CN111647744B - Method for recovering organic and rare earth from bastnaesite extraction three phases - Google Patents
Method for recovering organic and rare earth from bastnaesite extraction three phases Download PDFInfo
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Abstract
The invention discloses a method for recovering organic and rare earth from bastnaesite extraction three phases, which comprises the following steps: s1, separately collecting according to different formation mechanisms of the three-phase emulsion, then performing centrifugal separation to obtain filter residue and filtrate, adding a cosolvent into the three-phase emulsion when the collected three-phase emulsion is formed by organic supersaturated emulsification, and then performing centrifugal separation; s2, transferring the filter residue into a reaction tank, and adding industrial sulfuric acid into the reaction tank until the filter residue is completely carbonized; and S3, adding water into the reaction tank to make the acidity in the reaction tank be 0.5-1.2 mol/L. Through adopting centrifugal mode to realize the separation, not only practiced thrift the cosolvent, still shortened processing cycle, simultaneously, adopt the carbonization to handle the three-phase carbonization that can directly form organic, tombarthite and other impurity, need not handle useless organic in the waste water again like this, practiced thrift the waste water treatment cost, can not cause the enrichment of non-tombarthite impurity on the production line, overcome prior art's not enough.
Description
Technical Field
The invention relates to the technical field of bastnaesite hydrometallurgy, in particular to a method for recovering organic and rare earth from bastnaesite extraction three phases.
Background
Now it isMost of rare earth hydrometallurgical production enterprises in Sichuan province are Yak plateau rare earth ores in crown county of Sichuan province, the ore belongs to bastnaesite, the general rare earth grade of the ore is about 65%, the content of non-rare earth impurities F is about 7.0%, the content of Ca is about 1.5%, and SiO is about2The content of the rare earth chloride is about 1.2 percent, and other non-rare earth impurities such as barite and non-rare earth impurities containing , iron, aluminum and the like are also included, so that the mixed rare earth chloride produced in the rare earth hydrometallurgy process can form non-rare earth impurities containing calcium, fluorine, silicon oxide or silicon, sulfate radical and the like, three phases are easily formed near a feed inlet of an extraction section of extraction in the production process and are enriched in a space occupying an extraction tank body in a squeezing manner, and stable and difficultly treated three phases are formed, and the other phase is an emulsified three phase formed by loading organic supersaturation, so that the situation is easily generated in a rare earth soap section of extraction, and the two three-phase extraction substances are generated in the production process, and the loss of extraction organic and rare earth materials is easily caused.
In order to treat the triphase substances, two modes are mainly adopted at present, namely, the mode is mainly used for preventing the generation of the triphase substances, namely, the impurities of the mixed rare earth chloride and the impurities of acid and alkali entering an extraction tank are mainly controlled, but the mode can only reduce the triphase substances but cannot completely eliminate the triphase substances; and the second is to treat the generated three phases by adopting a mode of recovering organic matters and rare earth. Chinese patent CN108330301A discloses a method for treating three-phase emulsion in bastnaesite smelting separation, and specifically discloses the following treatment steps: collecting the three-phase emulsion, adding an auxiliary leaching agent, filtering, carrying out alkali-to-acid dissolution on filter residues to obtain a rare earth solution, and standing and clarifying the filtrate to obtain an organic phase and a rare earth water phase. The treatment method realizes comprehensive recycling of resources and recovers the organic matters and rare earth in the three-phase emulsion, but the method needs to use a sodium hydroxide leaching aid and filter pressing, so that the treatment cost is overhigh, the treatment period is overlong, the waste organic matters in the wastewater need to be treated, and the subsequent treatment cost is overhigh.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the method for recovering the organic and rare earth from the three phases of the bastnaesite extraction is provided, the separation is realized by adopting a centrifugal mode, so that the cosolvent is saved, the treatment period is shortened, meanwhile, the carbonization treatment is adopted, the three phases formed by the organic, rare earth and other impurities can be directly carbonized, the waste organic in the wastewater is not required to be treated, the wastewater treatment cost is saved, the impurities can be removed, the enrichment of non-rare earth impurities on a production line is avoided, and the defects of the prior art are overcome.
The technical scheme adopted by the invention is as follows: the method for recovering organic and rare earth from the three phases of bastnaesite extraction is characterized by comprising the following steps of:
s1, separately collecting three-phase substances according to different formation mechanisms of the three-phase substances, then separating the three-phase substances from a liquid phase in a centrifugal separation mode to obtain filter residues and filtrate, wherein when the collected three-phase emulsion is formed by organic supersaturated emulsification, a cosolvent for changing the hydrophilicity of the three-phase emulsion is added into the three-phase emulsion, and then the centrifugal separation treatment is carried out;
s2, transferring the filter residue into a reaction tank, and adding industrial sulfuric acid into the reaction tank until the filter residue is completely carbonized;
s3, after the carbonization reaction is finished, adding water into the reaction tank to ensure that the acidity in the reaction tank is 0.5-1.2mol/L, then heating to above 80 ℃, and stirring for reaction for 1-2 hours;
s4, after the stirring reaction is finished, filtering and separating to obtain carbon-containing waste residues and carbonized filtrate, transferring the carbon-containing waste residues to a waste residue treatment process, adding soluble sodium salt or soluble potassium salt into the carbonized filtrate to perform double salt precipitation treatment, filtering and washing the filtrate to obtain rare earth sulfate double salt;
and clarifying and fractionating the filtrate in S5 and S2 to obtain an organic phase and a rare earth water phase.
