CN105385849A - Stone coal navajoite enrichment U3O8 - Google Patents

Stone coal navajoite enrichment U3O8 Download PDF

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Publication number
CN105385849A
CN105385849A CN201510808558.7A CN201510808558A CN105385849A CN 105385849 A CN105385849 A CN 105385849A CN 201510808558 A CN201510808558 A CN 201510808558A CN 105385849 A CN105385849 A CN 105385849A
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uranium
coal navajoite
vanadium
bone coal
enrichment
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CN201510808558.7A
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杨道印
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0221—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching
    • C22B60/0226—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors
    • C22B60/0234—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors sulfurated ion as active agent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B60/00—Obtaining metals of atomic number 87 or higher, i.e. radioactive metals
    • C22B60/02—Obtaining thorium, uranium, or other actinides
    • C22B60/0204—Obtaining thorium, uranium, or other actinides obtaining uranium
    • C22B60/0217—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes
    • C22B60/0252—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries
    • C22B60/0278—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries by chemical methods
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention aims at providing a method for enriching U3O8 from stone coal navajoite. The technology process includes the steps that (1) stone coal navajoite is crushed, ground and roasted; (2) roasted ore is leached through dilute sulphuric acid, and pickle liquor containing vanadium, uranium and the like is obtained through filtering; (3) under the ambient temperature condition, edulcoration is not needed, a composite precipitator is directly added into the pickle liquor, polyoxovanadate and precipitate such as uranium, aluminum and phosphorus are obtained; (4) vanadium, uranium and the like are separated through alkali dissolution precipitate, and vanadium is left in filter liquor; and (5) filter residues are secondary ore of uranium, U3O8 in the stone coal navajoite is enriched to more than 40 times, the high grade being larger than or equal to 0.2% is achieved, and the recovery rate is larger than 99%; and when one ton of V2O5 is produced each time, 2.5-3 tons of secondary ore of uranium can be obtained at the same time. By means of the method, uranium resources in the stone coal navajoite are effectively used; and in addition, the method has the advantages that the process procedure is short, the working procedure is simple and convenient, the working efficiency is high, a reagent material is low in cost, and the environmental pollution is further reduced.

