CN108034816A - A kind of rare earths separation method in monazite - Google Patents
A kind of rare earths separation method in monazite Download PDFInfo
- Publication number
- CN108034816A CN108034816A CN201711387558.XA CN201711387558A CN108034816A CN 108034816 A CN108034816 A CN 108034816A CN 201711387558 A CN201711387558 A CN 201711387558A CN 108034816 A CN108034816 A CN 108034816A
- Authority
- CN
- China
- Prior art keywords
- small
- rare earth
- ore
- solution
- thorium
- 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
Classifications
-
- 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
- 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
- C22B3/065—Nitric 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
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- 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
- C22B59/00—Obtaining rare earth metals
-
- 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
- C22B60/0221—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
- C22B60/0239—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes by leaching using acidic solutions or liquors nitric acid containing 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
- C22B60/026—Obtaining thorium, uranium, or other actinides obtaining uranium by wet processes treatment or purification of solutions or of liquors or of slurries liquid-liquid extraction with or without dissolution in organic solvents
-
- 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
- C22B60/0291—Obtaining thorium, uranium, or other actinides obtaining thorium
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of rare earths separation method in monazite, comprise the following steps：Solitary stone ore mischmetal ore deposit is first worn into mineral powder, granularity in mineral powder is 80um, first using open-circuit grinding in batches, again using imitative closed circuit grinding, its method is that the raw ore chosen is ground to after a certain period of time, and it is more than 70um products to sift out grade, oversize is regrinded, ore milling concentration when water when regrinding should be by oversize weight and mill raw ore adds, until when the miberal powder content of 50um reaches more than 80%, washes mineral powder；By solitary rock ballast (㎏)：Sour (L)=1:1~15 ratio, solitary rock ballast is added in the sulfuric acid solution that concentration is 0.25mol/L~0.5mol/L, is heated to 40 DEG C~100 DEG C, when stirring 5 is small~8 it is small when, cooling and standings clarification 4 it is small when~8 it is small when, siphon supernatant obtain containing uranium, thorium, rare earth valuable element solution.
Description
Technical field
The present invention relates to the rare earth in a kind of monazite, and in particular to a kind of rare earths separation method in monazite.
Background technology
Monazite is one of essential mineral of metallic ore of rare earth, normal thoriated, zirconium etc..Monoclinic system, crystal are in tiny tabular.
Reddish brown, yellow or yellow green, greasy luster or glassy lustre, conchoidal to irregular columnar fracture.Crisp, the hardness 5~5.5 of property, density 4.9
~5.5g/cm3.Emerald green fluorescence is issued in ultraviolet light.Because of normal uranium-bearing, thorium, radium, therefore with compared with high radioactivity, monazite
In contain substantial amounts of rare earth element, but it is also very difficult to remove harmful radioactive materials therein such as uranium etc. at the same time, therefore anxious in the industry
Need a kind of rare earths separation method in monazite.
The content of the invention
It is various in monazite to remove present invention aims at a kind of rare earths separation method provided in monazite
Impurity and radioactive element, obtain pure rare earth element.
In order to solve the above technical problem, the present invention provides following technical solution：
The present invention provides a kind of rare earths separation method in monazite, comprise the following steps：
Step 1)：Solitary stone ore mischmetal ore deposit is first worn into mineral powder, the granularity in mineral powder is -80um, is first used
Open-circuit grinding in batches, then using imitative closed circuit grinding, its method is that the raw ore chosen is ground to after a certain period of time, sift out grade for-
More than 70um products, oversize are regrinded, and ore milling concentration when water when regrinding should be by oversize weight and mill raw ore adds
Add, until when the miberal powder content of -50um reaches more than 80%, wash mineral powder.
Step 2)：By solitary rock ballast (㎏)：Sour (L)=1:1~15 ratio, solitary rock ballast is added to concentration is
In the sulfuric acid solution of 0.25mol/L~0.5mol/L, be heated to 40 DEG C~100 DEG C, when stirring 5 is small~8 it is small when, cooling and standings are clear
It is clear 4 it is small when~8 it is small when, siphon supernatant obtain containing uranium, thorium, rare earth valuable element solution.