In the method, the triphase substance generally belongs to a chelate, a cosolvent is directly added, organic and valuable rare earth is difficult to recover, and a direct filtering mode is adopted, so that the problems of long filtering period and difficult recovery are caused by the hydrophilicity of the triphase emulsion. Further, filter residue after centrifugal filtration is carbonized, and the reaction principle is as follows:
wherein A is-Represents an organic ion.
Further, after the carbonization reaction, the acidity of the carbonized filtrate is adjusted to realize the separation of rare earth ions and carbon residue, and the reaction principle is as follows:
RE3++SO4 2-＝RE2(SO4)3
the filtered carbon-containing waste residue is transferred to a mine landfill, an organic phase is completely carbonized and removed, carbonized filtrate can be directly transferred to a double salt precipitation process to carry out double salt precipitation and recover rare earth, acid dissolution is carried out by sulfuric acid, non-rare earth impurities such as calcium, barium and the like are still left in the carbon residue and are not left in the filtrate, so that the rare earth is effectively recovered without enrichment of the non-rare earth impurities, soluble sodium salt or soluble potassium salt is subsequently added into the carbonized filtrate, rare earth ions in the carbonized filtrate are recovered in a double salt precipitation mode, and rare earth sulfate double salt (for example, Na can be obtained) is obtained after filtration2SO4·RE2(SO4)3) The rare earth sulfate double salt can be converted by soluble carbonate and then dissolved by hydrochloric acid to obtain mixed rare earth chloride, the mixed rare earth chloride can be used as a rare earth extraction raw material, the residual liquid after filtration can be discharged after reaching the standard due to simple treatment without containing waste organic matter, the treatment cost is low, and the problems of high treatment cost and long treatment period of the existing treatment process are solved.
In the method of the present invention, in order to better perform centrifugal separation of the triphase, after collecting the triphase, the triphase is first subjected to static fractionation to remove a part of the organic phase, and then subjected to centrifugal separation.
In the invention, when the collected three-phase emulsion is formed by organic supersaturated emulsification or formed by excessively large organic three-phase load, a cosolvent for changing the hydrophilicity of the three-phase emulsion needs to be added into the three-phase emulsion, and then the three-phase emulsion is subjected to standing fractionation treatment, so that the standing fractionation treatment effect is improved, and the working strength of centrifugal separation is reduced. Therefore, by respectively treating the three-phase substances with different sources, the separation effect is ensured, the use amount of the cosolvent can be greatly reduced, the treatment cost is saved, and the treatment period is shortened.
Further, the cosolvent is hydrochloric acid, soluble organic or soluble carbonate, and hydrochloric acid is preferred.
In the invention, the soluble sodium salt or the soluble potassium salt is one of sodium carbonate, sodium bicarbonate, sodium chloride, sodium hydroxide, sodium sulfate, potassium carbonate, potassium chloride and potassium hydroxide. Still further, the soluble sodium salt is preferably sodium carbonate.
Further, in S4, the filtered water and the washed water are transferred to a wastewater treatment process for standard treatment and then discharged.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the invention realizes the separation of three-phase substances by adopting a centrifugal mode, not only saves cosolvent, but also shortens the treatment period, simultaneously, the carbonization treatment can be adopted to directly carbonize three phases formed by organic, rare earth and other impurities, when the rare earth ions in the three-phase emulsion are recovered, the organic phase in the three-phase emulsion is removed, further no waste organic is generated, the wastewater treatment cost is saved, the non-rare earth impurities can be removed by the subsequently formed rare earth sulfate double salt, the enrichment of the non-rare earth impurities on a production line can not be caused, the defects of the prior art are overcome, the experiment shows that the method provided by the invention is adopted to recover and extract the organic and rare earth in the three phases, the recovery rate of the organic phase reaches 65%, the recovery rate of the rare earth reaches 85%, the treatment period is only 8 h/batch, and the technical effect is outstanding.
