CN102267724A - Method for preparing ammonium molybdate - Google Patents

Method for preparing ammonium molybdate Download PDF

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Publication number
CN102267724A
CN102267724A CN2011101899139A CN201110189913A CN102267724A CN 102267724 A CN102267724 A CN 102267724A CN 2011101899139 A CN2011101899139 A CN 2011101899139A CN 201110189913 A CN201110189913 A CN 201110189913A CN 102267724 A CN102267724 A CN 102267724A
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ammonium molybdate
warm air
ammonia
air
preparation
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CN2011101899139A
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武洲
孙院军
厉学武
卜春阳
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Jinduicheng Molybdenum Co Ltd
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Jinduicheng Molybdenum Co Ltd
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Abstract

The invention discloses a method for preparing ammonium molybdate. The method comprises the following steps of: 1, filtering air through an air filter, heating the air to form hot air, and introducing the hot air into a drying chamber of atomization equipment through a hot air distributor; 2, filtering ammonium molybdate solution by using a filter, spraying the ammonium molybdate solution into the drying chamber through a sprayer of the atomization equipment to perform atomization and drying treatment, and thus obtaining settled ammonium molybdate at a discharge hole of the drying chamber; 3, introducing the hot air in the drying chamber and ammonia generated in the atomization and drying treatment into a cyclone separator, and settling and reclaiming the ammonium molybdate carried in the hot air after being separated by cyclone; 4, introducing the hot air subjected to cyclone separation and the ammonia into a bag filter to perform filtration and dust removal, and introducing the ammonia into a reclaiming system; and 5, reclaiming, combining and screening the ammonium molybdate, and thus obtaining an ammonium molybdate finished product. The method is simple in operation, low in production cost and high in production efficiency, and can realize continuous production of the ammonium molybdate.