Description

Bone coal navajoite enrichment U 3o 8
Technical field
The present invention relates to one enrichment U from bone coal navajoite 3o 8method.
Background technology
Bone coal navajoite is a kind of low-grade many metals mineral intergrowth, in bone coal except vanadium, also containing elements such as silicon, carbon, phosphorus, aluminium and uranium.China's bone coal resource is extremely abundant, and reserves 61,800,000,000 tons, in bone coal, vanadium grade is generally 0.13 ~ 1.2%.The associated element uranium contained in bone coal navajoite, grade is extremely low, is generally (3 ~ 7) × 10 -5.Only with Xiangxi autonomous prefecture bone coal navajoite resource 31.7 hundred million tons measuring and calculating, uranium reserve more than 15.0 ten thousand tons.
Current exploitation uranium resources is mainly by mining-ore dressing-extraction conventional flowsheet and Situ Leaching method.Industry is thought, uranium ore grade has extraction value higher than 0.05%.
Uranium is distributed in sulfuric acid immersion liquid in extracting vanadium by acid leaching of stone coal process, and uranium concentration is generally tens milligrams often liter, is difficult to the uranium in the physical method enrichment immersion liquid such as extraction or resin absorption.
The present invention can by the U in bone coal navajoite 3o 8enrichment reaches>=the middle higher-grade of 0.2%, and rate of recovery > 99%; Often produce 1 ton of V 2o 5, 2.5 ~ 3.0 tons of uranium secondary ores can be obtained simultaneously.
Summary of the invention
The object of the present invention is to provide one enrichment U from bone coal navajoite 3o 8method, wherein uranium resources is effectively used.
The present invention is enrichment U from bone coal navajoite 3o 8method, it is characterized in that comprising following steps successively:
(1) bone coal navajoite is carried out fragmentation, grinding, grinding particle size > 20 order;
(2) roasting bone coal navajoite, temperature 650 DEG C ~ 900 DEG C;
(3) calcining dilute sulphuric acid leaches, and sulfuric acid dosage is 1 ~ 8% of stone coal mine quality, liquid-solid ratio=3: 1 ~ 1: 1, and normal temperature circulation drenches leaching or multistage agitation leach, agitation leach time 2 ~ 8h;
(4) solid-liquid separation, filters and obtains pickling liquor, pickling liquor vanadium concentration > 6.0g/L;
(5) under normal temperature condition, without the need to removal of impurities, directly in step (4) pickling liquor, add ammonium salt class compound precipitants, to adjust and control pH is 3.0 ~ 6.5, obtain the throw out such as polyoxovanadate and uranium, aluminium and phosphorus.Wherein compound precipitants is (NH 4) 2sO 4, NH 4hSO 4, NH 4cl, NH 4nO 3, (NH 4) 2hPO 4, (NH 4) 3pO 4, NH 4hCO 3, (NH 4) 2cO 3, NH 4two kinds in F and ammoniacal liquor combine.Effective reaction time 1 ~ 5h, vanadium deposition rate >=95%.
(6) according to content of vanadium in step (5) throw out, calculate amount of water, make solution vanadium concentration > 20g/L, and heat solution to 40 ~ 80 DEG C, adding alkaline matter adjustment pH is 8 ~ 9, effective reaction time 0.5 ~ 3h.Wherein alkaline matter is ammoniacal liquor, C a(OH) 2, N aoH, KOH and N a2cO 3in one.
(7) filter alkaline solution, be separated with uranium etc. by vanadium, vanadium is stayed in filtrate, molten yield >=95% of vanadium.
(8) filter residue such as uranium-bearing is uranium secondary ore, U 3o 8grade>=0.2%, rate of recovery > 99%; Often produce 1 ton of V 2o 5, 2.5 ~ 3.0 tons of uranium secondary ores can be obtained simultaneously.
Tool of the present invention has the following advantages:
1, normal temperature Direct precipitation vanadium enrichment uranium.Under normal temperature condition, do not need complicated removal of impurities operation for the immersion liquid of bone coal calcining diluted acid, Direct precipitation vanadium, and make the uranium be dispersed in immersion liquid be able to enrichment.Adjustment calcining acid leaching process, while raising pickling liquor vanadium concentration, significantly can promote uranium secondary ore grade.
2, can effectively vanadium in throw out be separated with uranium etc.
3, technical process is short, and operation is easy, and effective reaction time is short, and work efficiency is high.
4, technical parameter is reliable and stable, workable, easily realizes industrial automation.
5, production unit is simple, and except the broken mill of bone coal navajoite, roasting, all the other respectively walk major equipment only needs setting tank and pressure filter.
