CN109574076A - A kind of preparation method of high-purity molybdenum trioxide - Google Patents
A kind of preparation method of high-purity molybdenum trioxide Download PDFInfo
- Publication number
- CN109574076A CN109574076A CN201811587964.5A CN201811587964A CN109574076A CN 109574076 A CN109574076 A CN 109574076A CN 201811587964 A CN201811587964 A CN 201811587964A CN 109574076 A CN109574076 A CN 109574076A
- Authority
- CN
- China
- Prior art keywords
- molybdenum trioxide
- purity
- calcination
- preparation
- molybdenum
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to a kind of preparation methods of high-purity molybdenum trioxide comprising following steps: after ammonium molybdate is carried out calcination at 600~700 DEG C, obtaining molybdenum trioxide crude product；The molybdenum trioxide crude product is added in nitric acid solution, is filtered after dissolution, filter residue is collected；The filter residue is added in ammonium hydroxide, is concentrated after dissolution, obtains concentrate；After concentrate drying, calcination is carried out at 600~700 DEG C, obtains the high-purity molybdenum trioxide.Compared with prior art, for the present invention with following the utility model has the advantages that present invention process has the features such as safe and environment-friendly, reaction speed is fast, product purity height is convenient for expanding production by oxidation obtained.
Description
Technical field
The invention belongs to high purity reagent technical fields, are related to a kind of preparation method of high-purity molybdenum trioxide.
Background technique
Molybdenum trioxide, English name: Molybdenum trioxide, molecular formula: MoO3.White is heated to grey powder
Shi Huangse is slightly soluble in water, is dissolved in concentrated nitric acid, concentrated hydrochloric acid, is soluble in concentrated base.
The compound of molybdenum is widely used as various catalyst materials.Molybdenum trioxide is a kind of highly important Industrial Catalysis
Agent, photoelectricity device material and gas sensor material.In addition, the compound of molybdenum and molybdenum can also be applied to battery, air-sensitive material
Material and media inhibitor etc..Usually, the toxicity of molybdenum base material is all relatively low, this is conducive to our health and environment
Protection.
According to domestic and foreign literature document announcement, in traditional handicraft, as Chinese patent CN104651637A disclose it is a kind of high
The processing technology of pure molybdenum trioxide, this method process molybdenum concentrate using sublimed method, processing step are as follows: Step 1: screening
Processing；Step 2: the molybdenum concentrate screened is placed in water, clean, impregnates 3 days；It is made Step 3: carrying out roasting in calcining furnace
Roast sand；Step 4: roasting sand is crossed 20 meshes, sieving powder is obtained；Step 5: reducing agent is added in sieving powder；Step
Rapid six, sieving powder is placed in calcining furnace, calcining in-furnace temperature is risen to 800~900 DEG C and is distilled；Step 7: with rapid
Cold medium cools down gaseous state molybdenum trioxide, and material after cooling is high-purity molybdenum trioxide after dedusting, and this method needs
Multiple calcination crushes or the methods of spent ion exchange resin processing, as Chinese patent CN107364889A disclose it is a kind of high
Pure molybdenum trioxide and preparation method thereof, the preparation method include the following steps: that ammonium molybdate is dissolved in ammonium hydroxide by (1), obtain molybdenum
Acid ammonium solution；(2) ammonium molybdate solution is contacted with acid cation exchange resin, obtains ammonium molybdate solution after purification；
(3) it is 7-8.5 that ammonium hydroxide is added in the ammonium molybdate solution of Xiang Suoshu after purification and adjusts pH value, and nitric acid is then added and carries out the heavy knot of acid
Crystalline substance is finally separated by solid-liquid separation and obtains solid phase；(4) solid phase is dried, obtains high-purity ammonium molybdate；(5) by the High-Purity Molybdenum
Sour ammonium is calcined, and high-purity molybdenum trioxide is obtained.This method process route is long.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of high-purity molybdenum trioxide, to solve in the prior art high-purity three
The above problem present in the preparation of molybdenum oxide.
