CN103952534A - Method for preparing sodium molybdate from nickel-molybdenum ore - Google Patents
Method for preparing sodium molybdate from nickel-molybdenum ore Download PDFInfo
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Abstract
The invention relates to a method for preparing sodium molybdate from nickel-molybdenum ore and belongs to the technical field of non-ferrous metallurgy. The method comprises the following steps of a, crushing nickel-molybdenum ore and carrying out oxidizing roasting for decomposition desulfurization to obtain a roasted product, b, mixing the roasted product and a sodium-modification agent to obtain a uniform mixture, carrying out sodium-modification roasting to obtain a sodium-modified material, adding water into the sodium-modified material to immerse it, and carrying out filtration to respectively obtain a sodium molybdate solution and water-insoluble nickel slag, c, adding an impurity removal agent into the sodium molybdate solution, carrying out purification impurity-removal, adding an acid into the purified sodium molybdate solution, and carrying out filtration to respectively obtain molybdate precipitates and a filtrate, d, dissolving the molybdate precipitates in a sodium hydroxide solution and carrying out filtration to obtain a pure sodium molybdate solution, and e, concentrating the pure sodium molybdate solution until concentrate specific gravity is 1.4-1.6g/cm<3>, carrying out crystallization and carrying out filtration and drying. The method has a low cost and does not pollute the environment. The sodium molybdate obtained by the method satisfies the HG3-1087-77 sodium molybdate first-order product standards.
Description
Technical field
The invention belongs to the technical field of nonferrous metallurgy, be specifically related to a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate.
Background technology
Existing Sodium orthomolybdate production technology all adopts wet processing to produce, mainly with the ammonium molybdate slag that gives up, industrial molybdenum trioxide, non-standard molybdic oxide, useless molybdenum material and useless molybdenum catalyst, produce, prepared by external main pure molybdic oxide or the industrial molybdenum trioxide hydrochloric acid decomposition method of adopting.
1, useless ammonium molybdate slag is the ammonia leached mud of industrial molybdenum trioxide, and it is low containing molybdenum, through adding alkali sodium roasting, molybdenum is changed into water soluble Sodium orthomolybdate, through water-soluble sodium molybdate solution, reconcentration crystallization, filtration, dry to obtain Sodium orthomolybdate product, it is second-rate, price is also low.
2, with sodium hydroxide solution dissolving industrial molybdenum trioxide or non-standard molybdic oxide, obtain sodium molybdate solution, through condensing crystal, produce Sodium orthomolybdate product, its quality is better than the Sodium orthomolybdate that 1 method is produced.
3, in production of molybdic ammonium, the heavy mother liquor of acid, also can output Sodium orthomolybdate product through dissolution of sodium hydroxide, concentrated, crystallization through the molybdic acid of the heavy output of quadratic acid, and its quality is better than the first two and plants Sodium orthomolybdate.
4, the molybdenum waste material such as useless molybdenum powder obtains molybdic oxide through subliming method, then dissolves, purifies with sodium hydroxide solution, and through condensing crystal, dewatered drying obtains Sodium orthomolybdate product.
In the above-mentioned method of preparing Sodium orthomolybdate, all exist the shortcomings such as contaminate environment, tooling cost height.
Be showed no the Technology of producing Sodium orthomolybdate with nickel-molybdenum ore both at home and abroad.
Summary of the invention
The object of this invention is to provide a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate, tooling cost is low, does not pollute the environment, and gained Sodium orthomolybdate is superior in quality.
The technical solution used in the present invention is a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate, and the method comprises the following steps:
A, nickel-molybdenum ore is pulverized after, desulfurization is decomposed in oxidizing roasting, obtains calcining; Particularly preferred, the granularity that nickel-molybdenum ore is pulverized is 200 orders.
B, described calcining and sodium agent are mixed after, carry out sodium roasting, obtain sodium material, then soak described sodium material, filter, obtain respectively sodium molybdate solution and water-fast nickel slag; Wherein, when calcining mixes with sodium agent, the add-on of sodium agent is 20%～60% of calcining weight.
