CN110422870A - The deoiling method of rare earth bromide solution - Google Patents
The deoiling method of rare earth bromide solution Download PDFInfo
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- CN110422870A CN110422870A CN201910745878.0A CN201910745878A CN110422870A CN 110422870 A CN110422870 A CN 110422870A CN 201910745878 A CN201910745878 A CN 201910745878A CN 110422870 A CN110422870 A CN 110422870A
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- rare earth
- earth bromide
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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Abstract
The invention discloses a kind of deoiling methods of rare earth bromide solution, by rare earth bromide solution according to the flow of 20~80L/h by carrying out oil removing filled with cross-linked styrene-divinyl benzene polymers resin column, the rare earth bromide solution after obtaining oil removing；Wherein, the oil concentration in the rare earth bromide solution is 1~35mg/L, and the concentration of rare earth bromide is 0.5~4.0mol/L, and hydrogen ion concentration is 0.005~0.030mol/L.Deoiling method deoiling effect of the invention is good.
Description
Technical field
The present invention relates to a kind of deoiling method of rare earth compound, especially a kind of deoiling method of rare earth bromide.
Background technique
Scintillation crystal refers under the shock of high energy particle, and the functional shift of high energy particle can flash for luminous energy
Crystal.Scintillation crystal can be used for the detection of x-ray, gamma-rays, neutron and other high energy particles, using scintillation crystal as the spy of core
It surveys and imaging technique is in sides such as nuclear medicine, high-energy physics, safety inspection, industrial non-destructive flaw detection, space physics and core mine locatings
Face is widely used.
The rare earth bromide purified out in Rare Earth Mine is the important source material for preparing scintillation crystal.Rare earth bromine used at present
Compound is would generally be containing big in the rare earth bromide for being obtained by passing through extraction and separation in Rare Earth Mine, but being obtained by this method
The oil of amount, so that the rare earth bromide being prepared cannot be directly used to the preparation of scintillation crystal, otherwise scintillation crystal appearance is in
Existing grey.These oil mostly come from during flotation concentrate used in collecting agent, it is extractant used in extraction process, dilute
Agent is released, the surfactant etc. being added in precipitating reagent ammonium hydrogen carbonate.
Deoiling method used at present mainly has biochemical method, gas floatation process, membrane separation process and absorption method.Biochemical method is gentle
Float glass process is easy to produce secondary pollution during processing, and oil removing is not thorough, it is also necessary to which subsequent technique continues oil removal treatment.
Membrane separation process is easy to produce fouling membrane, and treating capacity is small, does not adapt to be mass produced.
Absorption method is broadly divided into activated carbon adsorption and resin adsorption.Application No. is 201010241210.1 Chinese patent public affairs
A kind of method for preparing oil-free rare earth carbonate as adsorbent using active carbon, plant ash or rice husk ash is opened, including as follows
Step: 1, single or mixed rare earth chloride liquid, nitric rare earth feed liquid, sulfuric acid rare earth feed liquid suction has been put into feedstock processing:
In attached dose of filtering ponds, oil-free feed liquid is obtained；Precipitating reagent is put into the filtering ponds of adsorbent, it is molten that oil-free precipitating reagent is obtained by filtration
Liquid；2, it precipitates: oil-free rare earth chloride liquid, nitric rare earth feed liquid, sulfuric acid rare earth feed liquid being added in oil-free precipitating reagent, obtained
To single rare earth carbonate or mischmetal carbonate；3, rinsing, centrifugal dehydration: the single or mixed rare earth carbonic acid that will be obtained
Salt rinsing, drying, obtain oil-free single or mischmetal carbonate.But the adsorption capacity of active carbon, plant ash or rice husk ash
Limited, deoiling effect is bad, and regeneration is difficult, at high cost.
In addition, application No. is the Chinese patents of 200810150419.X to disclose a kind of production work of oil-free cerium carbonate
Skill: 1, squeezing into cerous nitrate mother liquor in enamel slot, adjusts pH value, heating, by cerous carbonate cake filtration oil removing, molten except obtaining after iron
Liquid is spare；2, solution obtained in step 1 is precipitated with precipitating reagent, obtains oil-free cerous carbonate；3, the nothing for obtaining step 2
Oily cerous carbonate washing, dehydration, obtain oil-free cerium carbonate.Technology utilization cerous carbonate cake filtration progress oil removing, but its
Deoiling effect is not ideal enough, cannot obtain the oil-free cerous carbonate of high quality.