Description

A kind of preparation method of ammonium molybdate
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of preparation method of ammonium molybdate.
Background technology
Ammonium molybdate is a kind of important product in the molybdenum heavy chemicals, is not only the main raw material of producing molybdenum powder, molybdenum goods, also can be used for aspects such as chemical reagent, catalyzer, fire retardant, little fertilizer and medicine.Molybdate has very strong condensation in weak acid environment, can form comparatively complicated polyacid and salt thereof such as heavy molybdic acid, three molybdic acids.In the time of 25 ℃～85 ℃, MoO 3-NH 3-H 2To separate out different compounds such as positive ammonium molybdate, ammonium dimolybdate, ammonium paramolybdate and ammonium octamolybdate under the different condition in the O system.Ammonium paramolybdate is heated to 245 ℃ or ammonium molybdate solution pH=2～3 that neutralize o'clock are obtained ammonium tetramolybdate.
Current industrial production mainly contains ammonium dimolybdate, ammonium tetramolybdate and ammonium octamolybdate etc. in the molybdenum chemical industry.Ammonium dimolybdate is to be formed by the crystallization of ammonium molybdate solution direct evaporation, can be the continuous crystallizer continuous production, also can be the discontinuous crystallizer batch production.Ammonium tetramolybdate be domestic production early, larger product, adopt the molybdenum calcining through pickling, ammonia soak, purify, acid heavy in and the crystalline method prepare.Ammonium octamolybdate is mainly used in efficient, the environmentally friendly flame-retardant smoke inhibition material of preparation, is to adopt ammonium dimolybdate solution and molybdic oxide to produce under 90 ℃.At present, yet there are no the report that adopts method of the present invention to prepare ammonium molybdate.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned the deficiencies in the prior art, provides a kind of simple to operate, and production cost is low, the preparation method of the ammonium molybdate that production efficiency is high.This method is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product by exporting in kiln discharge port and the cyclonic separator, can be realized the continuous production of ammonium molybdate continuously.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of ammonium molybdate is characterized in that this method comprises following concrete steps:
Step 1, air is filtered by air filter (1), heater via (2) adds the thermosetting warm air then, feeds warm air in the kiln (4) of atomising unit by hot-air distributor (3) again;
Step 2, ammonium molybdate solution is filtered the atomizer (6) of back by atomising unit with strainer (5) spray into and carry out atomization drying in the kiln (4) that feeds warm air in the step 1 and handle, obtain sedimentary ammonium molybdate at the discharge port of kiln (4);
Step 3, the ammonia that atomization drying processing in warm air in the kiln (4) and the step 2 is produced feed cyclonic separator (7), and the ammonium molybdate of carrying secretly in the warm air deposits recovery after cyclonic separation;
Step 4, warm air after cyclonic separation and ammonia in the step 3 fed in the bag filter (8) carry out dust removal by filtration, feed the recycling of carrying out ammonia in the ammonia recovery system (9) then;
Step 5, the ammonium molybdate that deposition reclaims after cyclonic separation in sedimentary ammonium molybdate and the step 3 described in the step 2 is merged the back screening obtain the finished product ammonium molybdate.
The preparation method of above-mentioned a kind of ammonium molybdate, the temperature of warm air described in the step 1 are 240 ℃～390 ℃.
The preparation method of above-mentioned a kind of ammonium molybdate, atomising unit described in step 1 and the step 2 is drying machine with centrifugal spray or Pressuresprayingdrier.
The preparation method of above-mentioned a kind of ammonium molybdate, the rotating speed of described drying machine with centrifugal spray is 10000 rev/mins～22000 rev/mins.
The preparation method of above-mentioned a kind of ammonium molybdate, the pressure of described Pressuresprayingdrier is 0.2MPa～0.5MPa.
Preparation method of the present invention realizes by equipment shown in Figure 2, this equipment comprises air filter, well heater, hot-air distributor and the kiln that is communicated with successively by pipeline, the kiln top is provided with atomizer, the strainer that is used to filter ammonium molybdate solution is connected with atomizer by pipeline, the venting port of kiln is connected with cyclonic separator, the bag filter that is used for dust removal by filtration is connected with the venting port at cyclonic separator top, and the venting port of bag filter is connected with the ammonia recovery system.
The present invention compared with prior art has the following advantages:
1, method of the present invention is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate.
2, the present invention is by converging ammonium molybdate solution after the atomizer atomizing of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
3, adopt the ammonium molybdate granularity of method preparation of the present invention little and be evenly distributed, granularity can reach about 1 μ m.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
The device structure synoptic diagram of Fig. 2 for realizing that the present invention adopts.
Fig. 3 is the electron microscopic shape appearance figure of the ammonium molybdate of the embodiment of the invention 1 preparation.
Description of reference numerals
The 1-air filter; The 2-well heater; The 3-hot-air distributor;
The 4-kiln; The 5-strainer; The 6-atomizer;
The 7-cyclonic separator; The 8-bag filter; 9-ammonia recovery system.
Embodiment
Preparation method of the present invention realizes by equipment shown in Figure 2, this equipment comprises air filter 1, well heater 2, hot-air distributor 3 and the kiln 4 that is communicated with successively by pipeline, kiln 4 tops are provided with atomizer 6, the strainer 5 that is used to filter ammonium molybdate solution is connected with atomizer 6 by pipeline, the venting port of kiln 4 is connected with cyclonic separator 7, the bag filter 8 that is used for dust removal by filtration is connected with the venting port at cyclonic separator 7 tops, and the venting port of bag filter 8 is connected with ammonia recovery system 9.
Embodiment 1