Step 3)：Secondary pickling is carried out, by solitary rock ballast (㎏)：Sour (L)=1：1~3 ratio, is by concentration
The sulfuric acid solution of 0.25mol/L~0.5mol/L is added in the slurry after siphon supernatant, is heated to 40 DEG C~100 DEG C, is stirred
Mix 5 it is small when~8 it is small when, when cooling and standings clarification 4 is small~8 it is small when, siphon supernatant merge to obtain with gained supernatant containing uranium,
The solution of thorium, rare earth valuable element.
Step 4)：The slurry after siphon supernatant is squeezed into plate and frame filter press press filtration to no solution with pump to flow out, filtrate with
Step 3) supernatant merges.
Step 5)：The filter residue of plate and frame filter press is added into water washing, to water inlet is stopped during filtrate pH value 2~3, press dry filter residue,
Water lotion merges with the supernatant in step 3), obtains containing uranium, thorium, the limpid aqueous solution of rare earth and containing monazite, zirconium English
The ores such as stone and residual uranium, thorium, the filter residue of rare earth compound.
Step 6)：Add water size mixing with 45-55% sodium hydroxide carried out at 130-140 degrees Celsius of temperature 3-6 it is small when
Caustic digestion efficiency is about 98%, and alkaline ore pulp is again with 96% concentrated nitric acid with ore pulp；Nitric acid=1.0:0.4 volume ratio is 70-80
Rare earth is leached at a temperature of degree Celsius (reaction heat) and leaches terminal PH=4.0-5.0, more than 99% rare earth is transferred to nitric acid at this time
Solution and thorium and uranium and a small amount of rare earth are stayed in leached mud, filtrate sends to recovering rare earth after filtering；Useful 96% concentrated nitric acid
The volume ratio for dissolving nitric acid and thorium cake is 1:0.3 temperature be about 50 degrees Celsius of (reaction heat) times 1 it is small when or so dissolution rate 99%；
Then the sodium hydroxide adjustment spent acid amount for adding 45% carries out sludge extraction with TBP again for 4-5NHNO3.The first step is left with 35%
Thorium in nitric acid leaching ore pulp, substantially all be extracted into organic phase of uranium are reached thorium, uranium and rare earth by right TBP- kerosins
Separation.
As a preferred technical solution of the present invention, device therefor is conical ball mill during the ore grinding.
As a preferred technical solution of the present invention, pickling can be also carried out after the secondary pickling, by solitary rock ballast
(㎏)：Sour (L)=1：1~3 ratio, siphon supernatant is added to by the sulfuric acid solution that concentration is 0.10mol/L~0.25mol/L
In slurry after liquid, be heated to 40 DEG C~100 DEG C, when stirring 0.5 is small~1 it is small when, when cooling and standings clarification 4 is small~8 it is small when, rainbow
Supernatant obtained by sucting clear liquid and step 2) merge to obtain containing uranium, thorium, rare earth valuable element solution.
, can be with extractant organic solution, extraction and recovery after the separation as a preferred technical solution of the present invention
Rare earth after separation in solution, and remove the raffinate of one calcium of phosphoric acid.
As a preferred technical solution of the present invention, before the addition extractant, alkalescence is first added in the solution
Material, using regulation system pH value as 0.1~0.5, preferable ph is 0.2~0.4.
In technical scheme, turn to the phosphate transfection of these elements in ore with caustic digestion monazite concentrate
Hydroxide uranium generates sodium diuranate, adds water to size mixing and is carried out with 45-55% sodium hydroxide at 130-140 degrees Celsius of temperature
3-6 it is small when caustic digestion efficiency be about 98%, alkaline ore pulp is again with 96% concentrated nitric acid with ore pulp；Nitric acid=1.0:0.4 volume ratio
Rare earth is leached at a temperature of 70-80 degrees Celsius (reaction heat) and leaches terminal PH=4.0-5.0, at this time more than 99% rare earth
It is transferred to salpeter solution and thorium and uranium and a small amount of rare earth are stayed in leached mud, filtrate sends to recovering rare earth after filtering；Useful 96%
The volume ratio of concentrated nitric acid dissolving nitric acid and thorium cake be 1:0.3 temperature be about 50 degrees Celsius of (reaction heat) times 1 it is small when or so it is molten
Solution rate 99%；Then the sodium hydroxide adjustment spent acid amount for adding 45% carries out sludge extraction with TBP again for 4-5NHNO3.The first step
With 35% or so TBP- kerosins by nitric acid leach ore pulp in thorium, uranium it is substantially all be extracted into organic phase reach thorium,
The separation of uranium and rare earth.Apply the technical scheme of the present invention, be directed to the special circumstances of the mineral of phosphorus ore containing monazite, using wherein
The architectural feature of the difficult rare-earth mineral decomposed such as monazite cause its decomposition condition relative to phosphorus ore it is harsh the characteristics of, using phosphoric acid
Leaching processing is carried out to phosphorus ore containing monazite, phosphorus ore is dissolved production one-lime phosphate (Ca (H2PO4) 2) enters liquid phase, so that
Apatite is separated with monazite.Meanwhile one-lime phosphate solution is neutralized in solid slag containing monazite respectively in the present invention
The rare earths of two kinds of different phases recycled, while improving rare earth and returning rate, reduce the chemical industry consumptive material dosage such as acid, alkali.