Summary of the invention
The present invention provides a kind of method of rare earth bromide solution oil removing, deoiling effect is good.Further, of the invention
Adsorbent material it is reusable, be conducive to industrialized production.
The present invention provides a kind of deoiling method of rare earth bromide solution, includes the following steps:
By rare earth bromide solution according to the flow of 20~80L/h by gathering filled with cross-linked styrene-divinylbenzene
The resin column for closing object carries out oil removing, the rare earth bromide solution after obtaining oil removing；Wherein, in the rare earth bromide solution
Oil concentration is 1~35mg/L, and the concentration of rare earth bromide is 0.5~4.0mol/L, and hydrogen ion concentration be 0.005~
0.030mol/L。
Deoiling method according to the present invention, it is preferable that the rare earth bromide is one of lanthanum bromide or bromination cerium
Or two kinds.
Deoiling method according to the present invention, it is preferable that cross-linked styrene-divinyl benzene polymers specific surface
Product is not less than 900m2/ g, wet apparent density are 0.50~0.90g/ml, and wet true density is 1.00~1.50g/ml.
Deoiling method according to the present invention, it is preferable that cross-linked styrene-divinyl benzene polymers specific surface
Product is not less than 1200m2/ g, wet apparent density are 0.65~0.75g/ml, and wet true density is 1.05~1.15g/ml.
Deoiling method according to the present invention, it is preferable that the oil concentration in the rare earth bromide solution is 3~25mg/
L, the concentration of rare earth bromide is 0.5~3.0mol/L, and hydrogen ion concentration is 0.005~0.015mol/L.
Deoiling method according to the present invention, it is preferable that the cross-linked styrene-divinyl benzene polymers are resin
Grain, and resin particle content of the partial size within the scope of 0.2mm~2.00mm is 85%~100%.
Deoiling method according to the present invention, it is preferable that the ratio between the diameter of the resin column and height are 1:3~20.
Deoiling method according to the present invention, it is preferable that the ratio between the diameter of the resin column and height are 1:7~12.
Deoiling method according to the present invention, it is preferable that the flow of rare earth bromide solution is 30~70L/h.
Deoiling method according to the present invention, it is preferable that oil concentration is less than 0.2mg/L in the rare earth bromide after oil removing.
The present invention, which carries out oil removing to rare earth bromide using cross-linked styrene-divinyl benzene polymers, effectively to be subtracted
Oil content in few rare earth bromide, deoiling effect are good.Using resin as adsorbent material, facilitates and realize to adsorbent material again
Raw and recycling, is conducive to industrialized production.In preferred technical solution of the invention, cross-linked styrene-divinyl
The specific surface area of benzene polymer is not less than 900m2/ g, wet apparent density be 0.50~0.90g/ml, wet true density be 1.00~
1.50g/ml, it is ensured that cross-linked styrene-divinyl benzene polymers adsorption capacity enhances the oil removing to rare earth bromide
Effect.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
Rare earth bromide of the invention includes lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium
(Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), yttrium (Y) and scandium (Sc)
Bromide.According to embodiment of the present invention, rare earth bromide is one or both of lanthanum bromide or bromination cerium.
Deoiling method of the invention includes according to 20~80L/h of flow by rare earth bromide solution by filling crosslinking benzene
Ethylene-divinyl benzene polymers resin column carries out oil removing, the rare earth bromide solution after obtaining oil removing.
In the present invention, the oil concentration in the rare earth bromide solution is 1~35mg/L, the concentration of rare earth bromide
For 0.5~4.0mol/L, hydrogen ion concentration is 0.005~0.030mol/L.Preferably, the oil in the rare earth bromide solution
Concentration is 3~25mg/L, and the concentration of rare earth bromide is 0.5~3.0mol/L, and hydrogen ion concentration is 0.005~0.015mol/
L.It is highly preferred that oil concentration in the rare earth bromide solution is 3~20mg/L, the concentration of rare earth bromide is 1~
1.5mol/L, hydrogen ion concentration are 0.005~0.01mol/L.It can guarantee the deoiling effect of rare earth bromide in this way.