Step 1, air is filtered by air filter 1, heater via 2 (electrical heating power is 70KW) heating formation temperature is 240 ℃ a warm air then, again with warm air by hot-air distributor 3 in the shape of a spiral shape enter equably in the kiln 4 of atomising unit (Pressuresprayingdrier);
Step 2, be that the ammonium molybdate solution of 200g/L filters with strainer 5 with molybdenum content, adopt the pressure atomization mode then, spray volume with 100mL/min, with the atomizer 6 (rock field spray gun) of the ammonium molybdate solution after filtering by atomising unit (Pressuresprayingdrier), under the pressure of 0.2MPa, spray into imperceptible vaporific liquid pearl and enter in the step 1 and carry out atomization drying in the kiln 4 that feeds warm air and handle, obtain sedimentary ammonium molybdate at the discharge port of kiln 4;
Step 3, the ammonia that atomization drying processing in warm air in the kiln 4 and the step 2 is produced feed cyclonic separator 7, and the ammonium molybdate of carrying secretly in the warm air deposits recovery after cyclonic separation;
Step 4, warm air after cyclonic separation and ammonia in the step 3 fed in the bag filter 8 carry out dust removal by filtration, feed the recycling of carrying out ammonia in the ammonia recovery system 9 then;
Step 5, the ammonium molybdate that deposition reclaims after cyclonic separation in sedimentary ammonium molybdate and the step 3 described in the step 2 is merged the back screening obtain the finished product ammonium molybdate that granularity is about 1 μ m.
Fig. 3 is the electron microscopic shape appearance figure of the ammonium molybdate of present embodiment preparation, and as can be seen from Figure, the ammonium molybdate grain thickness of preparation is a Nano grade, and granularity little (about 1 μ m) is evenly distributed.
Present embodiment is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate, and the ammonium molybdate granularity of preparation is little and be evenly distributed.Present embodiment is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
Embodiment 2
The preparation method of present embodiment is identical with embodiment 1, and wherein difference is: the temperature of warm air is 390 ℃, and the pressure of Pressuresprayingdrier is 0.5MPa.
Present embodiment is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate, and the ammonium molybdate granularity of preparation is little and be evenly distributed.Present embodiment is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
Embodiment 3
The preparation method of present embodiment is identical with embodiment 1, and wherein difference is: the temperature of warm air is 300 ℃, and the pressure of Pressuresprayingdrier is 0.4MPa.
Present embodiment is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate, and the ammonium molybdate granularity of preparation is little and be evenly distributed.Present embodiment is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
Embodiment 4
Step 1, air is filtered by air filter 1, heater via 2 (electrical heating power is 70KW) heating formation temperature is 390 ℃ a warm air then, again with warm air by hot-air distributor 3 in the shape of a spiral shape enter equably in the kiln 4 of atomising unit (drying machine with centrifugal spray);
Step 2, be that the ammonium molybdate solution of 220g/L filters with strainer 5 with molybdenum content, adopt the centrifugal spraying mode then, with the atomizer 6 (centrifugal spraying head) of the ammonium molybdate solution after filtering by atomising unit (drying machine with centrifugal spray), under 10000 rev/mins speed conditions, spray into imperceptible vaporific liquid pearl and enter in the step 1 and carry out atomization drying in the kiln 4 that feeds warm air and handle, obtain sedimentary ammonium molybdate at the discharge port of kiln 4;
Step 3, the ammonia that atomization drying processing in warm air in the kiln 4 and the step 2 is produced feed cyclonic separator 7, and the ammonium molybdate of carrying secretly in the warm air deposits recovery after cyclonic separation;
Step 4, warm air after cyclonic separation and ammonia in the step 3 fed in the bag filter 8 carry out dust removal by filtration, feed the recycling of carrying out ammonia in the ammonia recovery system 9 then;
Step 5, the ammonium molybdate that deposition reclaims after cyclonic separation in sedimentary ammonium molybdate and the step 3 described in the step 2 is merged the back screening obtain the finished product ammonium molybdate that granularity is about 5 μ m.
Present embodiment is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate, and the ammonium molybdate granularity of preparation is little and be evenly distributed.Present embodiment is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
Embodiment 5
The preparation method of present embodiment is identical with embodiment 4, and wherein difference is: the temperature of warm air is 350 ℃, and the rotating speed of drying machine with centrifugal spray is 15000 rev/mins.
Present embodiment is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate, and the ammonium molybdate granularity of preparation is little and be evenly distributed.Present embodiment is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
Embodiment 6
The preparation method of present embodiment is identical with embodiment 4, and wherein difference is: the temperature of warm air is 240 ℃, and the rotating speed of drying machine with centrifugal spray is 22000 rev/mins.
Present embodiment is simple to operate, and production cost is low, and the production efficiency height can be realized the continuous production of ammonium molybdate, and the ammonium molybdate granularity of preparation is little and be evenly distributed.Present embodiment is by converging ammonium molybdate solution after the atomizer of atomising unit forms imperceptible vaporific liquid pearl with warm air, become ammonium molybdate crystal after the drying, finished product is continuously by exporting in kiln discharge port and the cyclonic separator, waste gas enters the ammonia recovery system after the bag filter dust removal by filtration, environmentally safe, the ammonia of recovery can be used once more.
The above; it only is preferred embodiment of the present invention; be not that the present invention is done any restriction, everyly any simple modification that above embodiment did, change and equivalent structure changed, all still belong in the protection domain of technical solution of the present invention according to the invention technical spirit.