Beneficial effects of the present invention：The special circumstances of the mineral of phosphorus ore containing monazite are directed to, utilize the difficulties such as wherein monazite
The architectural feature of the rare-earth mineral of decomposition cause its decomposition condition relative to phosphorus ore it is harsh the characteristics of, using phosphoric acid to containing monazite
Phosphorus ore carries out leaching processing, and phosphorus ore is dissolved production one-lime phosphate (Ca (H2PO4) 2) enters liquid phase so that apatite with it is only
Stone is occupied to be separated.Meanwhile neutralize two kinds of differences in solid slag containing monazite to one-lime phosphate solution respectively in the present invention
The rare earth of phase is recycled, and while rare earth time rate is improved, reduces the chemical industry consumptive material dosage such as acid, alkali, and can be effective
Radioactive element in rare-earth separating, obtains purer rare earth element.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
Below by embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
The present invention provides a kind of rare earths separation method in monazite, comprises the following steps：
Step 1)：Solitary stone ore mischmetal ore deposit is first worn into mineral powder, the granularity in mineral powder is -80um, is first used
Open-circuit grinding in batches, then using imitative closed circuit grinding, its method is that the raw ore chosen is ground to after a certain period of time, sift out grade for-
More than 70um products, oversize are regrinded, and ore milling concentration when water when regrinding should be by oversize weight and mill raw ore adds
Add, until when the miberal powder content of -50um reaches more than 80%, wash mineral powder.
Step 2)：By solitary rock ballast (㎏)：Sour (L)=1:1~15 ratio, solitary rock ballast is added to concentration is
In the sulfuric acid solution of 0.25mol/L~0.5mol/L, be heated to 40 DEG C~100 DEG C, when stirring 5 is small~8 it is small when, cooling and standings are clear
It is clear 4 it is small when~8 it is small when, siphon supernatant obtain containing uranium, thorium, rare earth valuable element solution.
Step 3)：Secondary pickling is carried out, by solitary rock ballast (㎏)：Sour (L)=1：1~3 ratio, is by concentration
The sulfuric acid solution of 0.25mol/L~0.5mol/L is added in the slurry after siphon supernatant, is heated to 40 DEG C~100 DEG C, is stirred
Mix 5 it is small when~8 it is small when, when cooling and standings clarification 4 is small~8 it is small when, siphon supernatant merge to obtain with gained supernatant containing uranium,
The solution of thorium, rare earth valuable element.
Step 4)：The slurry after siphon supernatant is squeezed into plate and frame filter press press filtration to no solution with pump to flow out, filtrate with
Step 3) supernatant merges.
Step 5)：The filter residue of plate and frame filter press is added into water washing, to water inlet is stopped during filtrate pH value 2~3, press dry filter residue,
Water lotion merges with the supernatant in step 3), obtains containing uranium, thorium, the limpid aqueous solution of rare earth and containing monazite, zirconium English
The ores such as stone and residual uranium, thorium, the filter residue of rare earth compound.