In certain embodiments, rare earth bromide solution is passed through into the crosslinking benzene second of filling according to 30~70L/h of flow
Alkene-divinyl benzene polymers resin column.Preferably, rare earth bromide solution is according to 35~65L/h of flow by being filled with
Cross-linked styrene-divinyl benzene polymers resin column.Both the oil in rare earth bromide solution can so sufficiently adsorbed,
Diffusion, it is also ensured that the oil removal efficiency of rare earth bromide solution.
Cross-linked styrene-divinyl benzene polymers of the invention can be obtained using conventional method.For example, by benzene second
Alkene, divinylbenzene obtain cross-linked styrene-divinyl benzene polymers by the method for suspension polymerisation.Crosslinking benzene second of the invention
Alkene-divinyl benzene polymers are not limited by suspension polymerisation acquisition.Cross-linked styrene-divinyl benzene polymers specific surface
Product is not less than 900m2/ g, wet apparent density are 0.50~0.90g/ml, and wet true density is 1.00~1.50g/ml.Preferably, compare table
Area is not less than 1200m2/g.Preferably, wet apparent density is 0.65~0.75g/ml.Preferably, wet true density be 1.05~
1.15g/ml.The adsorption capacity that can guarantee polymer in this way, reaches better deoiling effect.
In the present invention, cross-linked styrene-divinyl benzene polymers are resin particle, and partial size is in 0.2~2.00mm model
Resin particle content in enclosing is 85%~100%.Preferably, resin particle content of the partial size within the scope of 0.4~1.25mm
It is 95%~100%.Its aperture of granular resin is more uniform, and the organic matter for being conducive to wherein to adsorb desorbs, with
The regeneration and recycling of resin are completed, and can guarantee the deoiling effect to Brominated rare earth solution.
In the present invention, the ratio between the diameter of the resin column and height are 1:3~20；Preferably, the diameter of resin column with
The ratio between height is 1:7~12；It is highly preferred that the diameter of resin column: being highly 1:8~10.It can both guarantee the speed of absorption in this way
Rate, and resin can be made full use of, reach maximal absorptive capacity.
In the present invention, it is, for example, less than 0.15mg/ that oil concentration, which is less than 0.2mg/L, in the rare earth bromide after the oil removing
L is for another example less than 0.1mg/L.
Cross-linked styrene used in the following embodiment-divinyl polymer performance is referring to following table.
Table 1
Oil concentration is tested with the following method in the rare earth bromide solution of following embodiment:
Rare earth is measured using " the measurement infrared spectrophotometer of water-quality petroleum and animals and plants oils " (HJ637-2012)
Oil concentration in bromide solution.Under the conditions of as defined in this standard, oil be refer to by carbon tetrachloride extraction and in wave number be
2930cm-1、2960cm-1、3030cm-1There is the substance of characteristic absorption at all or part of bands of a spectrum, mainly includes petroleum-type and dynamic plant
Object oils.
The oil of following embodiment includes extractant P507, diluent kerosene, surfactant and rare earth in ammonium hydrogen carbonate
The organic impurities that concentrate introduces.
