CN101205085A - Method for producing secondary ammonium molybdate by molybdenum recovery material - Google Patents
Method for producing secondary ammonium molybdate by molybdenum recovery material Download PDFInfo
- Publication number
- CN101205085A CN101205085A CNA2007101926854A CN200710192685A CN101205085A CN 101205085 A CN101205085 A CN 101205085A CN A2007101926854 A CNA2007101926854 A CN A2007101926854A CN 200710192685 A CN200710192685 A CN 200710192685A CN 101205085 A CN101205085 A CN 101205085A
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- ammonium molybdate
- reclaimed materials
- ammonium
- pure water
- 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
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for producing secondary ammonium molybdate by using recycling material of molybdenum, which includes in turn: sorting and removing sundries; sieving at 40meshes to 100meshes; oxidizing and roasting in 480 DEG C to 550 DEG C for 5 to 8 hours; according to quality percentage of calcine: pure water: ammonia =1(0.7 to 0.9) : (1.2 to 1.4), sufficiently stirring and heating , lixiviating and purifying the calcine, the pure water and the ammonia in 70 DEG C to 80 DEG C; with proportion of ammonium molybdate solution reaching 1.18 g/cm<3>-1.22g/cm<3>, stopping stirring and heating; acid-precipitating supernatant in the temperature of 40 DEG C to 60 DEG C with hydrochloride and controlling solution pH value at 1.5 to 2.5; filtering acid precipitation slurry to obtain multiple ammonium molybdate precipitate and after evaporating and crystallizing, separating, parching, and blending, obtaining the secondary ammonium molybdate conforming with international standard. The invention has high recovery utilization ratio of molybdenum and the produced secondary ammonium molybdate can not be used for preparing molybdenum power as well as preparing products or deeply-processing molybdenum products.
Description
Technical field:
The method that the present invention relates to utilize the reclaimed materials of molybdenum to produce ammonium paramolybdate, especially utilize residual, the inferior powder of molybdenum and gather dust, method that the reclaimed materials such as car cutting base bits of trench, settling bowl material or pressed compact are produced ammonium paramolybdates.
Background technology:
Ammonium molybdate (comprising ammonium dimolybdate, ammonium tetramolybdate, many ammonium molybdates and ammonium paramolybdate etc.) is mainly used in to produce produces metal molybdenum powder, also is commonly used for catalyzer, the chemical reagent of petrochemical complex and produces industrial chemicals etc.Metal molybdenum powder is mainly used in metal productss such as making molybdenum processing material, molybdenum plug, molybdenum plate base, molybdenum bar, molybdenum sheet, molybdenum filament.In the smelting of being engaged in molybdenum is produced, the metal molybdenum powder production process can produce some residual, inferior powder and gather dust, trench, settling bowl material, the metal molybdenum production of articles can produce, and car cutting base inferior, give up pressed compact and a lot of molybdenum bases is considered to be worth doing, the processing of metal molybdenum deep processed product, distillation rolling, that pulling process also can the produce molybdenum material that gathers dust, utilize residual, the inferior powder of these molybdenums and gather dust, the car cutting base bits of trench, settling bowl material or pressed compact etc. produce qualified molybdenum powder again as reclaimed materials, not only save resource, also effectively reduced production cost.Also utilizing the reclaimed materials of molybdenum to prepare ammonium molybdate in the industrial production at present, is the feedstock production molybdenum powder again with the ammonium molybdate.Usually utilize the reclaimed materials of molybdenum to prepare the method for ammonium molybdate, be with the inferior reclaimed materials of molybdenum in nitric acid after the sour molten leaching, through purify, acid is heavy and baking operation.What adopt aforesaid method production is many ammonium molybdates, the molten extraction time of its method acid is quite long, generally need more than 30 days at least, adopt nitric acid having relatively high expectations to equipment and pipeline, not only increased the cost of recycling, and some impurity element of many ammonium molybdates of producing easily exceeds standard, molybdenum powder use properties with these many ammonium molybdate preparations is relatively poor relatively, generally can only be applicable to the common molybdenum product of preparation, as primary products such as molybdenum-iron or steel-making additives, and be not suitable for preparation molybdenum product or deep processed product, as molybdenum plug, molybdenum plate base, molybdenum bar, molybdenum sheet, molybdenum filament etc.
Summary of the invention:
The present invention is directed to above-mentioned deficiency, a kind of method of utilizing the reclaimed materials production ammonium paramolybdate of molybdenum is provided, low for equipment requirements, the production cycle is shorter, the real rate of recovery of the utilization ratio of molybdenum reclaimed materials and molybdenum is higher, reduced production cost effectively, saved the molybdenum resource, the ammonium paramolybdate of producing is up to state standards, not only can be applicable to the preparation of molybdenum powder, also can be applicable to prepare goods or deep processing molybdenum product simultaneously.