Step 6)：Add water size mixing with 45-55% sodium hydroxide carried out at 130-140 degrees Celsius of temperature 3-6 it is small when
Caustic digestion efficiency is about 98%, and alkaline ore pulp is again with 96% concentrated nitric acid with ore pulp；Nitric acid=1.0:0.4 volume ratio is 70-80
Rare earth is leached at a temperature of degree Celsius (reaction heat) and leaches terminal PH=4.0-5.0, more than 99% rare earth is transferred to nitric acid at this time
Solution and thorium and uranium and a small amount of rare earth are stayed in leached mud, filtrate sends to recovering rare earth after filtering；Useful 96% concentrated nitric acid
The volume ratio for dissolving nitric acid and thorium cake is 1:0.3 temperature be about 50 degrees Celsius of (reaction heat) times 1 it is small when or so dissolution rate 99%；
Then the sodium hydroxide adjustment spent acid amount for adding 45% carries out sludge extraction with TBP again for 4-5NHNO3.The first step is left with 35%
Thorium in nitric acid leaching ore pulp, substantially all be extracted into organic phase of uranium are reached thorium, uranium and rare earth by right TBP- kerosins
Separation.
Embodiment 2
The present invention provides a kind of rare earths separation method in monazite, comprises the following steps：
Step 1)：Solitary stone ore mischmetal ore deposit is first worn into mineral powder, the granularity in mineral powder is -80um, is first used
Open-circuit grinding in batches, then using imitative closed circuit grinding, its method is that the raw ore chosen is ground to after a certain period of time, sift out grade for-
More than 70um products, oversize are regrinded, and ore milling concentration when water when regrinding should be by oversize weight and mill raw ore adds
Add, until when the miberal powder content of -50um reaches more than 80%, wash mineral powder.
Step 2)：By solitary rock ballast (㎏)：Sour (L)=1:1~15 ratio, solitary rock ballast is added to concentration is
In the sulfuric acid solution of 0.25mol/L~0.5mol/L, be heated to 40 DEG C~100 DEG C, when stirring 5 is small~8 it is small when, cooling and standings are clear
It is clear 4 it is small when~8 it is small when, siphon supernatant obtain containing uranium, thorium, rare earth valuable element solution.
Step 3)：Secondary pickling is carried out, by solitary rock ballast (㎏)：Sour (L)=1：1~3 ratio, is by concentration
The sulfuric acid solution of 0.25mol/L~0.5mol/L is added in the slurry after siphon supernatant, is heated to 40 DEG C~100 DEG C, is stirred
Mix 5 it is small when~8 it is small when, when cooling and standings clarification 4 is small~8 it is small when, siphon supernatant merge to obtain with gained supernatant containing uranium,
The solution of thorium, rare earth valuable element.
Step 4)：The slurry after siphon supernatant is squeezed into plate and frame filter press press filtration to no solution with pump to flow out, filtrate with
Step 3) supernatant merges.
Step 5)：The filter residue of plate and frame filter press is added into water washing, to water inlet is stopped during filtrate pH value 2~3, press dry filter residue,
Water lotion merges with the supernatant in step 3), obtains containing uranium, thorium, the limpid aqueous solution of rare earth and containing monazite, zirconium English
The ores such as stone and residual uranium, thorium, the filter residue of rare earth compound.
Step 6)：Add water size mixing with 45-55% sodium hydroxide carried out at 130-140 degrees Celsius of temperature 3-6 it is small when
Caustic digestion efficiency is about 98%, and alkaline ore pulp is again with 96% concentrated nitric acid with ore pulp；Nitric acid=1.0:0.4 volume ratio is 70-80
Rare earth is leached at a temperature of degree Celsius (reaction heat) and leaches terminal PH=4.0-5.0, more than 99% rare earth is transferred to nitric acid at this time
Solution and thorium and uranium and a small amount of rare earth are stayed in leached mud, filtrate sends to recovering rare earth after filtering；Useful 96% concentrated nitric acid
The volume ratio for dissolving nitric acid and thorium cake is 1:0.3 temperature be about 50 degrees Celsius of (reaction heat) times 1 it is small when or so dissolution rate 99%；
Then the sodium hydroxide adjustment spent acid amount for adding 45% carries out sludge extraction with TBP again for 4-5NHNO3.The first step is left with 35%
Thorium in nitric acid leaching ore pulp, substantially all be extracted into organic phase of uranium are reached thorium, uranium and rare earth by right TBP- kerosins
Separation.