C, described sodium molybdate solution is added after cleaner purification and impurity removal, add acid, filter, obtain respectively precipitate molybdic acid thing and filtrate; Wherein, while adding cleaner purification and impurity removal, the add-on of cleaner adds 5～15kg to carry out by the sodium molybdate solution of every cubic metre; Add sour amount to add the acid of 0.5～2 part of weight to carry out by the weight that often obtains 1 part of described precipitate molybdic acid thing.
D, described precipitate molybdic acid thing dissolve with sodium hydroxide solution, filter, and obtain pure sodium molybdate solution;
E, described pure sodium molybdate solution is concentrated, to the proportion of concentrated solution be 1.4～1.6g/cm
3, crystallization, filtration drying, obtains.
Preferably, in described step a, the temperature of oxidizing roasting is 550 ℃～850 ℃, and the time of oxidizing roasting is 1～7 hour.Particularly preferred, the temperature of oxidizing roasting is 600 ℃, 650 ℃, 700 ℃, 750 ℃ and 800 ℃; The time of oxidizing roasting is 2 hours, 3 hours, 4 hours, 5 hours and 6 hours.
Preferably, in described step b, sodium agent is selected from a kind of in sodium carbonate or sodium bicarbonate or their mixture.Particularly preferred, when sodium agent adopts the mixture of sodium carbonate and sodium bicarbonate, by weight, sodium carbonate: sodium bicarbonate is 35:10.
Preferably, in described step b, the temperature of sodium roasting is 550 ℃～750 ℃, and the time of sodium roasting is 2～7 hours, and sodium roasting adopts rotary kiln or reverberatory furnace to carry out.Particularly preferred, the temperature of sodium roasting is 600 ℃, 650 ℃ and 700 ℃; The time of sodium roasting is 3 hours, 4 hours, 5 hours and 6 hours.
Preferably, in described step b, the weight ratio of water and sodium material is 2.5～3:1, and the temperature of immersion is 20 ℃～60 ℃, and the time of immersion is 2～4 hours.Particularly preferred, the temperature of immersion is 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃ and 55 ℃; The time of soaking is 3 hours.
Preferably, in described step c, cleaner is selected from a kind of in the mixture of magnesium chloride or magnesium chloride and ammonium chloride.Particularly preferred, when cleaner is selected from the mixture of magnesium chloride and ammonium chloride, by weight, magnesium chloride: ammonium chloride is 5～9:2～6.Particularly preferred, when cleaner is selected from the mixture of magnesium chloride and ammonium chloride, by weight, magnesium chloride: ammonium chloride is 2:1.
Preferably, in described step c, acid is selected from a kind of in hydrochloric acid, nitric acid.
Preferably, in described steps d, the weight ratio of precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2.
Preferably, in described step e, concentrated temperature is 90 ℃～100 ℃, and dry temperature is 80 ℃～85 ℃, time of drying >=3 hour.Particularly preferred, concentrated temperature is 95 ℃, and the dry time is 4 hours, 5 hours, 6 hours and 7 hours.
The present invention also provides a kind of described method of preparing Sodium orthomolybdate utilizing nickel-molybdenum ore to prepare the application in Sodium orthomolybdate.
Beneficial effect of the present invention is: the Sodium orthomolybdate that (1) utilizes the inventive method to prepare, meet < < HG3-1087-77 > > Sodium orthomolybdate first class product standard, can obtain 98% or 93% the industrial sulphuric acid product that meets < < GB/T534-2002 > > industrial sulphuric acid standard.(2) preparation method of the present invention, pollution-free generation, production cost is low.(3) can make the molybdenum in nickel-molybdenum ore effectively separated with nickel, and the rate of recovery of nickel and molybdenum is high.(4) compare with the existing technology of preparing Sodium orthomolybdate, there is better economic benefit and social benefit.
Embodiment
For making those skilled in the art understand in detail production technique of the present invention and technique effect, with concrete production instance, further introduce application of the present invention and technique effect below.