Embodiment 1
Oil concentration is 20mg/L, bromination la concn is 1.5mol/L, hydrogen ion concentration is 0.01mol/L lanthanum bromide is molten
Liquid at room temperature, according to 50L/h flow by filled with cross-linked styrene-divinyl benzene polymers particle resin column into
Row oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Embodiment 2
Oil concentration is 3mg/L, bromination la concn is 1.5mol/L, hydrogen ion concentration is 0.01mol/L lanthanum bromide is molten
Liquid at room temperature, according to 50L/h flow by filled with cross-linked styrene-divinyl benzene polymers particle resin column into
Row oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Embodiment 3
The bromination cerium that by oil concentration be 3mg/L, bromination cerium concentration is 1.5mol/L, hydrogen ion concentration is 0.01mol/L is molten
Liquid at room temperature, according to 50L/h flow by filled with cross-linked styrene-divinyl benzene polymers particle resin column into
Row oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Embodiment 4
Oil concentration is 20mg/L, bromination la concn is 1.5mol/L, hydrogen ion concentration is 0.01mol/L lanthanum bromide is molten
Liquid at room temperature, according to 35L/h flow by filled with cross-linked styrene-divinyl benzene polymers particle resin column into
Row oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Embodiment 5
Oil concentration is 3mg/L, bromination la concn is 1.5mol/L, hydrogen ion concentration is 0.01mol/L lanthanum bromide is molten
Liquid at room temperature, according to 65L/h flow by filled with cross-linked styrene-divinyl benzene polymers particle resin column into
Row oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Comparative example 1
Oil concentration is 20mg/L, bromination la concn is 1.5mol/L, hydrogen ion concentration is 0.01mol/L lanthanum bromide is molten
Liquid at room temperature, passes through according to the flow of 100L/h filled with cross-linked styrene-divinyl benzene polymers particle resin column
Carry out oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Comparative example 2
Oil concentration is 50mg/L, bromination la concn is 1.5mol/L, hydrogen ion concentration is 0.01mol/L lanthanum bromide is molten
Liquid at room temperature, according to 50L/h flow by filled with cross-linked styrene-divinyl benzene polymers particle resin column into
Row oil removing.The diameter of resin column is 0.3 meter, is highly 3 meters.
Table 2
Present invention is not limited to the embodiments described above, without departing from the essence of the present invention, this field skill
Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.
Claims (10)
1. a kind of deoiling method of rare earth bromide solution, which comprises the steps of:
By rare earth bromide solution according to the flow of 20~80L/h by being filled with cross-linked styrene-divinyl benzene polymers
Resin column carry out oil removing, the rare earth bromide solution after obtaining oil removing；
Wherein, the oil concentration in the rare earth bromide solution is 1~35mg/L, the concentration of rare earth bromide is 0.5~
4.0mol/L, and hydrogen ion concentration is 0.005~0.030mol/L.
2. deoiling method according to claim 1, which is characterized in that the rare earth bromide is lanthanum bromide or bromination cerium
One or both of.
3. deoiling method according to claim 1, which is characterized in that the cross-linked styrene-divinyl benzene polymer
The specific surface area of object is not less than 900m2/ g, wet apparent density are 0.50~0.90g/ml, and wet true density is 1.00~1.50g/ml.
4. deoiling method according to claim 1, which is characterized in that the cross-linked styrene-divinyl benzene polymer
The specific surface area of object is not less than 1200m2/ g, wet apparent density are 0.65~0.75g/ml, and wet true density is 1.05~1.15g/ml.
5. deoiling method according to claim 1, which is characterized in that the oil concentration in the rare earth bromide solution is
3~25mg/L, the concentration of rare earth bromide is 0.5~3.0mol/L, and hydrogen ion concentration is 0.005~0.015mol/L.
6. deoiling method according to claim 1, which is characterized in that the cross-linked styrene-divinyl benzene polymer
Object is resin particle, and resin particle content of the partial size within the scope of 0.2mm~2.00mm is 85%~100%.
7. deoiling method according to claim 1, which is characterized in that the ratio between the diameter of the resin column and height are 1:
3~20.
8. deoiling method according to claim 1, which is characterized in that the ratio between the diameter of the resin column and height are 1:
7~12.
9. deoiling method according to claim 1, which is characterized in that the flow of rare earth bromide solution is 30~70L/h.
10. seeking 1~9 described in any item deoiling methods according to right, which is characterized in that oil is dense in the rare earth bromide after oil removing
Degree is less than 0.2mg/L.
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| CN107879370A (en) * | 2017-10-27 | 2018-04-06 | 包头稀土研究院 | The preparation method of oil-free carbonated rare earth |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107879370A (en) * | 2017-10-27 | 2018-04-06 | 包头稀土研究院 | The preparation method of oil-free carbonated rare earth |
Non-Patent Citations (1)
| Title |
|---|
| 张文娟等: ""聚苯乙烯树脂处理稀土皂化含油废水试验研究"", 《湿法冶金》 * |
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