Claims (5)

1. the preparation method of an ammonium molybdate is characterized in that, this method comprises following concrete steps:
Step 1, air is filtered by air filter (1), heater via (2) adds the thermosetting warm air then, feeds warm air in the kiln (4) of atomising unit by hot-air distributor (3) again;
Step 2, ammonium molybdate solution is filtered the atomizer (6) of back by atomising unit with strainer (5) spray into and carry out atomization drying in the kiln (4) that feeds warm air in the step 1 and handle, obtain sedimentary ammonium molybdate at the discharge port of kiln (4);
Step 3, the ammonia that atomization drying processing in warm air in the kiln (4) and the step 2 is produced feed cyclonic separator (7), and the ammonium molybdate of carrying secretly in the warm air deposits recovery after cyclonic separation;
Step 4, warm air after cyclonic separation and ammonia in the step 3 fed in the bag filter (8) carry out dust removal by filtration, feed the recycling of carrying out ammonia in the ammonia recovery system (9) then;
Step 5, the ammonium molybdate that deposition reclaims after cyclonic separation in sedimentary ammonium molybdate and the step 3 described in the step 2 is merged the back screening obtain the finished product ammonium molybdate.
2. the preparation method of a kind of ammonium molybdate according to claim 1 is characterized in that, the temperature of warm air described in the step 1 is 240 ℃～390 ℃.
3. the preparation method of a kind of ammonium molybdate according to claim 1 is characterized in that, atomising unit described in step 1 and the step 2 is drying machine with centrifugal spray or Pressuresprayingdrier.
4. the preparation method of a kind of ammonium molybdate according to claim 3 is characterized in that, the rotating speed of described drying machine with centrifugal spray is 10000 rev/mins～22000 rev/mins.
5. the preparation method of a kind of ammonium molybdate according to claim 3 is characterized in that, the pressure of described Pressuresprayingdrier is 0.2MPa～0.5MPa.
CN2011101899139A 2011-07-07 2011-07-07 Method for preparing ammonium molybdate Pending CN102267724A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104649322A (en) * 2014-12-23 2015-05-27 金堆城钼业股份有限公司 Preparation method of high-purity ammonium heptamolybdate
CN108550792A (en) * 2018-04-26 2018-09-18 桂林理工大学 A kind of preparation method and application of ammonium molybdate lithium ion battery negative material
CN112499683A (en) * 2020-12-30 2021-03-16 洛阳科硕钨钼材料有限责任公司 Ammonium molybdate preparation method and device
CN114309639A (en) * 2022-01-07 2022-04-12 郑州大学 Environment-friendly process for preparing molybdenum powder by ammonia gas and hydrogen gas relay reduction of ammonium molybdate

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CN1752023A (en) * 2005-08-11 2006-03-29 上海交通大学 Preparation method of inorganic fullerene structured molybdenium disulfide

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104649322A (en) * 2014-12-23 2015-05-27 金堆城钼业股份有限公司 Preparation method of high-purity ammonium heptamolybdate
CN104649322B (en) * 2014-12-23 2016-04-20 金堆城钼业股份有限公司 A kind of preparation method of high-purity Ammonium Heptamolybdate
CN108550792A (en) * 2018-04-26 2018-09-18 桂林理工大学 A kind of preparation method and application of ammonium molybdate lithium ion battery negative material
CN112499683A (en) * 2020-12-30 2021-03-16 洛阳科硕钨钼材料有限责任公司 Ammonium molybdate preparation method and device
CN112499683B (en) * 2020-12-30 2023-02-03 洛阳科硕钨钼材料有限责任公司 Ammonium molybdate preparation method and device
CN114309639A (en) * 2022-01-07 2022-04-12 郑州大学 Environment-friendly process for preparing molybdenum powder by ammonia gas and hydrogen gas relay reduction of ammonium molybdate
CN114309639B (en) * 2022-01-07 2024-05-28 郑州大学 Green preparation technology of molybdenum powder by relay reduction of ammonium molybdate by ammonia gas and hydrogen gas

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Application publication date: 20111207