Can be with extractant organic solution, the rare earth after extraction and recovery separation in solution after step 7) separation, and remove and contain
The raffinate of one-lime phosphate.Before adding extractant, alkaline matter first is added in the solution, using regulation system pH value as 0.1
~0.5, preferable ph is 0.2~0.4.
| Extraction of rare eart rate % | Phosphorus content % | Proportion | Radioactivity | |
| Embodiment 1 | 98.98 | 0.368 | 1.95-5.5 | Nothing |
| Embodiment 2 | 99.25 | 0.125 | 1.86-5,0 | Nothing |
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To modify to the technical solution described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent replacement, improvement and so on, should be included in the present invention's
Within protection domain.
Claims (5)
1. a kind of rare earths separation method in monazite, it is characterised in that comprise the following steps：
Step 1)：Solitary stone ore mischmetal ore deposit is first worn into mineral powder, the granularity in mineral powder is -80um, first using in batches
Open-circuit grinding, then using imitative closed circuit grinding, its method is that the raw ore chosen is ground to after a certain period of time, sift out grade for -70um with
Upper product, oversize are regrinded, and ore milling concentration when water when regrinding should be by oversize weight and mill raw ore adds, and treats
When reaching more than 80% to the miberal powder content of -50um, mineral powder is washed.
Step 2)：By solitary rock ballast (㎏)：Sour (L)=1:1~15 ratio, it is 0.25mol/ that solitary rock ballast is added to concentration
In the sulfuric acid solution of L~0.5mol/L, be heated to 40 DEG C~100 DEG C, when stirring 5 is small~8 it is small when, when cooling and standings clarification 4 is small
~8 it is small when, siphon supernatant obtain containing uranium, thorium, rare earth valuable element solution.
Step 3)：Secondary pickling is carried out, by solitary rock ballast (㎏)：Sour (L)=1：1~3 ratio, is 0.25mol/L by concentration
The sulfuric acid solution of~0.5mol/L is added in the slurry after siphon supernatant, is heated to 40 DEG C~100 DEG C, when stirring 5 is small~8
Hour, cooling and standings clarification 4 it is small when~8 it is small when, siphon supernatant merges to obtain with gained supernatant to be had containing uranium, thorium, rare earth
The solution of valency element.
Step 4)：The slurry after siphon supernatant is squeezed into plate and frame filter press press filtration to no solution with pump to flow out, filtrate and step
3) supernatant merges.
Step 5)：The filter residue of plate and frame filter press is added into water washing, to water inlet is stopped during filtrate pH value 2~3, filter residue is pressed dry, washes
Liquid merges with the supernatant in step 3), obtains containing uranium, thorium, the limpid aqueous solution of rare earth and containing monazite, zircon etc.
Ore and residual uranium, thorium, the filter residue of rare earth compound.
Step 6)：Add water size mixing with 45-55% sodium hydroxide carried out at 130-140 degrees Celsius of temperature 3-6 it is small when alkali point
It is about 98% to solve efficiency, and alkaline ore pulp is again with 96% concentrated nitric acid with ore pulp；Nitric acid=1.0:0.4 volume ratio is Celsius 70-80
Rare earth is leached at a temperature of spending (reaction heat) and leaches terminal PH=4.0-5.0, and more than 99% rare earth is transferred to salpeter solution at this time
And thorium and uranium and a small amount of rare earth are stayed in leached mud, filtrate sends to recovering rare earth after filtering；Useful 96% concentrated nitric acid dissolving
The volume ratio of nitric acid and thorium cake is 1:0.3 temperature be about 50 degrees Celsius of (reaction heat) times 1 it is small when or so dissolution rate 99%；Then
The sodium hydroxide adjustment spent acid amount for adding 45% carries out sludge extraction with TBP again for 4-5NHNO3.The first step is with 35% or so
Thorium in nitric acid leaching ore pulp, uranium substantially all be extracted into are reached thorium, uranium and rare earth by TBP- kerosins in organic phase
Separation.
2. the rare earths separation method in a kind of monazite according to claim 1, it is characterised in that during the ore grinding
Device therefor is conical ball mill.
3. a kind of rare earths separation method in monazite according to claim 1-2, it is characterised in that described secondary
Pickling can be also carried out after acidleach, by solitary rock ballast (㎏)：Sour (L)=1：1~3 ratio, by concentration for 0.10mol/L~
The sulfuric acid solution of 0.25mol/L is added in the slurry after siphon supernatant, is heated to 40 DEG C~100 DEG C, when stirring 0.5 is small~
1 it is small when, when cooling and standings clarification 4 is small~8 it is small when, siphon supernatant and step 2) gained supernatant merge to obtain containing uranium, thorium,
The solution of rare earth valuable element.
