CN103952534B - A kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate - Google Patents
A kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate, belong to the technical field of nonferrous metallurgy.Its method comprises the following steps: a, by nickel-molybdenum ore pulverize after, oxidizing roasting decompose desulfurization, obtain calcining; B, calcining and sodium agent are mixed after, carry out sodium roasting, obtain sodium material, then soak sodium material, filter, obtain sodium molybdate solution and water-fast nickel slag respectively; C, sodium molybdate solution is added cleaner purification and impurity removal after, add acid, filter, obtain precipitate molybdic acid thing and filtrate respectively; D, precipitate molybdic acid thing sodium hydroxide solution dissolve, and filter, obtain pure sodium molybdate solution; E, concentrated by pure sodium molybdate solution, the proportion to concentrated solution is 1.4 ~ 1.6g/cm
3, crystallization, filtration drying, to obtain final product.The invention has the beneficial effects as follows: can reduce costs, not pollute the environment, gained Sodium orthomolybdate meets the standard of " HG3-1087-77 " Sodium orthomolybdate first class product.
Description
Technical field
The invention belongs to the technical field of nonferrous metallurgy, be specifically related to a kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate.
Background technology
Existing Sodium orthomolybdate production technology all adopts wet processing to produce, mainly produce with useless ammonium molybdate slag, industrial molybdenum trioxide, non-standard molybdic oxide, useless molybdenum material and useless molybdenum catalyst, prepared by external main pure molybdic oxide or the industrial molybdenum trioxide hydrochloric acid decomposition method of adopting.
1, the ammonia leached mud of useless ammonium molybdate slag and industrial molybdenum trioxide, it is low containing molybdenum, through adding alkali sodium roasting, molybdenum is changed into water soluble Sodium orthomolybdate, obtain sodium molybdate solution, reconcentration crystallization, filtration through water-soluble, dry to obtain Sodium orthomolybdate product, it is second-rate, price is also low.
2, obtain sodium molybdate solution with sodium hydroxide solution dissolving industrial molybdenum trioxide or non-standard molybdic oxide, produce Sodium orthomolybdate product through condensing crystal, 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 sinks the molybdic acid of output through quadratic acid, and dissolve through sodium hydroxide, concentrated, crystallization also can output Sodium orthomolybdate product, its quality is better than the first two and plants Sodium orthomolybdate.
4, the molybdenum waste materials such as molybdenum powder that give up obtain molybdic oxide through subliming method, then dissolve with sodium hydroxide solution, purify, and through condensing crystal, dewatered drying obtains Sodium orthomolybdate product.
Above-mentionedly prepare in the method for Sodium orthomolybdate, all there is the shortcomings such as contaminate environment, tooling cost are high.
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 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 utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate, and the method comprises the following steps:
A, by nickel-molybdenum ore pulverize after, oxidizing roasting decompose desulfurization, obtain 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 sodium molybdate solution and water-fast nickel slag respectively; 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 cleaner purification and impurity removal after, add acid, filter, obtain precipitate molybdic acid thing and filtrate respectively; Wherein, when 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; The amount adding acid adds by the weight often obtaining 1 part of described precipitate molybdic acid thing that the acid of 0.5 ~ 2 part of weight carries out.
D, described precipitate molybdic acid thing sodium hydroxide solution dissolve, and filter, obtain pure sodium molybdate solution;
E, concentrated by described pure sodium molybdate solution, the proportion to concentrated solution is 1.4 ~ 1.6g/cm
3, crystallization, filtration drying, to obtain final product.
Preferably, the temperature of oxidizing roasting in described step a is 550 DEG C ~ 850 DEG C, and the time of oxidizing roasting is 1 ~ 7 hour.Particularly preferred, the temperature of oxidizing roasting is 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C and 800 DEG C; 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 DEG C ~ 750 DEG C, 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 DEG C, 650 DEG C and 700 DEG C; 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 DEG C ~ 60 DEG C, and the time of immersion is 2 ~ 4 hours.Particularly preferred, the temperature of immersion is 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C and 55 DEG C; The time of soaking is 3 hours.
Preferably, in described step c, cleaner is selected from the one 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 the one 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, temperature concentrated in described step e is 90 DEG C ~ 100 DEG C, and dry temperature is 80 DEG C ~ 85 DEG C, time of drying >=3 hours.Particularly preferred, concentrated temperature is 95 DEG C, and the dry time is 4 hours, 5 hours, 6 hours and 7 hours.
The present invention also provides a kind of described method preparing Sodium orthomolybdate to prepare application in Sodium orthomolybdate utilizing nickel-molybdenum ore.
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 meet " GB/T534-2002 " industrial sulphuric acid standard 98% or 93% industrial sulphuric acid product.(2) preparation method of the present invention, pollution-free generation, production cost is low.(3) molybdenum in nickel-molybdenum ore can be made effectively to be separated with nickel, and the rate of recovery of nickel and molybdenum is high.(4) compared with the existing technology preparing Sodium orthomolybdate, there is better economic benefit and social benefit.
