CN1850623A - Method for producing ammonium molybdate from high-impurity ferro-molybdenum - Google Patents
Method for producing ammonium molybdate from high-impurity ferro-molybdenum Download PDFInfo
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- CN1850623A CN1850623A CN 200610031634 CN200610031634A CN1850623A CN 1850623 A CN1850623 A CN 1850623A CN 200610031634 CN200610031634 CN 200610031634 CN 200610031634 A CN200610031634 A CN 200610031634A CN 1850623 A CN1850623 A CN 1850623A
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- ammonium molybdate
- molybdenum
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Abstract
The invention is a method for producing ammonium molybdate with high- impurity content Mo-Fe alloy, comprising the processes of: mechanically activating and calcining high-impurity content Mo-Fe alloy and sodium carbonate, adding water into calcine, blending and leaching, adding inorganic acid into leachate to regulate pH value, exchanging Mo with weak-base anion-exchange resin, placing ammonium molybdate solution still and depositing V, purifying with MgCl2 to remove P, As and Si by MgCl2, making deep V removing with strong-base anion-exchange resin, crystallizing ammonium molybdate, etc. And its advantages lie in that: the process has strong adaptability the ammonium molybdate has good quality, Mo recovery is high, total yield of the process can reach above 90%, and the ammonium molybdate quality can reach above second-grade national standard.
Description
Technical field the present invention relates to a kind of particularly carbon containing nickel-molybdenum ore method of smelting the producing ammonium molybdate from high-impurity ferro-molybdenum obtain of high impurity ferro-molybdenum of utilizing.
Background technology carbon containing nickel-molybdenum ore difficulty is selected difficult smelting, after this ore deposit exploits out, adopts electric furnace to be smelt high impurity ferro-molybdenum mostly, and its typical chemical ingredients is: Mo 10～20%, and Fe 55～70%, and Ni 4.5～10%, and P 4.5～6%, SiO
210～15%, V
2O
50.5～3%, As 0.3～1%.Ferro-molybdenum is mainly used in steel industry, but the ferro-molybdenum that is used for steel industry has strict restriction to the content of impurity such as P.Therefore, high impurity ferro-molybdenum has only in advance that impurity such as effective elimination P just can be used for steel industry.Yet the technology that does not have maturation to be suitable at present can be with the impurity removals such as P in the high impurity molybdenum-iron.
The traditional technology that with the brightness concentrated molybdenum ore is the raw material production ammonium molybdate is for producing ammonium molybdate from high-impurity ferro-molybdenum and inapplicable, because high impurity ferro-molybdenum fusing point is low, maturing temperature is controlled under its fusing point and will could incites somebody to action wherein molybdenum oxidation through the repeated multiple times roasting, calcining leaches with ammoniacal liquor, the leaching yield of Mo also only 80～85%, the ammonium molybdate solution that leaching obtains contains impurity such as a large amount of P, As, Si, V, Ni, and the ammonium molybdate quality that does not have the crystallization of strong purification means to obtain is also poor.
Summary of the invention removes the impurity P in the high impurity ferro-molybdenum in order effectively to utilize high impurity ferro-molybdenum, for steel industry provides acceptable material, the invention provides a kind of method of producing ammonium molybdate from high-impurity ferro-molybdenum.
A kind of method of producing ammonium molybdate from high-impurity ferro-molybdenum mainly may further comprise the steps: high impurity ferro-molybdenum and yellow soda ash mechanical activating roasting, calcining add water agitation leach, weak base negative resin ion-exchange molybdenum, ammonium molybdate solution and leave standstill after precipitation, the precipitation liquid magnesium chloride and purify and remove liquid strong base negative resin ion-exchange deeply removing vanadium after P, As, Si, the purification, remove liquid crystallization ammonium molybdate behind the vanadium.But liquid direct evaporation condensing crystal ammonium molybdate also can add hydrochloric acid or nitric acid neutralization precipitation crystallization ammonium molybdate behind the purification and impurity removal.Concrete processing parameter is: Na
2CO
3Extraordinarily go into by 0.5～0.8 of roasting reactive chemistry metering; Grind negative 200 orders of granularity of back material; 450～700 ℃ of maturing temperatures, roasting time 30～60min; Water logging solid-liquid weight ratio 1: 4～8; 45～100 ℃ of extraction temperatures, extraction time 0.5～3h; Leach liquor adds mineral acid (hydrochloric acid, sulfuric acid or nitric acid) adjust pH 2.5～5.0; Feed liquid is by 30～90min duration of contact of weak base (macroporous type or gel-type) negative resin ion exchange column; Negative molybdenum resin ammoniacal liquor (4～8mol/L NH
3) desorb; Resin after the desorb is regenerated with hydrochloric acid (1.2～2.5mol/L HCl); The ammonium molybdate solution room temperature that desorb obtains left standstill precipitation 0.0～2.0 day; Magnesium chloride is extraordinarily gone into by purifying reaction (P, As) stoichiometric 1.0～1.5,40～80 ℃ of insulation 0.5～1h; Purify back liquid and add hydrochloric acid or nitric acid adjust pH 6.0～8.5; Liquid is by 20～100min duration of contact of highly basic (macroporous type or gel-type) negative resin ion exchange column after the acid adjustment; Negative vanadium resin is with 2.0～6.0mol/L HCl solution or 0.2～1mol/L NaOH and 2.0～4.0mol/L NaCl mixing solutions desorption and regeneration; Ammonium molybdate solution can be evaporated to density 1.36～1.40g/cm
3Crystallisation by cooling also can 30～60 ℃ be extraordinarily gone into nitric acid or hydrochloric acid precipitated crystal by 1.0～1.1 of the heavy reactive chemistry metering of acid.
