CN103408071A - Process for producing ammonium molybdate - Google Patents
Process for producing ammonium molybdate Download PDFInfo
- Publication number
- CN103408071A CN103408071A CN201310374833XA CN201310374833A CN103408071A CN 103408071 A CN103408071 A CN 103408071A CN 201310374833X A CN201310374833X A CN 201310374833XA CN 201310374833 A CN201310374833 A CN 201310374833A CN 103408071 A CN103408071 A CN 103408071A
- Authority
- CN
- China
- Prior art keywords
- ammonium molybdate
- heavy metal
- ammonium
- organic solvent
- mother liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 title claims abstract description 40
- 229940010552 ammonium molybdate Drugs 0.000 title claims abstract description 39
- 235000018660 ammonium molybdate Nutrition 0.000 title claims abstract description 39
- 239000011609 ammonium molybdate Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 15
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 15
- 238000002386 leaching Methods 0.000 claims abstract description 12
- 239000012452 mother liquor Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 150000002576 ketones Chemical class 0.000 claims abstract description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 4
- 239000007790 solid phase Substances 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
- 238000001953 recrystallisation Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 abstract description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 3
- 239000011733 molybdenum Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 229910052785 arsenic Inorganic materials 0.000 abstract description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 231100000614 poison Toxicity 0.000 abstract description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 abstract description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003440 toxic substance Substances 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- XUFUCDNVOXXQQC-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)molybdenio)oxy-dioxomolybdenum Chemical compound N.N.O[Mo](=O)(=O)O[Mo](O)(=O)=O XUFUCDNVOXXQQC-UHFFFAOYSA-L 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a process for producing ammonium molybdate. The process comprises the steps of leaching molybdenum trioxide by using ammonia water so as to obtain ammonium molybdate ((NH4)2MoO4), adding sodium sulfide or introducing hydrogen sulfide, and then, filtrating so as to remove heavy metals. The process is characterized by comprising the steps of adding an alcohol or ketone organic solvent in a volume, which is 2-4 times that of a heavy metal removed ammonia leachate, into the heavy metal removed ammonia leachate, mixing thoroughly, precipitating ammonium molybdate crystals, standing and filtrating, thereby obtaining a solid phase which is crude ammonium molybdate; re-crystallizing the crude ammonium molybdate by using deionized water so as to obtain ammonium tetramolybdate ((NH4)2Mo4O13.2H2O); and reusing crude ammonium molybdate precipitated mother liquor to an ammonia leaching unit in a manner that the crude ammonium molybdate precipitated mother liquor is subjected to organic solvent recovery through distillation. The process has the advantages that the metal utilization ratio can reach over 99% and is much higher than 97% specified by molybdenum industry access conditions, 740kg of 98% nitric acid consumed by per ton of ammonium molybdate is reduced, and the production of ammonium nitrate waste liquid, which can cause secondary pollution due to the fact that the ammonium nitrate waste liquid contains a trace amount of toxic substances, such as heavy metal, arsenic and the like, is avoided.
Description
Technical field
The present invention relates to the production method of ammonium molybdate.
Background technology
Ammonium molybdate is important molybdenum salt intermediate and product, production technique was in the past, with certain density ammonia solvent molybdic oxide, generate ammonium molybdate solution, add sodium sulfide technique for removing heavy metal, after filtration, add nitric acid acid out precipitation ammonium molybdate, the ammonium nitrate waste liquid that this method produces is difficult to process, agriculture fertilizer is made with it by some enterprises, but wherein the toxic substances such as contained micro heavy, arsenic will cause secondary pollution, and ammonium molybdate per ton consumes 98% nitric acid 740kg.Reaction formula is as follows:
MoO
3+2NH
3.H
2O→(NH
4)
2MoO
4+H
2O
4(NH
4)
2MoO
4+6HNO
3→(NH
4)
2Mo
4O
13·2H
2O+6NH
4NO
3+H
2O
Summary of the invention
This process using organic solvent liberation method is processed ammonia leaching solution, then obtains ammonium molybdate through the water recrystallization, avoids using nitric acid, solves its Environment Obstacles.
The production technique of Yi Zhong Molybdenum acid ammonium, it comprises that molybdic oxide leaches and obtains ammonium molybdate ((NH with ammoniacal liquor
4)
2MoO
4) and add sodium sulphite or pass into hydrogen sulfide after filter, remove heavy metal, it is characterized in that: through removing the ammonia leaching solution of heavy metal, add alcohol or the organic solvent of ketone of 2～4 times of volumes, fully mix, separate out the ammonium molybdate crystallization, standing, filter, solid phase is thick ammonium molybdate; Thick ammonium molybdate, through the deionized water recrystallization, obtains ammonium tetramolybdate or ammonium dimolybdate; The mother liquor of separating out thick ammonium molybdate is recycled and reused for ammonia leaching unit after the Distillation recovery organic solvent.
The production technique of above-mentioned ammonium molybdate is characterized in that: described alcohol or organic solvent of ketone are methyl alcohol, ethanol, acetone or butanone.
The production technique of above-mentioned ammonium molybdate is characterized in that: described thick ammonium molybdate passes into hydrogen sulfide or ammonium sulfate and filters removal heavy metal after 3-5 time is repeated to apply mechanically through the mother liquor after the deionized water recrystallization, then continue to reuse.
The accompanying drawing explanation
Fig. 1 ammonium molybdate technical process of the present invention.
Embodiment
Below with embodiment, further illustrate the present invention.
Embodiment 1
Get the ammonium molybdate ammonia leaching solution 100mL concentration approximately 25% that removes heavy metal, under agitation add 400mL methyl alcohol, continue to stir 30min, vacuum filtration 10min; Filter cake adds deionized water 60ml, under stirring, is heated to 80～90 ℃, treats that ammonium molybdate is entirely molten, filtered while hot, and filtrate is cooled to room temperature, crystallization, suction filtration, filter cake are dried and are obtained ammonium tetramolybdate, purity 98.12%.