Embodiment
For making those skilled in the art understand production technique of the present invention and technique effect in detail, introduce application of the present invention and technique effect further with concrete production instance below.
Embodiment 1:
A, will containing molybdenum 4.5%, nickel 3.2%, after the nickel-molybdenum ore of carbon 9% and sulphur 22% is crushed to 200 orders, is placed in the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 4 that temperature is 750 DEG C, base pressure is 1000mmHg, must containing S be 2.5% calcining and containing SO
2concentration is the furnace gas of 9%; Adopt contact process to obtain furnace gas to meet the industrial sulphuric acid of GB, the tail gas discharged after relieving haperacidity meets Environmental-protection comprehensive emission standard " GB26132-2010 ", does not pollute the environment.
B, described calcining and sodium carbonate to be mixed, the add-on of this sodium carbonate is 40% of calcining weight, being placed in temperature is that the rotary kiln of 550 DEG C carries out sodium roasting 7 hours, obtains sodium material, then by weight, water: sodium material is the amount of 2.5:1, soak described sodium material, the temperature of immersion is 20 DEG C, and soak time is 4 hours, filter, obtain sodium molybdate solution and water-fast nickel slag respectively;
C, described sodium molybdate solution is added 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 hydrochloric acid that the add-on of this hydrochloric acid adds 1.5 parts of weight by the precipitate molybdic acid thing that every precipitation obtains 1 part of weight carries out, filter, obtain precipitate molybdic acid thing and filtrate respectively;
D, described precipitate molybdic acid thing sodium hydroxide solution dissolve, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, obtain pure sodium molybdate solution;
E, concentrated by described pure sodium molybdate solution, concentrated temperature is 95 DEG C, and the proportion to concentrated solution is 1.5g/cm
3, crystallization, filters, and under the condition of 80 DEG C, drying 3 hours, obtains Sodium orthomolybdate finished product.
Embodiment 2:
A, will containing molybdenum 4%, nickel 3%, after the nickel-molybdenum ore of carbon 12% and sulphur 20% is crushed to 200 orders, is placed in the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 5 that temperature is 800 DEG C, base pressure is 1100mmHg, must containing S be 3% calcining and containing SO
2concentration is the furnace gas of 8%; Adopt contact process to obtain furnace gas to meet the industrial sulphuric acid of GB, the tail gas discharged after relieving haperacidity meets Environmental-protection comprehensive emission standard " GB26132-2010 ", does not pollute the environment.
B, described calcining and sodium bicarbonate to be mixed, the add-on of this sodium bicarbonate is 20% of calcining weight, being placed in temperature is that the rotary kiln of 650 DEG C carries out sodium roasting 3 hours, obtains sodium material, then by weight, water: sodium material is the amount of 3:1, soak described sodium material, the temperature of immersion is 35 DEG C, and soak time is 3 hours, filter, obtain sodium molybdate solution and water-fast nickel slag respectively;
C, described sodium molybdate solution is added 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 hydrochloric acid subsequently, the hydrochloric acid that the add-on of this hydrochloric acid adds 1 part of weight by the precipitate molybdic acid thing that every precipitation obtains 1 part of weight carries out, filter, obtain precipitate molybdic acid thing and filtrate respectively;
D, described precipitate molybdic acid thing sodium hydroxide solution dissolve, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, obtain pure sodium molybdate solution;
E, concentrated by described pure sodium molybdate solution, concentrated temperature is 90 DEG C, and the proportion to concentrated solution is 1.4g/cm
3, crystallization, filters, and under the condition of 82 DEG C, drying 5 hours, obtains Sodium orthomolybdate finished product.
Embodiment 3:
A, will containing molybdenum 4.5%, nickel 3.2%, after the nickel-molybdenum ore of carbon 12% and sulphur 22% is crushed to 200 orders, is placed in the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 7 that temperature is 550 DEG C, base pressure is 1000mmHg, must containing S be 2.3% calcining and containing SO
2concentration is the furnace gas of 10%; Adopt contact process to obtain furnace gas to meet the industrial sulphuric acid of GB, the tail gas discharged 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 being placed in temperature is that the rotary kiln of 850 DEG C carries out sodium roasting 1 hour, obtain sodium material, then by weight, water: sodium material is the amount of 2.8:1, soak described sodium material, the temperature of immersion is 60 DEG C, and soak time is 4 hours, filter, obtain sodium molybdate solution and water-fast nickel slag respectively;
C, described sodium molybdate solution is added 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 nitric acid subsequently, the nitric acid that the add-on of this nitric acid adds 2 parts of weight by the precipitate molybdic acid thing that every precipitation obtains 1 part of weight carries out, filter, obtain precipitate molybdic acid thing and filtrate respectively;
D, described precipitate molybdic acid thing sodium hydroxide solution dissolve, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, obtain pure sodium molybdate solution;
E, concentrated by described pure sodium molybdate solution, concentrated temperature is 100 DEG C, and the proportion to concentrated solution is 1.6g/cm
3, crystallization, filters, and under the condition of 85 DEG C, drying 4 hours, obtains Sodium orthomolybdate finished product.