For realizing above purpose, the method that the present invention utilizes the reclaimed materials of molybdenum to produce ammonium paramolybdate comprises successively:
(1) select materials, impurities removing;
(2) adopt 40 orders ~ 100 purpose screen clothes that the reclaimed materials powder of molybdenum is sieved;
(3) undersize material is sent in the stoving oven oxidizing roasting 5 ~ 8h under 480 ℃ ~ 550 ℃ temperature;
(4) with the calcining that obtains after the roasting, calcining by mass percentage: pure water: ammoniacal liquor=1: (0.7 ~ 0.9): the ratio of (1.2 ~ 1.4), calcining, pure water, ammoniacal liquor are placed leaching vat, under 70 ℃ ~ 80 ℃, stir, production technique adds sodium sulphite and gac routinely, when ammonium molybdate solution proportion reaches 1.18g/cm
3~ 1.22g/cm
3In time, stop to stir and heating;
(5) treat ammonium molybdate solution clarification after, supernatant liquor is sucked in the enamel acid deep gouge, under 40 ℃ ~ 60 ℃ temperature, control solution pH value is 1.5 ~ 2.5, adopts hydrochloric acid to carry out acid and sinks;
(6) sour jetsam slurry is filtered, the many ammonium molybdates precipitations that obtain change in the crystallizer tank, after carrying out evaporative crystallization, separation, dry, close batch through production technique routinely, obtain meeting the ammonium paramolybdate of GB.
When reclaimed materials is trench material, settling bowl reclaimed materials, to dry before in step (1), step (1) is afterwards, step (2) carries out fragmentation before; When reclaimed materials during for block reclaimed materials such as compacting defect ware, car cutting base bits piece, immersion oil bases, step (1) afterwards, step (2) needs to carry out fragmentation before.
Stoving oven is tubular type retort furnace or reverberatory furnace.
Because the powder particle of reclaimed materials size directly influence roasting effect, therefore reclaimed materials employing fragmentation and 40 orders ~ 100 purpose screen clothes are sieved, reduce powder particle effectively, increased the specific surface area of powder; Control suitable maturing temperature and soaking time simultaneously, make in the roasting process powder oxidizing reaction abundant, both avoided on the low side or time of temperature shortly partially to cause the material oxidizing reaction incomplete, avoid the too high material caking that causes of temperature again, thereby avoided because of abundant oxidation and lumpd seriously causing the molybdenum in the material to be dissolved fully, to leach, improved the leaching effect and the real rate of recovery of molybdenum by ammoniacal liquor.
According to said method, the molybdenum powder that the molybdenum product production process produces and the ground lining of molybdenum oxide, the material that gathers dust, trench sedimentation material, compacting time waste product material, table top material, immersion oil material, the cutting powder of car cutting molybdenum product pressed compact, limit pin briquet, disconnected base, useless base etc. all kinds of inferior, reclaim molybdenum and all can produce ammonium paramolybdate, the molybdenum casting yield in the reclaimed materials reaches more than 94%.
Embodiment:
Embodiment 1: get 1000Kg through molybdenum powder ground, the table top of selecting, rejecting all kinds of foreign material, Powder Recovery material (molybdenum content is 97.4%) such as gather dust, by 40 eye mesh screens, under 480 ℃ ~ 500 ℃ temperature with the speed of 10Kg/h. platform, roasting 5h in many tubular type retort furnaces, press calcining: pure water: ammoniacal liquor=1: 0.8: 1.3, calcining, pure water, ammoniacal liquor are placed leaching vat, abundant mixing under 70 ℃～80 ℃, constantly stirring and heating down, production technique adding sodium sulphite and gac purify routinely, when ammonium molybdate solution proportion reaches 1.18g/cm
3In time, stop to stir and heating, treat after the ammonium molybdate solution clarification supernatant liquor to be sucked in the enamel acid deep gouge, under 40 ℃～60 ℃ temperature, the control pH value is that 1.5～2.5 to adopt hydrochloric acid to carry out acid heavy, and the many ammonium molybdates precipitations after the filtration change in the crystallizer tank, through evaporative crystallization, separation, dry, close criticize after, (molybdenum content is 56% to obtain ammonium paramolybdate, product index is up to state standards, down together) 1648Kg, the molybdenum casting yield is 94.75%.