The present invention is achieved by the following technical solutions:
The present invention provides a kind of preparation methods of high-purity molybdenum trioxide comprising following steps:
After ammonium molybdate is carried out calcination at 600~700 DEG C, molybdenum trioxide crude product is obtained；
The molybdenum trioxide crude product is added in 65~68% nitric acid solution, is filtered after dissolution, collects filter residue；
The filter residue is added in ammonium hydroxide, is concentrated after dissolution filter, obtains concentrate；
After concentrate drying, calcination is carried out at 600~700 DEG C, obtains the high-purity molybdenum trioxide, purity is
99.5% or more.
Preferably, the calcination temperature is 600~700 DEG C, and temperature is excessively high to have portioned product distillation loss, temperature
It spends low decomposition not exclusively, influences quality.
Preferably, the method for the concentration is vacuum distillation.
The fundamental reaction mechanism of the method for the present invention: ammonium molybdate is thermally decomposed into molybdenum trioxide crude product, is washed away with nitric acid solvable
Property impurity, then remove insoluble impurities with ammonia solvent, generate high-purity ammonium molybdate after obtained pure ammonium molybdate thermal decomposition.
Compared with prior art, the present invention have it is following the utility model has the advantages that
The purification process that present invention process is related to carries out in the solution, is all simple dissolution and filtering, does not need powder
The broken equal times are long and the process that is readily incorporated impurity, also do not need the post-processing using the complexity such as ion-exchange-resin process
Journey.This method has the features such as safe and environment-friendly, reaction speed is fast, molybdenum trioxide product purity is high obtained, convenient for expanding life
It produces.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
Embodiment l
Ammonium molybdate 500g is set enter in Muffle furnace on the enamel evaporating dish of 500ml 600 DEG C calcination 3 hours at molybdenum oxide.
Taking out calcination, good molybdenum oxide enters in the glass beaker of 2000ml, is added 65% nitric acid dousing of 500ml 5 hours.
Incline nitric acid, is washed with distilled water, and drains.
Crystallization is concentrated under reduced pressure in the molybdenum oxide ammonia solvent drained.
Crystallization evaporating dish enter in Muffle furnace 600 DEG C calcination 3 hours at molybdenum oxide.Yield 75.6%, content 99.5%.
Impurity content: silver (Ag) 0.00005%；Arsenic (As) 0.0005%；Barium (Ba) 0.0005%；Copper (Cu)
0.0001%；Iron (Fe) 0.0001%；Magnesium (Mg) 0.0001%；Manganese (Mn) 0.00005%；Nickel (Ni) 0.00005%；Lead (Pb)
0.0001%；Zinc (Zn) 0.0001%.
Embodiment 2
Ammonium molybdate 500g is set enter in Muffle furnace on the enamel evaporating dish of 500ml 600 DEG C calcination 3 hours at molybdenum oxide.
Taking out calcination, good molybdenum oxide enters in the glass beaker of 2000ml, is added 65% nitric acid dousing of 300ml 5 hours.
Incline nitric acid, is washed with distilled water, and drains.
Crystallization is concentrated under reduced pressure in the molybdenum oxide ammonia solvent drained.
Crystallization evaporating dish enter in Muffle furnace 600 DEG C calcination 3 hours at molybdenum oxide.Yield 73.2%, content 99.6%.
Impurity content: silver (Ag) 0.00005%；Arsenic (As) 0.0005%；Barium (Ba) 0.0005%；Copper (Cu)
0.0001%；Iron (Fe) 0.0001%；Magnesium (Mg) 0.0001%；Manganese (Mn) 0.00005%；Nickel (Ni) 0.00005%；Lead (Pb)
0.0001%；Zinc (Zn) 0.0001%.
Embodiment 3
Ammonium molybdate 500g is set enter in Muffle furnace on the enamel evaporating dish of 500ml 700 DEG C calcination 3 hours at molybdenum oxide.
Taking out calcination, good molybdenum oxide enters in the glass beaker of 2000ml, is added 65% nitric acid dousing of 300ml 5 hours.
Incline nitric acid, is washed with distilled water, and drains.
Crystallization is concentrated under reduced pressure in the molybdenum oxide ammonia solvent drained.