The present invention is with high impurity ferro-molybdenum and the levigate roasting of yellow soda ash mixing, and the molybdenum oxidation gets more thorough, and the leaching yield of molybdenum can reach 95～98%; Weak basic anion exchange resin absorption molybdenum, with the absorption of isopoly-acid root or heteropolyacid velamen, loading capacity reaches 60～130mg/ml to molybdenum in pH value 2.5～5.0, and the ammonium molybdate solution that obtains is metal ion such as iron content nickel not, do not need through ammonium sulfide purification and impurity removal operation, can avoid effectively that sulphur exceeds standard in the product; Increase the magnesium chloride cleaning section, but the P in the effective elimination ammonium molybdate solution, As, Si, the adaptive faculty that this had not only guaranteed quality product but also improved technology; Contain vanadium ammonium molybdate solution through leaving standstill precipitation, ion-exchange deeply removing vanadium, can improve ammonium molybdate product appearance quality and use properties; Ion-exchange is returned ion-exchange absorption molybdenum operation recovery V and Mo wherein except that the vanadium liquid of separating that vanadium obtains, and the total recovery that makes whole technology Mo is more than 90%, and the ammonium molybdate quality of output is more than the GB secondary.
Description of drawings
Fig. 1: producing ammonium molybdate from high-impurity ferro-molybdenum process flow diagram.
Embodiment
Below in conjunction with embodiment, the present invention is further described:
Embodiment 1
It is levigate to negative 200 orders to get 2kg high impurity ferro-molybdenum powder and 1kg anhydrous sodium carbonate mixing, 630 ℃ of roasting 60min of retort furnace, solid-liquid was than 1: 4,85 ℃ are leached 1h, leach liquor adds sour adjust pH 3.5, weak base negative resin (D314) absorption 60min duration of contact, molybdenum stripping liquid room temperature left standstill precipitation 2 days, added MgCl by 1.2 times 60 ℃ that purify the reactive chemistry metering
2Be incubated 1 hour, purify back liquid and add hydrochloric acid adjust pH to 6.5, liquid contacts the 60min deeply removing vanadium with strong base negative resin (D231) after the acid adjustment, except that the 1.05 times 50 ℃ adding nitric acid crystallization ammonium molybdates of liquid behind the vanadium by the heavy reactive chemistry metering of acid.(%) is as follows for the experimental result of producing ammonium molybdate from high-impurity ferro-molybdenum:
| Mo | Fe | Ni | P | As | Si | V | |
| Ferro-molybdenum | 13.90 | 59.63 | 7.69 | 4.37 | 0.56 | 5.31 | 0.95 |
| Leached mud | 0.52 | 51.40 | 6.63 | 0.75 | 0.19 | 1.85 | 0.21 |
| Ammonium molybdate | 58.21 | 0.0005 | 0.0005 | 0.0005 | 0.0001 | 0.0009 | 0.0015 |
Embodiment 2
It is levigate to negative 160 orders to get 2kg high impurity ferro-molybdenum powder and 1.2kg anhydrous sodium carbonate mixing, 600 ℃ of roasting 50min of groom's stove, solid-liquid was than 1: 4,80 ℃ are leached 2h, leach liquor adds sour adjust pH 3.1, weak base negative resin (D332) absorption 60min duration of contact, molybdenum stripping liquid room temperature left standstill precipitation 1.5 days, added MgCl by 1.1 times 60 ℃ that purify the reactive chemistry metering
2Be incubated 0.5 hour, purify back liquid and add hydrochloric acid adjust pH to 6.6, liquid contacts the 60min deeply removing vanadium with strong base negative resin (201 * 7) after the acid adjustment, except that liquid evaporation concentration to density behind the vanadium is 1.39g/cm