Embodiment 1:
A, will be containing molybdenum 4.5%, nickel 3.2%, the nickel-molybdenum ore of carbon 9% and sulphur 22% is crushed to after 200 orders, the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 4 that to be placed in temperature and to be 750 ℃, base pressure be 1000mmHg, the calcining that must be 2.5% containing S and containing SO
2concentration is 9% furnace gas; Furnace gas is adopted contact process to make to meet to the industrial sulphuric acid of GB, the tail gas discharging after relieving haperacidity meets Environmental-protection comprehensive emission standard < < GB26132-2010 > >, does not pollute the environment.
B, described calcining and sodium carbonate are mixed, the add-on of this sodium carbonate is 40% of calcining weight, the rotary kiln that is placed in temperature and is 550 ℃ carries out sodium roasting 7 hours, obtains sodium material, then by weight, water: the amount that sodium material is 2.5:1, soak described sodium material, the temperature of immersion is 20 ℃, and soak time is 4 hours, filter, obtain respectively sodium molybdate solution and water-fast nickel slag;
C, described sodium molybdate solution is added to magnesium chloride purification and impurity removal, the add-on of this magnesium chloride adds 7kg to carry out by the amount of every cubic metre of sodium molybdate solution, add hydrochloric acid, the precipitate molybdic acid thing that the add-on of this hydrochloric acid obtains 1 part of weight by every precipitation adds the hydrochloric acid of 1.5 parts of weight to carry out, filter, obtain respectively precipitate molybdic acid thing and filtrate;
D, described precipitate molybdic acid thing dissolve with sodium hydroxide solution, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, and obtain pure sodium molybdate solution;
E, described pure sodium molybdate solution is concentrated, concentrated temperature is 95 ℃, to the proportion of concentrated solution be 1.5g/cm
3, crystallization, filters, and under the condition of 80 ℃, is dried 3 hours, obtains Sodium orthomolybdate finished product.
Embodiment 2:
A, will be containing molybdenum 4%, nickel 3%, the nickel-molybdenum ore of carbon 12% and sulphur 20% is crushed to after 200 orders, the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 5 that to be placed in temperature and to be 800 ℃, base pressure be 1100mmHg, the calcining that must be 3% containing S and containing SO
2concentration is 8% furnace gas; Furnace gas is adopted contact process to make to meet to the industrial sulphuric acid of GB, the tail gas discharging after relieving haperacidity meets Environmental-protection comprehensive emission standard < < GB26132-2010 > >, does not pollute the environment.
B, described calcining and sodium bicarbonate are mixed, the add-on of this sodium bicarbonate is 20% of calcining weight, the rotary kiln that is placed in temperature and is 650 ℃ carries out sodium roasting 3 hours, obtains sodium material, then by weight, water: the amount that sodium material is 3:1, soak described sodium material, the temperature of immersion is 35 ℃, and soak time is 3 hours, filter, obtain respectively sodium molybdate solution and water-fast nickel slag;
C, described sodium molybdate solution is added to the mixture purification and impurity removal of magnesium chloride and ammonium chloride, the add-on of the mixture of this magnesium chloride and ammonium chloride adds 15kg to carry out by the amount of every cubic metre of sodium molybdate solution, wherein, by weight, magnesium chloride: ammonium chloride is 4:2, adds subsequently hydrochloric acid, the precipitate molybdic acid thing that the add-on of this hydrochloric acid obtains 1 part of weight by every precipitation adds the hydrochloric acid of 1 part of weight to carry out, filter, obtain respectively precipitate molybdic acid thing and filtrate;
D, described precipitate molybdic acid thing dissolve with sodium hydroxide solution, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, and obtain pure sodium molybdate solution;
E, described pure sodium molybdate solution is concentrated, concentrated temperature is 90 ℃, to the proportion of concentrated solution be 1.4g/cm
3, crystallization, filters, and under the condition of 82 ℃, is dried 5 hours, obtains Sodium orthomolybdate finished product.