Crystallization evaporating dish enter in Muffle furnace 700 DEG C calcination 3 hours at molybdenum oxide.Yield 74.1%, content 99.8%.
Impurity content: silver (Ag) 0.00005%；Arsenic (As) 0.0005%；Barium (Ba) 0.0005%；Copper (Cu)
0.0001%；Iron (Fe) 0.0001%；Magnesium (Mg) 0.0001%；Manganese (Mn) 0.00005%；Nickel (Ni) 0.00005%；Lead (Pb)
0.0001%；Zinc (Zn) 0.0001%.
Comparative example 1
The difference of this comparative example and embodiment 1 is only that the temperature of 2 calcinations is 800 DEG C, three oxidations being prepared
The yield 70.1% of molybdenum, content 98.4%.
Impurity content: silver (Ag) 0.00005%；Arsenic (As) 0.0005%；Barium (Ba) 0.0005%；Copper (Cu)
0.0001%；Iron (Fe) 0.0001%；Magnesium (Mg) 0.0001%；Manganese (Mn) 0.00005%；Nickel (Ni) 0.00005%；Lead (Pb)
0.0001%；Zinc (Zn) 0.0001%.
Comparative example 2
The difference of this comparative example and embodiment 1 is only that the temperature of 2 calcinations is 500 DEG C, three oxidations being prepared
The yield 73.1% of molybdenum, content 97.5%.
Impurity content: silver (Ag) 0.00005%；Arsenic (As) 0.0005%；Barium (Ba) 0.0005%；Copper (Cu)
0.0001%；Iron (Fe) 0.0001%；Magnesium (Mg) 0.0001%；Manganese (Mn) 0.00005%；Nickel (Ni) 0.00005%；Lead (Pb)
0.0001%；Zinc (Zn) 0.0001%.
In conclusion only presently preferred embodiments of the present invention, is not used to limit the scope of implementation of the present invention, it is all according to
Equivalent changes and modifications carried out by shape described in scope of the invention as claimed, construction, feature and spirit should be included in this
In the scope of the claims of invention.
Claims (3)
1. a kind of preparation method of high-purity molybdenum trioxide, which comprises the steps of:
After ammonium molybdate is carried out calcination at 600~700 DEG C, molybdenum trioxide crude product is obtained；
The molybdenum trioxide crude product is added in nitric acid solution, is filtered after dissolution, filter residue is collected；
The filter residue is added in ammonium hydroxide, is concentrated after dissolution, obtains concentrate；
After concentrate drying, calcination is carried out at 600~700 DEG C, obtains the high-purity molybdenum trioxide.
2. the preparation method of high-purity molybdenum trioxide as described in claim 1, which is characterized in that the calcination temperature be 600~
700℃。
3. the preparation method of high-purity molybdenum trioxide as described in claim 1, which is characterized in that the method for the concentration is decompression
Distillation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811587964.5A CN109574076A (en) | 2018-12-25 | 2018-12-25 | A kind of preparation method of high-purity molybdenum trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811587964.5A CN109574076A (en) | 2018-12-25 | 2018-12-25 | A kind of preparation method of high-purity molybdenum trioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109574076A true CN109574076A (en) | 2019-04-05 |
Family
ID=65931650
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811587964.5A Pending CN109574076A (en) | 2018-12-25 | 2018-12-25 | A kind of preparation method of high-purity molybdenum trioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109574076A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4555386A (en) * | 1984-02-29 | 1985-11-26 | Gte Products Corporation | Process for purifying molybdenum trioxide |
| US4612172A (en) * | 1985-02-22 | 1986-09-16 | Gte Products Corporation | Purification of molybdenum |
| JP2011184282A (en) * | 2010-02-10 | 2011-09-22 | Dowa Eco-System Co Ltd | Method for producing aqueous solution of molybdic acid and method for purifying molybdenum trioxide |
| CN103663561A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Recycling method of molybdenum in filament-melting waste acid |
| CN104651637A (en) * | 2013-11-18 | 2015-05-27 | 徐丽萍 | High-purity molybdenum trioxide processing technology |
| CN107364889A (en) * | 2017-09-19 | 2017-11-21 | 芜湖人本合金有限责任公司 | High-purity molybdenum trioxide and preparation method thereof |