Embodiment 2: get 1000Kg through selecting, reject the compacting defect ware of all kinds of foreign material, car cutting base bits piece, pressed compact reclaimed materials (molybdenum content is 92.3%) such as immersion oil base, after crusher in crushing, powder is by 80 eye mesh screens, under 480 ℃～510 ℃ temperature with the speed of 6Kg/h. platform, roasting 7h in many tubular type retort furnaces, press calcining: pure water: ammoniacal liquor=1: 0.7: 1.2, with calcining, pure water, ammoniacal liquor places leaching vat, abundant mixing under 70 ℃～80 ℃, constantly stirring and heating down, production technique adding sodium sulphite and gac purify routinely, when ammonium molybdate solution proportion reaches 1.20g/cm
3In time, stop to stir and heating, treat after the ammonium molybdate solution clarification supernatant liquor to be sucked in the enamel acid deep gouge, under 40 ℃～60 ℃ temperature, the control pH value is 1.5～2.5 to adopt hydrochloric acid to carry out acid to sink, many ammonium molybdate precipitations after the filtration change in the crystallizer tank, after evaporative crystallization, separation, drying, close batch, obtain ammonium paramolybdate 1558Kg, the molybdenum casting yield is 94.53%.
Embodiment 3: get 1000Kg through the drying room oven dry, despecking removes all kinds of foreign material, molybdenum powder after the crusher in crushing and molybdenum oxide trench, reclaimed materials such as settling bowl (molybdenum content is 78.8%), powder is by 80 eye mesh screens, under 500 ℃～540 ℃ temperature with the speed of 5Kg/h. platform, roasting 8h in many tubular type retort furnaces, press calcining: pure water: ammoniacal liquor=1: 0.8: 1.2, with calcining, pure water, ammoniacal liquor places leaching vat, abundant mixing under 70 ℃～80 ℃, constantly stirring and heating down, production technique adding sodium sulphite and gac purify routinely, when ammonium molybdate solution proportion reaches 1.22g/cm
3In time, stop to stir and heating, treat after the ammonium molybdate solution clarification supernatant liquor to be sucked in the enamel acid deep gouge, under 40 ℃～60 ℃ temperature, the control pH value is 1.5～2.5 to adopt hydrochloric acid to carry out acid to sink, many ammonium molybdate precipitations after the filtration change in the crystallizer tank, after evaporative crystallization, separation, drying, close batch, obtain ammonium paramolybdate 1325Kg, the molybdenum casting yield is 94.16%.
Embodiment 4: get 1000Kg through the drying room oven dry, despecking removes the compacting table top behind all kinds of foreign material, car cutting powder, reclaimed materials (molybdenum content is 85.6%) such as molybdenum oxide tread powder, after crusher in crushing, powder is by 80 eye mesh screens, under 480 ℃～520 ℃ temperature, once carry out stirring by per 45 ~ 55min, Yu Duotai reflection kiln roasting 6h, press calcining: pure water: ammoniacal liquor=1: 0.9: 1.3, with calcining, pure water, ammoniacal liquor places leaching vat, abundant mixing under 70 ℃～80 ℃, constantly stirring and heating down, production technique adding sodium sulphite and gac purify routinely, when ammonium molybdate solution proportion reaches 1.20g/cm
3In time, stop to stir and heating, treat after the ammonium molybdate solution clarification supernatant liquor to be sucked in the enamel acid deep gouge, under 40 ℃～60 ℃ temperature, the control pH value is 1.5～2.5 to adopt hydrochloric acid to carry out acid to sink, many ammonium molybdate precipitations after the filtration change in the crystallizer tank, after evaporative crystallization, separation, drying, close batch, obtain ammonium paramolybdate 1442Kg, the molybdenum casting yield is 94.34%.
Claims (3)
1. method that the reclaimed materials that utilizes molybdenum is produced ammonium paramolybdate comprises successively:
(1) select materials, impurities removing;
(2) adopt 40 orders ~ 100 purpose screen clothes that the reclaimed materials powder of molybdenum is sieved;
(3) undersize material is sent in the stoving oven oxidizing roasting 5 ~ 8h under 480 ℃ ~ 550 ℃ temperature;
(4) with the calcining that obtains after the roasting, calcining by mass percentage: pure water: ammoniacal liquor=1: (0.7 ~ 0.9): the ratio of (1.2 ~ 1.4), calcining, pure water, ammoniacal liquor are placed leaching vat, under 70 ℃ ~ 80 ℃, stir, production technique adds sodium sulphite and gac routinely, when ammonium molybdate solution proportion reaches 1.18g/cm
3~ 1.22g/cm
3In time, stop to stir and heating;
(5) treat ammonium molybdate solution clarification after, supernatant liquor is sucked in the enamel acid deep gouge, under 40 ℃ ~ 60 ℃ temperature, control solution pH value is 1.5 ~ 2.5, adopts hydrochloric acid to carry out acid and sinks;
(6) sour jetsam slurry is filtered, the many ammonium molybdates precipitations that obtain change in the crystallizer tank, after carrying out evaporative crystallization, separation, dry, close batch through production technique routinely, obtain meeting the ammonium paramolybdate of GB.