6, the uranium secondary ore that obtains (eliminate and reconnoitre-dig up mine-ore dressing-break the operation such as mill) is in powdery, loosely organized, is convenient to purify further operation.
7, reagent material is cheap, and production cost is lower.
8, environmental friendliness.In suitability for industrialized production of the present invention, water consumption is few and can recycle; Slag (comprising bone coal navajoite slag slag secondary to uranium), after extraction useful element relative " totally ", can be used as building materials or backfills second ploughing for mining area; Further reduction environmental pollution.
Accompanying drawing: bone coal navajoite enrichment U 3o 8process flow sheet
Embodiment
Below in conjunction with embodiment, the invention will be further described, and following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1
Get containing V 2o 58.56g/L, Si0.11g/L, F ethe bone coal calcining diluted acid immersion liquid 500ml of < 0.05g/L, Al1.92g/L, P2.13g/L and pH1.5, under normal temperature condition, directly adds compound precipitants, and adjustment pH value of solution is 6.5, effective reaction time 5h, vanadium deposition rate>=95%.According to content of vanadium in throw out, calculate amount of water, make solution vanadium concentration > 20g/L.Heat solution to 80 DEG C, adding alkaline matter adjustment pH is 8 ~ 9, effective reaction time 3h.Filter alkaline solution, be separated with uranium etc. by vanadium, vanadium is stayed in filtrate, molten yield>=95% of vanadium; The filter residues such as uranium-bearing are U 3o 8secondary ore, grade 0.2%, rate of recovery > 99%.
Embodiment 2
Get containing V 2o 516.26g/L, Si0.12g/L, F ebone coal calcining two sections of diluted acid immersion liquid 1000ml of < 0.05g/L, Al2.27g/L, P2.98g/L and pH1.3, under normal temperature condition, directly add compound precipitants, and adjustment pH value of solution is 6.0, effective reaction time 3h, vanadium deposition rate>=95%.According to content of vanadium in throw out, calculate amount of water, make solution vanadium concentration >=30g/L.Heat solution to 70 DEG C, adding alkaline matter adjustment pH is 8 ~ 9, effective reaction time 3h.Filter alkaline solution, be separated with uranium etc. by vanadium, vanadium is stayed in filtrate, molten yield>=95% of vanadium; The filter residues such as uranium-bearing are U 3o 8secondary ore, grade 0.23%, rate of recovery > 99%.
Embodiment 3
Get containing V 2o 525.55g/L, Si0.12g/L, F ebone coal calcining three sections of diluted acid immersion liquid 1000ml of < 0.05g/L, Al3.35g/L, P4.37g/L and pH1.0, under normal temperature condition, directly add compound precipitants, and adjustment pH value of solution is 5.5, effective reaction time 3h, vanadium deposition rate>=95%.According to content of vanadium in throw out, calculate amount of water, make solution vanadium concentration >=30g/L.Heat solution to 50 DEG C, adding alkaline matter adjustment pH is 8 ~ 9, effective reaction time 3h.Filter alkaline solution, be separated with uranium etc. by vanadium, vanadium is stayed in filtrate, molten yield>=95% of vanadium; The filter residues such as uranium-bearing are U 3o 8secondary ore, grade 0.375%, rate of recovery > 99%.
Embodiment 4
Get containing V 2o 58.98g/L, Si0.15g/L, F eimmersion liquid 19m is drenched in the bone coal calcining diluted acid circulation of < 0.05g/L, Al2.28g/L, P2.35g/L and pH1.33 3, under normal temperature condition, directly add compound precipitants, adjustment pH value of solution is 6.5, effective reaction time 3h, vanadium deposition rate>=95%.According to content of vanadium in throw out, calculate amount of water, make solution vanadium concentration >=30g/L.Heat solution to 70 DEG C, adding alkaline matter adjustment pH is 8 ~ 9, effective reaction time 3h.Filter alkaline solution, be separated with uranium etc. by vanadium, vanadium is stayed in filtrate, molten yield>=95% of vanadium; The filter residues such as uranium-bearing are U 3o 8secondary ore, grade 0.206%, rate of recovery > 99%; Often produce 1 ton of V 2o 5, 2.5 ~ 3.0 tons of uranium secondary ores can be obtained simultaneously.
The invention is not restricted to above-described embodiment, for persons skilled in the art, to any apparent change that it does under the prerequisite not deviating from the principle of the invention, all belong to the protection domain of claims of the present invention.

