic acid and ammonium carbonate, ammonium hydrogen carbonate, ammonium hydroxide molar ratio are 10:1.1:3.5:2.7, it is uniformly mixed, 110 DEG C of temperature,
Pressure is 1.4MPa, and reaction time 0.5h obtains product, X-ray diffraction analysis the result shows that, object present in product is mutually single
One, ten ammonium molybdate product purities>99%.
As seen from the above embodiment, the present invention provides a kind of preparation methods of ten ammonium molybdates：Molybdenum source and source of ammonium are carried out
Metathesis reaction obtains ten ammonium molybdates.The present invention is using ammonium tetramolybdate and/or molybdic acid as molybdenum source, with ammonium hydroxide, ammonium hydrogen carbonate and carbon
One or more of sour ammonium is used as source of ammonium, without adding a large amount of solvent and water, environmental protection and saving.It can by the result of embodiment
Know, preparation method provided by the present application can be successfully obtained ten ammonium molybdates, and the equal ＞ of its purity 99%.
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 (8)
1. a kind of preparation method of ten ammonium molybdates, comprises the following steps：
Molybdenum source and source of ammonium are subjected to metathesis reaction, obtain ten ammonium molybdates；
The molybdenum source is ammonium tetramolybdate and/or molybdic acid；
The source of ammonium is one or more of ammonium hydroxide, ammonium hydrogen carbonate and ammonium carbonate；
The molar ratio of the molybdenum source and source of ammonium is 10:(2~14)；
The temperature of the metathesis reaction is 100~130 DEG C；
The time of the metathesis reaction is 0.5~3h.
2. preparation method according to claim 1, which is characterized in that the molar ratio of the ammonium tetramolybdate and ammonium hydrogen carbonate is
10:(10~14).
3. preparation method according to claim 1, which is characterized in that the molar ratio of the ammonium tetramolybdate and ammonium carbonate is
10:(4~8).
4. preparation method according to claim 1, which is characterized in that NH in the ammonium tetramolybdate and ammonium hydroxide3·H2O's rubs
You are than being 10:(10~14).
5. preparation method according to claim 1, which is characterized in that the molar ratio of the molybdic acid and ammonium hydrogen carbonate is 10:
(6~10).
6. preparation method according to claim 1, which is characterized in that the molar ratio of the molybdic acid and ammonium carbonate is 10:(2
~6).
7. preparation method according to claim 1, which is characterized in that NH in the molybdic acid and ammonium hydroxide3·H2The molar ratio of O
It is 10:(6~10).
8. according to the preparation method described in claim 1~7 any one, which is characterized in that the pressure of the metathesis reaction
For 0.1~0.15MPa.
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