3, the crystallisation by cooling ammonium molybdate.(%) is as follows for the experimental result of producing ammonium molybdate from high-impurity ferro-molybdenum:
| Mo | Ni | Fe | V | P | As | Si | |
| Ferro-molybdenum | 21.31 | 9.42 | 54.46 | 1.27 | 5.14 | 0.43 | 5.11 |
| Leached mud | 0.43 | 8.12 | 46.95 | 0.17 | 0.86 | 0.17 | 1.68 |
| Ammonium molybdate | 56.71 | 0.0005 | 0.0005 | 0.0013 | 0.0005 | 0.0005 | 0.0008 |
Embodiment 3
It is levigate to negative 180 orders to get 3kg high impurity ferro-molybdenum powder and 1.2kg anhydrous sodium carbonate mixing, 580 ℃ of roasting 60min of groom's stove, solid-liquid was than 1: 4,90 ℃ are leached 1h, leach liquor adds sour adjust pH 3.5, weak base negative resin (D315) absorption 60min duration of contact adds MgCl by 1.2 times 60 ℃ that purify the reactive chemistry metering
2Be incubated 1 hour, purify back liquid and add hydrochloric acid adjust pH to 6.5, liquid contacts 60min absorption vanadium after the acid adjustment with strong base negative resin (D252), except that the 1.0 times 55 ℃ adding nitric acid crystallization ammonium molybdates of liquid behind the vanadium by the heavy reactive chemistry metering of acid.The experimental result (%) that ferro-molybdenum is produced ammonium molybdate is as follows:
| Mo | Fe | Ni | P | As | Si | V | |
| Ferro-molybdenum | 11.4 | 68.31 | 4.78 | 5.72 | 1.033 | 4.72 | 0.27 |
| Leached mud | 0.41 | 58.38 | 4.09 | 0.81 | 0.35 | 2.36 | 0.15 |
| Ammonium molybdate | 58.41 | 0.0005 | 0.0005 | 0.0005 | 0.0001 | 0.0009 | 0.0015 |
Claims (3)
1, a kind of method of producing ammonium molybdate from high-impurity ferro-molybdenum is characterized in that: comprise that mainly high impurity ferro-molybdenum and yellow soda ash mechanical activating roasting, calcining add water agitation leach, weak base negative resin ion-exchange molybdenum, ammonium molybdate solution and leave standstill after precipitation, the precipitation liquid magnesium chloride and purify and remove liquid strong base negative resin ion-exchange deeply removing vanadium after P, As, Si, the purification, remove liquid crystallization ammonium molybdate behind the vanadium;
Concrete processing parameter is: Na
2CO
3Extraordinarily go into by 0.5～0.8 of roasting reactive chemistry metering, grind negative 200 orders of granularity of back material, 450～700 ℃ of maturing temperatures, roasting time 30～60min;
Water logging solid-liquid weight ratio 1: 4～8,45～100 ℃ of extraction temperatures, extraction time 0.5～3h, leach liquor add mineral acid adjust pH 2.5～5.0;
Feed liquid is born the ammoniacal liquor desorb of molybdenum resin by 30～90min duration of contact of weak base negative resin ion exchange column, the resin regeneration of hydrochloric acid after the desorb, and the ammonium molybdate solution room temperature that desorb obtains left standstill precipitation 0.0～2.0 day;
P, As stoichiometric 1.0～1.5 extraordinarily goes into magnesium chloride in the reaction by purifying, 40～80 ℃ of insulation 0.5～1h; Purify back liquid and add hydrochloric acid or nitric acid adjust pH 6.0～8.5, liquid is by 20～100min duration of contact of strong base negative resin ion exchange column after the acid adjustment; Negative vanadium resin is regenerated with 2.0～6.0mol/L HCl solution stripping; Ammonium molybdate solution transpiration cooling crystallization.
2, method according to claim 1 is characterized in that, the negative also available 0.2～1mol/LNaOH of vanadium resin and 2.0～4.0mol/LNaCl mixing solutions desorption and regeneration.