Claims (6)

1. an enrichment U from bone coal navajoite 3o 8method, it is characterized in that comprising following steps successively:
(1) bone coal navajoite is carried out fragmentation, grinding, grinding particle size is > 20 order;
(2) roasting bone coal navajoite, temperature 650 DEG C ~ 900 DEG C;
(3) calcining dilute sulphuric acid leaches, and sour consumption is 1 ~ 8% of bone coal navajoite quality, liquid-solid ratio=3: 1 ~ 1: 1, and leaching or multistage agitation leach are drenched in normal temperature circulation;
(4) solid-liquid separation, filter and obtain pickling liquor, pickling liquor vanadium concentration is > 6.0g/L;
(5) under normal temperature condition, without the need to removal of impurities, directly in step (4) pickling liquor, add ammonium salt class compound precipitants, to adjust and control pH is 3.0 ~ 6.5, obtain throw out.
(6) according to content of vanadium in step (5) throw out, calculate amount of water, make solution vanadium concentration > 20g/L, and solution is heated to 40 ~ 80 DEG C, adding alkaline matter adjustment pH is 8 ~ 9.
(7) filter alkaline solution, be separated with uranium etc. by vanadium, vanadium is stayed in filtrate;
(8) filter residue such as uranium-bearing is the U of enrichment 3o 8secondary ore.
2. one according to claim 1 enrichment U from bone coal navajoite 3o 8method, it is characterized in that: bone coal navajoite torrefaction temperature 650 DEG C ~ 900 DEG C in (2).
3. one according to claim 1 enrichment U from bone coal navajoite 3o 8method, it is characterized in that: leaching or multistage agitation leach are drenched in the circulation of calcining dilute sulphuric acid normal temperature in (3), and sulfuric acid dosage is 1 ~ 8% of bone coal navajoite quality.
4. one according to claim 1 enrichment U from bone coal navajoite 3o 8method, it is characterized in that: compound precipitants is (NH in (5) 4) 2sO 4, NH 4hSO 4, NH 4cl, NH 4nO 3, (NH 4) 2hPO 4, (NH 4) 3pO 4, NH 4hCO 3, (NH 4) 2cO 3, NH 4two kinds in F and ammoniacal liquor combine.
5. one according to claim 1 enrichment U from bone coal navajoite 3o 8method, it is characterized in that: (6) neutral and alkali material is ammoniacal liquor, C a(OH) 2, N aoH, KOH and N a2cO 3in one as pH adjusting agent.
6. one according to claim 1 enrichment U from bone coal navajoite 3o 8method, it is characterized in that: the uranium secondary ore U of enrichment in (8) 3o 8reach>=0.2% in higher-grade, rate of recovery > 99%; Often produce 1 ton of V 2o 5, 2.5 ~ 3.0 tons of uranium secondary ores can be obtained simultaneously.
CN201510808558.7A 2015-11-23 2015-11-23 Stone coal navajoite enrichment U3O8 Pending CN105385849A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112457037A (en) * 2019-09-09 2021-03-09 天津大学 Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method
CN113088680A (en) * 2021-04-01 2021-07-09 河北工程大学 Leaching method of associated metal in coal mine

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101451199A (en) * 2008-12-16 2009-06-10 中色（宁夏）东方集团有限公司 Method for extracting vanadic anhydride from stone coal vanadium ore
CN102747225A (en) * 2012-07-10 2012-10-24 中南大学 Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid
CN104232940A (en) * 2013-06-14 2014-12-24 无锡市森信精密机械厂 Technology for extracting vanadic anhydride from bone coal by wet method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101451199A (en) * 2008-12-16 2009-06-10 中色（宁夏）东方集团有限公司 Method for extracting vanadic anhydride from stone coal vanadium ore
CN102747225A (en) * 2012-07-10 2012-10-24 中南大学 Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid
CN104232940A (en) * 2013-06-14 2014-12-24 无锡市森信精密机械厂 Technology for extracting vanadic anhydride from bone coal by wet method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
段冉: "高纯五氧化二钒的制备及偏钒酸铵结晶机理的研究", 《中国优秀硕士学位论文全文数据库》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112457037A (en) * 2019-09-09 2021-03-09 天津大学 Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method
CN112457037B (en) * 2019-09-09 2022-02-11 天津大学 Performance and application of mullite fiber whisker porous reinforcement reinforced silica aerogel composite material prepared based on liquid phase method
CN113088680A (en) * 2021-04-01 2021-07-09 河北工程大学 Leaching method of associated metal in coal mine

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Application publication date: 20160309