Solvent is separated out filtrate through Distillation recovery methyl alcohol, the about 80kg/t ammonium molybdate of methanol consumption.
Mother liquor is recycled and reused for the preparation ammonia leaching solution.Recrystallization mother liquor, after 3 recyclings, passes into a small amount of hydrogen sulfide or sulfuration ammonia and filters, removal heavy metal, then continue recycling.
Embodiment 2
Get the ammonium molybdate ammonia leaching solution 100mL concentration approximately 25% that removes heavy metal, under agitation add the 250mL butanone, continue to stir 30min, vacuum filtration 10min; Filter cake adds deionized water 70ml, and suitably adds ammoniacal liquor to regulate pH5.5～6.5, under stirring, is heated to 80～90 ℃, treats that ammonium molybdate is entirely molten, filtered while hot, and filtrate is cooled to room temperature, crystallization, suction filtration, filter cake are dried and are obtained ammonium dimolybdate, purity 98.2%.
Solvent is separated out filtrate through the Distillation recovery butanone, and butanone consumes about 70kg/t ammonium molybdate.
Mother liquor is recycled and reused for the preparation ammonia leaching solution.Recrystallization mother liquor, after 5 recyclings, passes into a small amount of hydrogen sulfide or sulfuration ammonia and filters, removal heavy metal, then continue recycling.
In above two embodiment, separate out mother liquor and recrystallization mother liquor and all can realize recycling due to solvent, only have drying course that a small amount of loss is arranged, the using rate of metal of whole process can reach more than 99%, far above 97% of " molybdenum industry access condition " regulation.
Claims (4)
1. the production technique of an ammonium molybdate, it comprises after molybdic oxide obtains ammonium molybdate and adds sodium sulphite or pass into hydrogen sulfide with the ammoniacal liquor leaching filters, remove heavy metal, it is characterized in that: through removing the ammonia leaching solution of heavy metal, add alcohol or the organic solvent of ketone of 2～4 times of volumes, fully mix, separate out the ammonium molybdate crystallization, standing, to filter, solid phase is thick ammonium molybdate; Thick ammonium molybdate, through the deionized water recrystallization, obtains ammonium tetramolybdate.
2. the production technique of ammonium molybdate according to claim 1, it is characterized in that: described alcohol or organic solvent of ketone are methyl alcohol, ethanol, acetone or butanone.
3. the production technique of ammonium molybdate according to claim 1 is characterized in that: described mother liquor of separating out thick ammonium molybdate is recycled and reused for ammonia leaching unit after the Distillation recovery organic solvent.
4. the production technique of ammonium molybdate according to claim 1, it is characterized in that: described thick ammonium molybdate, passes into hydrogen sulfide and filters removal heavy metal, then continue to reuse through the mother liquor after the deionized water recrystallization after 3-5 time is repeated to apply mechanically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310374833XA CN103408071A (en) | 2013-08-23 | 2013-08-23 | Process for producing ammonium molybdate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310374833XA CN103408071A (en) | 2013-08-23 | 2013-08-23 | Process for producing ammonium molybdate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103408071A true CN103408071A (en) | 2013-11-27 |
Family
ID=49601132
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310374833XA Pending CN103408071A (en) | 2013-08-23 | 2013-08-23 | Process for producing ammonium molybdate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103408071A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105314681A (en) * | 2014-07-05 | 2016-02-10 | 丁明 | Preparation method of molybdate |
| CN105439201A (en) * | 2014-09-30 | 2016-03-30 | 泰州市贝斯特钼制品有限公司 | Method for improving crystal quality of ammonium molybdate |
| 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 |
| CN112516752A (en) * | 2020-12-03 | 2021-03-19 | 金堆城钼业股份有限公司 | Method and device for treating ammonia-containing tail gas |
| CN113603612A (en) * | 2021-08-10 | 2021-11-05 | 长沙望城石油化工有限公司 | Molybdenum carbamate compound, production process thereof, lubricant and lubricating grease thereof |
| CN113893572A (en) * | 2021-11-23 | 2022-01-07 | 中南大学 | Crystallization method of beta-ammonium tetramolybdate |
-
2013
- 2013-08-23 CN CN201310374833XA patent/CN103408071A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 蒲敬文等: ""钼精矿制取四钼酸铵实验研究"", 《甘肃冶金》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105314681A (en) * | 2014-07-05 | 2016-02-10 | 丁明 | Preparation method of molybdate |
| CN105314681B (en) * | 2014-07-05 | 2017-03-22 | 丁明 | Preparation method of molybdate |
| CN105439201A (en) * | 2014-09-30 | 2016-03-30 | 泰州市贝斯特钼制品有限公司 | Method for improving crystal quality of ammonium molybdate |
| 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 |
| CN112516752A (en) * | 2020-12-03 | 2021-03-19 | 金堆城钼业股份有限公司 | Method and device for treating ammonia-containing tail gas |
| CN113603612A (en) * | 2021-08-10 | 2021-11-05 | 长沙望城石油化工有限公司 | Molybdenum carbamate compound, production process thereof, lubricant and lubricating grease thereof |
| CN113893572A (en) * | 2021-11-23 | 2022-01-07 | 中南大学 | Crystallization method of beta-ammonium tetramolybdate |
| CN113893572B (en) * | 2021-11-23 | 2022-07-05 | 中南大学 | Crystallization method of beta-ammonium tetramolybdate |
| US11701600B2 (en) | 2021-11-23 | 2023-07-18 | Central South University | Method for crystallization of β-ammonium tetramolybdate |
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Application publication date: 20131127 |