| CN107381642A (en) * | 2017-09-19 | 2017-11-24 | 芜湖人本合金有限责任公司 | High-purity molybdenum trioxide and preparation method thereof |
-
2018
- 2018-12-25 CN CN201811587964.5A patent/CN109574076A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4555386A (en) * | 1984-02-29 | 1985-11-26 | Gte Products Corporation | Process for purifying molybdenum trioxide |
| US4612172A (en) * | 1985-02-22 | 1986-09-16 | Gte Products Corporation | Purification of molybdenum |
| JP2011184282A (en) * | 2010-02-10 | 2011-09-22 | Dowa Eco-System Co Ltd | Method for producing aqueous solution of molybdic acid and method for purifying molybdenum trioxide |
| CN103663561A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工股份有限公司 | Recycling method of molybdenum in filament-melting waste acid |
| CN104651637A (en) * | 2013-11-18 | 2015-05-27 | 徐丽萍 | High-purity molybdenum trioxide processing technology |
| CN107364889A (en) * | 2017-09-19 | 2017-11-21 | 芜湖人本合金有限责任公司 | High-purity molybdenum trioxide and preparation method thereof |
| CN107381642A (en) * | 2017-09-19 | 2017-11-24 | 芜湖人本合金有限责任公司 | High-purity molybdenum trioxide and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113444885B (en) | Method for preferentially extracting metal lithium from waste ternary lithium ion battery and simultaneously obtaining battery-grade metal salt | |
| JP6336469B2 (en) | Method for producing scandium-containing solid material with high scandium content | |
| CN105776333A (en) | Preparation method of vanadium pentoxide | |
| Peng et al. | Vanadium properties, toxicity, mineral sources and extraction methods: a review | |
| CN102295308A (en) | Method for preparing zinc oxide by using zinc-containing waste liquid as raw material | |
| CN103055883A (en) | Supported nickel-based catalyst and its preparation method and use | |
| CN109336177B (en) | Method for cleanly producing high-purity vanadium pentoxide by using hydrogen peroxide and ammonia water | |
| CN107541599A (en) | Use the preparation method of acid high manganese high purity containing vanadium leachate vanadium | |
| CN1162330C (en) | Clean production method of potassium chromate | |
| CN113774220B (en) | Method for recovering molybdenum, bismuth and vanadium from waste catalysts of acrylic acid and methacrylic acid and esters thereof | |
| CN114085999A (en) | Method for recovering valuable metals from lithium battery anode leaching waste liquid | |
| CN106830077B (en) | A kind of method of vanadic anhydride purification | |
| CN111333112B (en) | Preparation of Cr (V) chromium salt calcium chromate Ca 5 (CrO 4 ) 3 O 0.5 Is a method of (2) | |
| CN103302299A (en) | Preparation method of high-purity tungsten powder for large-scale integrated circuit | |
| CN109574076A (en) | A kind of preparation method of high-purity molybdenum trioxide | |
| CN110760689B (en) | Method for removing iron in precious metal rhodium recovery process | |
| WO2020138137A1 (en) | Method for purifying vanadium oxide | |
| CN111778404A (en) | Leaching separation method of nickel-cobalt-molybdenum-phosphorus-vanadium alloy material | |
| CN114934169B (en) | Method for recycling tungsten-containing waste | |
| CN111392778A (en) | Method for deeply purifying and removing potassium from ammonium perrhenate solution | |
| KR101574847B1 (en) | Lithium-manganese complex oxides, lithium-manganese adsorption precursor and method for preparing the same, and lithium adsorbent using the same | |
| CN113041988B (en) | Titanium lithium ion sieve and preparation method and application thereof | |
| KR100277503B1 (en) | Separation and recovery of nickel, vanadium and molybdenum from petroleum desulfurization spent catalyst | |
| CN104831067A (en) | Method for separating and recovering arsenic from metallurgical material acid leaching liquid | |
| CN113479938A (en) | Method for preparing high-purity iron oxide by using iron oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190405 |
|
| WD01 | Invention patent application deemed withdrawn after publication |