Embodiment 3:
A, will be containing molybdenum 4.5%, nickel 3.2%, the nickel-molybdenum ore of carbon 12% and sulphur 22% is crushed to after 200 orders, the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 7 that to be placed in temperature and to be 550 ℃, base pressure be 1000mmHg, the calcining that must be 2.3% containing S and containing SO
2concentration is 10% furnace gas; Furnace gas is adopted contact process to make to meet to the industrial sulphuric acid of GB, the tail gas discharging after relieving haperacidity meets Environmental-protection comprehensive emission standard < < GB26132-2010 > >, does not pollute the environment.
B, described calcining and sodium agent are mixed, the add-on of this sodium agent is 60% of calcining weight, and its sodium agent adopts the mixture of sodium carbonate and sodium bicarbonate, by weight, and sodium carbonate: sodium bicarbonate is 35:10.Then the rotary kiln that is placed in temperature and is 850 ℃ carries out sodium roasting 1 hour, obtain sodium material, then by weight, water: the amount that sodium material is 2.8:1, soak described sodium material, the temperature of immersion is 60 ℃, and soak time is 4 hours, filter, obtain respectively sodium molybdate solution and water-fast nickel slag;
C, described sodium molybdate solution is added to the mixture purification and impurity removal of magnesium chloride and ammonium chloride, the add-on of the mixture of this magnesium chloride and ammonium chloride adds 12kg to carry out by the amount of every cubic metre of sodium molybdate solution, wherein, by weight, magnesium chloride: ammonium chloride is 5:6, adds subsequently nitric acid, the precipitate molybdic acid thing that the add-on of this nitric acid obtains 1 part of weight by every precipitation adds the nitric acid of 2 parts of weight to carry out, filter, obtain respectively precipitate molybdic acid thing and filtrate;
D, described precipitate molybdic acid thing dissolve with sodium hydroxide solution, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, and obtain pure sodium molybdate solution;
E, described pure sodium molybdate solution is concentrated, concentrated temperature is 100 ℃, to the proportion of concentrated solution be 1.6g/cm
3, crystallization, filters, and under the condition of 85 ℃, is dried 4 hours, obtains Sodium orthomolybdate finished product.
Embodiment 4:
A, will be containing molybdenum 4.2%, nickel 3.6%, the nickel-molybdenum ore of carbon 12% and sulphur 20% is crushed to after 200 orders, the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 5 that to be placed in temperature and to be 800 ℃, base pressure be 1100mmHg, the calcining that must be 3.4% containing S and containing SO
2concentration is 8.2% furnace gas; Furnace gas is adopted contact process to make to meet to the industrial sulphuric acid of GB, the tail gas discharging after relieving haperacidity meets Environmental-protection comprehensive emission standard < < GB26132-2010 > >, does not pollute the environment.
B, described calcining and sodium bicarbonate are mixed, the add-on of this sodium bicarbonate is 30% of calcining weight, the rotary kiln that is placed in temperature and is 650 ℃ carries out sodium roasting 3 hours, obtains sodium material, then by weight, water: the amount that sodium material is 2.8:1, soak described sodium material, the temperature of immersion is 40 ℃, and soak time is 4 hours, filter, obtain respectively sodium molybdate solution and water-fast nickel slag;
C, described sodium molybdate solution is added to the mixture purification and impurity removal of magnesium chloride and ammonium chloride, the add-on of the mixture of this magnesium chloride and ammonium chloride adds 5kg to carry out by the amount of every cubic metre of sodium molybdate solution, wherein, by weight, magnesium chloride: ammonium chloride is 9:2, adds subsequently hydrochloric acid, the precipitate molybdic acid thing that the add-on of this hydrochloric acid obtains 1 part of weight by every precipitation adds the hydrochloric acid of 1 part of weight to carry out, filter, obtain respectively precipitate molybdic acid thing and filtrate;
D, described precipitate molybdic acid thing dissolve with sodium hydroxide solution, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, and obtain pure sodium molybdate solution;
E, described pure sodium molybdate solution is concentrated, concentrated temperature is 95 ℃, to the proportion of concentrated solution be 1.4g/cm
3, crystallization, filters, and under the condition of 82 ℃, is dried 6 hours, obtains Sodium orthomolybdate finished product.