2. the reclaimed materials that utilizes molybdenum as claimed in claim 1 is produced the method for ammonium paramolybdate, it is characterized in that: when reclaimed materials is trench material, settling bowl reclaimed materials, dry before in step (1), step (1) afterwards, step (2) carries out fragmentation before; When reclaimed materials during for block reclaimed materials such as compacting defect ware, car cutting base bits piece, immersion oil bases, step (1) afterwards, step (2) carries out fragmentation before.
3. the method for utilizing the reclaimed materials production ammonium paramolybdate of molybdenum as claimed in claim 1 or 2, it is characterized in that: stoving oven is tubular type retort furnace or reverberatory furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101926854A CN101205085A (en) | 2007-12-19 | 2007-12-19 | Method for producing secondary ammonium molybdate by molybdenum recovery material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101926854A CN101205085A (en) | 2007-12-19 | 2007-12-19 | Method for producing secondary ammonium molybdate by molybdenum recovery material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101205085A true CN101205085A (en) | 2008-06-25 |
Family
ID=39565596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101926854A Pending CN101205085A (en) | 2007-12-19 | 2007-12-19 | Method for producing secondary ammonium molybdate by molybdenum recovery material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101205085A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436695A (en) * | 2013-08-30 | 2013-12-11 | 金堆城钼业股份有限公司 | Commercial molybdenum oxide ammonia leaching technology capable of reducing slagging rate and molybdenum content in slag |
| CN104003445B (en) * | 2014-06-06 | 2015-10-28 | 江苏峰峰钨钼制品股份有限公司 | A kind of method of producing high-dissolvability Ammonium Heptamolybdate |
| 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 |
-
2007
- 2007-12-19 CN CNA2007101926854A patent/CN101205085A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436695A (en) * | 2013-08-30 | 2013-12-11 | 金堆城钼业股份有限公司 | Commercial molybdenum oxide ammonia leaching technology capable of reducing slagging rate and molybdenum content in slag |
| CN103436695B (en) * | 2013-08-30 | 2015-07-29 | 金堆城钼业股份有限公司 | A kind of molybdenum calcining ammonia soaking technology reducing molybdenum content in slagging rate and slag |
| CN104003445B (en) * | 2014-06-06 | 2015-10-28 | 江苏峰峰钨钼制品股份有限公司 | A kind of method of producing high-dissolvability Ammonium Heptamolybdate |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104876250B (en) | Method for extracting lithium and removing aluminum by treating lepidolite with sulfuric acid | |
| CN101792187B (en) | Method for producing feed grade ferrous sulfate monohydrate from titanium pigment waste acid condensed slag | |
| CN101914678B (en) | Method for producing industry molybdenum oxide from molybdenum concentrate | |
| CN101921001B (en) | Technology for preparing cobalt hydroxide from cobaltous sulfate solution | |
| CN102094119A (en) | Method for preparing electrolytic manganese metal with low-grade pyrolusite wet leaching | |
| CN103088207A (en) | Efficient vanadium extraction method by performing alkali roasting on vanadium mineral | |
| CN104232941B (en) | A kind of method of synthetical recovery molybdenum and rhenium from high rhenium concentrated molybdenum ore | |
| CN105776333A (en) | Preparation method of vanadium pentoxide | |
| CN109402380B (en) | Method for extracting vanadium from vanadium slag | |
| CN1207409C (en) | Wet process of extracting vanadium and/or molybdenum from waste catalyst | |
| CN112111661A (en) | Method for extracting vanadium by calcium-manganese composite roasting of vanadium slag | |
| CN105349792B (en) | A kind of brass clinker recycling technique | |
| CN110306065A (en) | A kind of method that vanadium slag prepares ammonium metavanadate | |
| CN102220499B (en) | Roasting-leaching method of fine vanadium slags | |
| CN101712491A (en) | Process method for producing vanadic oxide from vanadium-contained wastewater slag | |
| CN102732727B (en) | Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag | |
| CN107475511A (en) | It is a kind of by low nickel matte calcification baking acidleach high efficiency extraction nickel, copper, cobalt method | |
| CN101205085A (en) | Method for producing secondary ammonium molybdate by molybdenum recovery material | |
| CN101693554A (en) | Method for extracting vanadium pentoxide from stone coal ores | |
| CN113387387A (en) | Method for preparing sodium tungstate solution by utilizing tungsten-containing waste in short process | |
| CN105671324A (en) | Method for preparing ammonium rhenate from rhenium-enriched slags | |
| CN113060765A (en) | Oxygen-enriched decomposition process of tungsten raw material | |
| KR101718440B1 (en) | Method for preparing magnesium compound from Fe-Ni slag | |
| KR101690173B1 (en) | slag treatment method for extracting silic and magnesia | |
| CN105399132B (en) | A kind of technique for preparing basic copper chloride and basic zinc chloride with brass clinker and flue dust containing zinc |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080625 |