3, method according to claim 1 is characterized in that, liquid is extraordinarily gone into nitric acid or hydrochloric acid precipitated crystal at 30～60 ℃ by 1.0～1.1 of the heavy reactive chemistry metering of acid behind the purification and impurity removal.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101386922B (en) * | 2008-10-21 | 2010-06-02 | 中南大学 | Method for extracting molybdenum by roasting high impurity sodium carbonate nickel-ferro-molybdenum |
| CN102219260A (en) * | 2010-04-14 | 2011-10-19 | 湖南荣宏钼业材料股份有限公司 | Calcination method for producing ammonium molybdate from high-impurity ferromolybdenum alloy |
| CN102219258A (en) * | 2010-04-14 | 2011-10-19 | 湖南荣宏钼业材料股份有限公司 | Method for extracting molybdenum from waste materials in ammonium molybdate production field |
| CN103060563A (en) * | 2013-01-18 | 2013-04-24 | 成都西顿硬质合金有限公司 | Technology of deep purification and impurity removal of ammonium tungstate or ammonium molybdate solution |
| CN103343244A (en) * | 2013-07-16 | 2013-10-09 | 红河州四通矿产有限责任公司 | Process for separating and purifying molybdenum in low-molybdenum-content tailings |
| CN104894370A (en) * | 2015-05-29 | 2015-09-09 | 河北钢铁股份有限公司承德分公司 | Method for leaching soluble vanadium from roasted vanadic slag by using low-concentration sulfuric acid |
| CN109517988A (en) * | 2018-10-31 | 2019-03-26 | 眉山顺应动力电池材料有限公司 | A kind of leaching novel method for separating of the nickel cobalt (alloy) material of the vanadium containing molybdenum |
| CN110921706A (en) * | 2019-11-22 | 2020-03-27 | 西北矿冶研究院 | Method for preparing ammonium molybdate by using molybdenum-containing catalyst |
| CN111411237A (en) * | 2020-04-29 | 2020-07-14 | 核工业北京化工冶金研究院 | Method for extracting and separating molybdenum in phosphorus-containing sulfuric acid system |
Family Cites Families (4)
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| US4601890A (en) * | 1984-02-29 | 1986-07-22 | Gte Products Corporation | Process for purifying molybdenum trioxide |
| JP2710049B2 (en) * | 1987-12-25 | 1998-02-10 | 株式会社 ジャパンエナジー | Method for producing high-purity ammonium molybdate crystal |
| CN1014698B (en) * | 1988-04-19 | 1991-11-13 | 伍宏培 | Method for producing ammonium molybdate and nickel-ammonium sulphate from molybdenucm-nickel ore |
| CN1191202C (en) * | 2003-07-22 | 2005-03-02 | 株洲硬质合金集团有限公司 | Method for preparing high pure ammonium paramolybdate |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101386922B (en) * | 2008-10-21 | 2010-06-02 | 中南大学 | Method for extracting molybdenum by roasting high impurity sodium carbonate nickel-ferro-molybdenum |
| CN102219260A (en) * | 2010-04-14 | 2011-10-19 | 湖南荣宏钼业材料股份有限公司 | Calcination method for producing ammonium molybdate from high-impurity ferromolybdenum alloy |
| CN102219258A (en) * | 2010-04-14 | 2011-10-19 | 湖南荣宏钼业材料股份有限公司 | Method for extracting molybdenum from waste materials in ammonium molybdate production field |
| CN103060563A (en) * | 2013-01-18 | 2013-04-24 | 成都西顿硬质合金有限公司 | Technology of deep purification and impurity removal of ammonium tungstate or ammonium molybdate solution |
| CN103343244A (en) * | 2013-07-16 | 2013-10-09 | 红河州四通矿产有限责任公司 | Process for separating and purifying molybdenum in low-molybdenum-content tailings |
| CN103343244B (en) * | 2013-07-16 | 2014-11-05 | 红河州四通矿产有限责任公司 | Process for separating and purifying molybdenum in low-molybdenum-content tailings |
| CN104894370A (en) * | 2015-05-29 | 2015-09-09 | 河北钢铁股份有限公司承德分公司 | Method for leaching soluble vanadium from roasted vanadic slag by using low-concentration sulfuric acid |
| CN104894370B (en) * | 2015-05-29 | 2017-07-07 | 河北钢铁股份有限公司承德分公司 | The method for leaching solvable vanadium from roasted vanadic slag with low-concentration sulfuric acid |
| CN109517988A (en) * | 2018-10-31 | 2019-03-26 | 眉山顺应动力电池材料有限公司 | A kind of leaching novel method for separating of the nickel cobalt (alloy) material of the vanadium containing molybdenum |
| CN110921706A (en) * | 2019-11-22 | 2020-03-27 | 西北矿冶研究院 | Method for preparing ammonium molybdate by using molybdenum-containing catalyst |
| CN110921706B (en) * | 2019-11-22 | 2022-07-19 | 西北矿冶研究院 | Method for preparing ammonium molybdate by using molybdenum-containing catalyst |
| CN111411237A (en) * | 2020-04-29 | 2020-07-14 | 核工业北京化工冶金研究院 | Method for extracting and separating molybdenum in phosphorus-containing sulfuric acid system |
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