The invention described above embodiment gained Sodium orthomolybdate, all meet < < HG3-1087-77 > > Sodium orthomolybdate first class product standard, and it is effective separated to make molybdenum in nickel-molybdenum ore and nickel obtain, and the rate of recovery of nickel and molybdenum is high.Wherein, the rate of recovery of nickel is respectively 89%, 88%, 86% and 91%; The rate of recovery of molybdenum is respectively: 86%, 87%, 89% and 84%.
Finally it should be noted that, above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to above-described embodiment, those skilled in the art are to be understood that, still can modify or be equal to replacement the present invention, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (10)
1. utilize nickel-molybdenum ore to prepare a method for Sodium orthomolybdate, it is characterized in that: the method comprises the following steps:
A, nickel-molybdenum ore is pulverized after, desulfurization is decomposed in oxidizing roasting, obtains calcining;
B, described calcining and sodium agent are mixed after, carry out sodium roasting, obtain sodium material, then soak described sodium material, filter, obtain respectively sodium molybdate solution and water-fast nickel slag;
C, described sodium molybdate solution is added after cleaner purification and impurity removal, add acid, filter, obtain respectively precipitate molybdic acid thing and filtrate;
D, described precipitate molybdic acid thing dissolve with sodium hydroxide solution, filter, and obtain pure sodium molybdate solution;
E, described pure sodium molybdate solution is concentrated, to the proportion of concentrated solution be 1.4～1.6g/cm
3, crystallization, filtration drying, obtains.
2. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step a, the temperature of oxidizing roasting is 550 ℃～850 ℃, and the time of oxidizing roasting is 1～7 hour.
3. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step b, sodium agent is selected from a kind of in sodium carbonate or sodium bicarbonate or their mixture.
4. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, it is characterized in that: in described step b, the temperature of sodium roasting is 550 ℃～750 ℃, the time of sodium roasting is 2～7 hours, and sodium roasting adopts rotary kiln or reverberatory furnace to carry out.
5. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step b, the weight ratio of water and sodium material is 2.5～3:1, and the temperature of immersion is 20 ℃～60 ℃, and the time of immersion is 2～4 hours.
6. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step c, cleaner is selected from a kind of in the mixture of magnesium chloride or magnesium chloride and ammonium chloride.
7. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step c, acid is selected from a kind of in hydrochloric acid, nitric acid.
8. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described steps d, the weight ratio of precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2.
9. a kind of method of utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step e, concentrated temperature is 90 ℃～100 ℃, and dry temperature is 80 ℃～85 ℃, time of drying >=3 hour.
10. the method based on preparing Sodium orthomolybdate described in any one in claim 1-9 is utilizing nickel-molybdenum ore to prepare the application in Sodium orthomolybdate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104445411A (en) * | 2014-12-23 | 2015-03-25 | 金堆城钼业股份有限公司 | Preparation method of large granular molybdic acid |
| CN107585789A (en) * | 2017-09-26 | 2018-01-16 | 河南科技大学 | A kind of method that high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concntrate |
| CN112875753A (en) * | 2021-03-22 | 2021-06-01 | 天津四方化工有限公司 | Preparation method of low-sodium low-ammonium high-purity molybdic acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445411A (en) * | 2014-12-23 | 2015-03-25 | 金堆城钼业股份有限公司 | Preparation method of large granular molybdic acid |
| CN104445411B (en) * | 2014-12-23 | 2016-04-20 | 金堆城钼业股份有限公司 | A kind of preparation method of macrobead molybdic acid |
| CN107585789A (en) * | 2017-09-26 | 2018-01-16 | 河南科技大学 | A kind of method that high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concntrate |
| CN107585789B (en) * | 2017-09-26 | 2019-08-23 | 河南科技大学 | A method of high-purity molybdenum trioxide is prepared using hydrometallurgy molybdenum concentrate |
| CN112875753A (en) * | 2021-03-22 | 2021-06-01 | 天津四方化工有限公司 | Preparation method of low-sodium low-ammonium high-purity molybdic acid |
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| CN103952534B (en) | 2016-03-16 |
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