4. a kind of rare earths separation method in monazite according to claim 1-3, it is characterised in that the separation
After can be with extractant organic solution, the rare earth after extraction and recovery separation in solution, and remove the raffinate of one calcium of phosphoric acid.
5. a kind of rare earths separation method in monazite according to claim 1-4, it is characterised in that add described
Before entering extractant, alkaline matter first is added in the solution, using regulation system pH value as 0.1~0.5, preferable ph 0.2
~0.4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711387558.XA CN108034816A (en) | 2017-12-20 | 2017-12-20 | A kind of rare earths separation method in monazite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711387558.XA CN108034816A (en) | 2017-12-20 | 2017-12-20 | A kind of rare earths separation method in monazite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108034816A true CN108034816A (en) | 2018-05-15 |
Family
ID=62100239
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711387558.XA Pending CN108034816A (en) | 2017-12-20 | 2017-12-20 | A kind of rare earths separation method in monazite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108034816A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651648A (en) * | 2018-12-18 | 2019-04-19 | 泉州市利芝新材料科技有限公司 | Utilize the method for monazite tailings production negative oxygen ion powder and the application of negative oxygen ion powder |
| CN111020242A (en) * | 2019-09-09 | 2020-04-17 | 湖南中核金原新材料有限责任公司 | Process method for smelting and separating uranium, thorium and rare earth from monazite concentrate |
| CN111235411A (en) * | 2020-03-02 | 2020-06-05 | 包头稀土研究院 | Process for removing calcium-containing minerals in rare earth concentrate and application of sulfuric acid solution |
| CN111270092A (en) * | 2020-02-07 | 2020-06-12 | 包头稀土研究院 | Method for decomposing mixed rare earth ore |
| CN111575485A (en) * | 2020-05-09 | 2020-08-25 | 湛江市红日稀土有限公司 | Recovery processing method for reducing radioactivity of rare earth slag |
| CN114645137A (en) * | 2022-03-17 | 2022-06-21 | 四川省冕宁县方兴稀土有限公司 | Method for resource utilization of iron-thorium waste residues |
| CN115818694A (en) * | 2022-12-09 | 2023-03-21 | 包头稀土研究院 | Method for treating monazite |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925681A (en) * | 2012-11-27 | 2013-02-13 | 益阳鸿源稀土有限责任公司 | Method for separating valuable components of monazite slags |
| CN103014359A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of monazite slag |
| CN106367590A (en) * | 2015-07-22 | 2017-02-01 | 永州市湘江稀土有限责任公司 | Monazite ore comprehensive utilization and recovery process |
| CN107262224A (en) * | 2017-07-31 | 2017-10-20 | 长沙矿冶研究院有限责任公司 | A kind of zinc oxygen leaching method for preparing raw material and two sections of vertical stirring mill series connection open-circuit grinding systems |
-
2017
- 2017-12-20 CN CN201711387558.XA patent/CN108034816A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102925681A (en) * | 2012-11-27 | 2013-02-13 | 益阳鸿源稀土有限责任公司 | Method for separating valuable components of monazite slags |
| CN103014359A (en) * | 2012-11-27 | 2013-04-03 | 益阳鸿源稀土有限责任公司 | Separation and recovery method of monazite slag |
| CN106367590A (en) * | 2015-07-22 | 2017-02-01 | 永州市湘江稀土有限责任公司 | Monazite ore comprehensive utilization and recovery process |
| CN107262224A (en) * | 2017-07-31 | 2017-10-20 | 长沙矿冶研究院有限责任公司 | A kind of zinc oxygen leaching method for preparing raw material and two sections of vertical stirring mill series connection open-circuit grinding systems |
Non-Patent Citations (1)
| Title |
|---|
| 代书华: "《有色金属冶金概论》", 30 September 2015, 冶金工业出版社 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109651648A (en) * | 2018-12-18 | 2019-04-19 | 泉州市利芝新材料科技有限公司 | Utilize the method for monazite tailings production negative oxygen ion powder and the application of negative oxygen ion powder |