Embodiment 4:
A, will containing molybdenum 4.2%, nickel 3.6%, after the nickel-molybdenum ore of carbon 12% and sulphur 20% is crushed to 200 orders, is placed in the little time decomposition desulfurization of fluidizing furnace oxidizing roasting 5 that temperature is 800 DEG C, base pressure is 1100mmHg, must containing S be 3.4% calcining and containing SO
2concentration is the furnace gas of 8.2%; Adopt contact process to obtain furnace gas to meet the industrial sulphuric acid of GB, the tail gas discharged after relieving haperacidity meets Environmental-protection comprehensive emission standard " GB26132-2010 ", does not pollute the environment.
B, described calcining and sodium bicarbonate to be mixed, the add-on of this sodium bicarbonate is 30% of calcining weight, being placed in temperature is that the rotary kiln of 650 DEG C carries out sodium roasting 3 hours, obtains sodium material, then by weight, water: sodium material is the amount of 2.8:1, soak described sodium material, the temperature of immersion is 40 DEG C, and soak time is 4 hours, filter, obtain sodium molybdate solution and water-fast nickel slag respectively;
C, described sodium molybdate solution is added 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 hydrochloric acid subsequently, the hydrochloric acid that the add-on of this hydrochloric acid adds 1 part of weight by the precipitate molybdic acid thing that every precipitation obtains 1 part of weight carries out, filter, obtain precipitate molybdic acid thing and filtrate respectively;
D, described precipitate molybdic acid thing sodium hydroxide solution dissolve, and the weight ratio of this precipitate molybdic acid thing and sodium hydroxide solution is 1.5:2, filter, obtain pure sodium molybdate solution;
E, concentrated by described pure sodium molybdate solution, concentrated temperature is 95 DEG C, and the proportion to concentrated solution is 1.4g/cm
3, crystallization, filters, and under the condition of 82 DEG C, drying 6 hours, obtains Sodium orthomolybdate finished product.
The invention described above embodiment gained Sodium orthomolybdate, all meets " HG3-1087-77 " Sodium orthomolybdate first class product standard, and the molybdenum in nickel-molybdenum ore can be made to obtain with nickel be effectively separated, 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 with reference to above-described embodiment to invention has been detailed description, those skilled in the art are to be understood that, still can modify to the present invention or equivalent replacement, and not departing from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in right 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, by nickel-molybdenum ore pulverize after, oxidizing roasting decompose desulfurization, obtain calcining;
B, described calcining and sodium agent are mixed after, carry out sodium roasting, obtain sodium material, then soak described sodium material, filter, obtain sodium molybdate solution and water-fast nickel slag respectively;
C, described sodium molybdate solution is added cleaner purification and impurity removal after, add acid, filter, obtain precipitate molybdic acid thing and filtrate respectively;
D, described precipitate molybdic acid thing sodium hydroxide solution dissolve, and filter, obtain pure sodium molybdate solution;
E, concentrated by described pure sodium molybdate solution, the proportion to concentrated solution is 1.4 ~ 1.6g/cm
3, crystallization, filtration drying, to obtain final product.
2. a kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: the temperature of oxidizing roasting in described step a is 550 DEG C ~ 850 DEG C, and the time of oxidizing roasting is 1 ~ 7 hour.
3. a kind of method 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 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 DEG C ~ 750 DEG C, 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 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 DEG C ~ 60 DEG C, and the time of immersion is 2 ~ 4 hours.
6. a kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step c, cleaner is selected from the one in the mixture of magnesium chloride or magnesium chloride and ammonium chloride.
7. a kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: in described step c, acid is selected from the one in hydrochloric acid, nitric acid.
8. a kind of method 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 utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate according to claim 1, is characterized in that: temperature concentrated in described step e is 90 DEG C ~ 100 DEG C, and dry temperature is 80 DEG C ~ 85 DEG C, time of drying >=3 hours.
10. prepare application in Sodium orthomolybdate based on the method preparing Sodium orthomolybdate according to any one of claim 1-9 utilizing nickel-molybdenum ore for one kind.
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| 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 |
| CN112875753B (en) * | 2021-03-22 | 2022-10-04 | 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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| CN1177012A (en) * | 1997-06-23 | 1998-03-25 | 贵州天星钼镍冶金有限公司 | Process for separation molybdenum and nickel from black shale by sodium carbonate conversion treatment |
| CN103555933A (en) * | 2013-11-18 | 2014-02-05 | 中南大学 | Method for extracting molybdenum and nickel and enriching precious metals from nickel and molybdenum ores |
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| CN1177012A (en) * | 1997-06-23 | 1998-03-25 | 贵州天星钼镍冶金有限公司 | Process for separation molybdenum and nickel from black shale by sodium carbonate conversion treatment |
| CN103555933A (en) * | 2013-11-18 | 2014-02-05 | 中南大学 | Method for extracting molybdenum and nickel and enriching precious metals from nickel and molybdenum ores |
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