| CN109651648B (en) * | 2018-12-18 | 2020-07-17 | 泉州市利芝新材料科技有限公司 | Method for producing negative oxygen ion powder by using monazite tailings and application of negative oxygen ion powder |
| CN111020242A (en) * | 2019-09-09 | 2020-04-17 | 湖南中核金原新材料有限责任公司 | Process method for smelting and separating uranium, thorium and rare earth from monazite concentrate |
| CN111020242B (en) * | 2019-09-09 | 2021-07-20 | 湖南中核金原新材料有限责任公司 | Process method for smelting and separating uranium, thorium and rare earth from monazite concentrate |
| CN111270092A (en) * | 2020-02-07 | 2020-06-12 | 包头稀土研究院 | Method for decomposing mixed rare earth ore |
| CN111270092B (en) * | 2020-02-07 | 2022-08-05 | 包头稀土研究院 | Method for decomposing mixed rare earth ore |
| CN111235411A (en) * | 2020-03-02 | 2020-06-05 | 包头稀土研究院 | Process for removing calcium-containing minerals in rare earth concentrate and application of sulfuric acid solution |
| CN111575485A (en) * | 2020-05-09 | 2020-08-25 | 湛江市红日稀土有限公司 | Recovery processing method for reducing radioactivity of rare earth slag |
| CN114645137A (en) * | 2022-03-17 | 2022-06-21 | 四川省冕宁县方兴稀土有限公司 | Method for resource utilization of iron-thorium waste residues |
| CN114645137B (en) * | 2022-03-17 | 2024-05-31 | 四川省冕宁县方兴稀土有限公司 | Method for recycling iron thorium waste residues |
| CN115818694A (en) * | 2022-12-09 | 2023-03-21 | 包头稀土研究院 | Method for treating monazite |
| CN115818694B (en) * | 2022-12-09 | 2024-01-23 | 包头稀土研究院 | Method for treating monazite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108034816A (en) | A kind of rare earths separation method in monazite | |
| CN103014359B (en) | Separation and recovery method of monazite slag | |
| CN104775026B (en) | A kind of method that high-purity uranium, thorium and mischmetal are extracted from excellent molten slag | |
| CN103014333B (en) | Separation and recovery method of uranium, thorium and rare earth in monazite slag | |
| CN102796876B (en) | Method for extracting scandium oxide from titanium slag chloride waste | |
| CN111020242B (en) | Process method for smelting and separating uranium, thorium and rare earth from monazite concentrate | |
| CN101824536A (en) | Process for extracting rare-earth from sulfuric acid treating phosphorite process | |
| CN103695671A (en) | Method for recycling and purifying scandium oxide powder from waste acid in zirconium salt production | |
| CN105256143B (en) | Scandium and the method for other rare earths are extracted from zirconium oxychloride acid pickle | |
| CN102312090A (en) | Process for extracting scandium from ore containing scandium through pressure leaching | |
| CN106367590A (en) | Monazite ore comprehensive utilization and recovery process | |
| CN107641724A (en) | One kind improves WO in scheelite3The method of leaching rate | |
| CN103695643A (en) | Method for extracting vanadium pentoxide from stone coal vanadium ore acid-mixed pile ore | |
| CN102925681B (en) | Method for separating valuable components of monazite slags | |
| CN103184343A (en) | Method for recovering rare earth, thorium and iron in waste residue of rare earth acid technological process | |
| CN103352130A (en) | Scandium combined extraction method from red mud and titanium dioxide waste liquid | |
| CN102154546A (en) | Method for smelting molybdenum-nickel mineral association by wet process | |
| Seidel | Extracting uranium from its ores | |
| CN111004933A (en) | Six-stage continuous complete dissolution method for monazite optimal dissolution slag | |
| CN103014358B (en) | Treatment method of tailings after separation and recovery of monazite slag | |
| CN106745084A (en) | Utilization method of glauberite ore | |
| CN114277265A (en) | Method for preparing thorium oxide by using monazite optimum-solubility slag | |
| CN107012342A (en) | A kind of method for extracting low-grade ion type rareearth raw ore rare earth elements | |
| CN106756129A (en) | A kind of method that uranium is extracted from stone containing betafite | |
| CN100400687C (en) | Method of extracting radioactive uranium in phosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180515 |