Drawings
FIG. 1 is a process flow diagram of a method for recovering organic and rare earth from bastnaesite extraction three phases according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
As shown in fig. 1, a method for recovering organic and rare earth from bastnaesite extraction three phases includes the following steps:
s1, collecting a common three-phase emulsion (namely, a first three-phase emulsion in figure 1) formed by non-rare earth impurities, organic substances and rare earth, standing and fractionating to remove a part of organic phase, and separating the three-phase emulsion from a liquid phase in a centrifugal separation mode to obtain filter residue and filtrate;
s2, transferring the filter residue into a reaction tank, and slowly adding industrial sulfuric acid (with the concentration of 98%) into the reaction tank until the carbonization reaction is finished;
s3, after the carbonization reaction is finished, adding water into the reaction tank to ensure that the acidity in the reaction tank is 0.5-1.2mol/L (a specific acidity value is selected according to actual conditions), then heating to about 80 ℃, and stirring for reaction for 1.5 h;
s4, after the stirring reaction is finished, filtering and separating to obtain carbon-containing waste residues and carbonized filtrate, transferring the carbon-containing waste residues to a waste residue treatment process, adding sodium carbonate into the carbonized filtrate to perform double salt precipitation treatment, filtering and washing the carbonized filtrate to obtain rare earth sulfate double salt, dissolving the rare earth sulfate double salt with acid to obtain a mixed rare earth chloride solution, transferring the filtered water and the washed washing water into a wastewater treatment process to reach the standard, and discharging the treated water and the washing water;
and clarifying and fractionating the filtrate in S5 and S2 to obtain an organic phase and a rare earth water phase.
Example 2
As shown in fig. 1, a method for recovering organic and rare earth from bastnaesite extraction three phases includes the following steps:
s1, collecting a three-phase emulsion (namely, a second three-phase emulsion in figure 1) formed by organic supersaturated emulsification or formed by excessive organic three-phase loading, standing and fractionating to remove a part of an organic phase, adding hydrochloric acid into the three-phase emulsion, and then separating the three-phase emulsion from a liquid phase in a centrifugal separation mode to obtain filter residue and filtrate;
s2, transferring the filter residue into a reaction tank, and slowly adding industrial sulfuric acid (with the concentration of 98%) into the reaction tank until the carbonization reaction is finished;
s3, after the carbonization reaction is completed, adding water into the reaction tank to ensure that the acidity in the reaction tank is 0.5-1.2mol/L (a specific acidity value is selected according to actual conditions), then heating to about 80 ℃, and stirring for reaction for 1.5 h;
s4, after the stirring reaction is finished, filtering and separating to obtain carbon-containing waste residues and carbonized filtrate, transferring the carbon-containing waste residues to a waste residue treatment process, adding sodium chloride into the carbonized filtrate to perform double salt precipitation treatment, filtering and washing the filtrate to obtain rare earth sulfate double salt, dissolving the rare earth sulfate double salt with acid to obtain a mixed rare earth chloride solution, transferring the filtered water and the washed washing water into a wastewater treatment process to reach the standard, and discharging the treated water and the washing water;
and clarifying and fractionating the filtrate in S5 and S2 to obtain an organic phase and a rare earth water phase.
Example 3
As shown in fig. 1, a method for recovering organic and rare earth from bastnaesite extraction three phases includes the following steps:
s1, collecting general three-phase emulsions (namely, a first three-phase emulsion in figure 1) formed by non-rare earth impurities, organic substances and rare earth and three-phase emulsions (namely, a second three-phase emulsion in figure 1) formed by organic supersaturated emulsification or organic three-phase overload, standing and fractionating the first three-phase emulsion, removing part of organic phases, separating by a centrifugal separation method to obtain filter residues and filtrate, standing and fractionating the second three-phase emulsion, removing the organic phases, adding hydrochloric acid, separating by a centrifugal separation method to obtain the filter residues and the filtrate, and respectively combining the filter residues and the filtrate of the first three-phase emulsion and the filtrate of the second three-phase emulsion;
s2, transferring the filter residue into a reaction tank, and slowly adding industrial sulfuric acid (with the concentration of 98%) into the reaction tank until the carbonization reaction is finished;
s3, after the carbonization reaction is completed, adding water into the reaction tank to ensure that the acidity in the reaction tank is 0.5-1.2mol/L (a specific acidity value is selected according to actual conditions), then heating to about 80 ℃, and stirring for reaction for 1.5 h;
s4, after the stirring reaction is finished, filtering and separating to obtain carbon-containing waste residues and carbonized filtrate, transferring the carbon-containing waste residues to a waste residue treatment process, adding sodium carbonate into the carbonized filtrate to perform double salt precipitation treatment, filtering and washing the carbonized filtrate to obtain rare earth sulfate double salt, dissolving the rare earth sulfate double salt with acid to obtain a mixed rare earth chloride solution, transferring the filtered water and the washed washing water into a wastewater treatment process to reach the standard, and discharging the treated water and the washing water;
and clarifying and fractionating the filtrate in S5 and S2 to obtain an organic phase and a rare earth water phase.
According to the method for recovering the organic and rare earth from the three phases extracted from the bastnaesite, the recovery rate of the organic phase reaches 65%, the recovery rate of the rare earth reaches 85%, the treatment period is only 8 h/batch, the rare earth and the organic phase are effectively recovered, the treatment period is obviously shortened, the treatment cost is obviously reduced, the technical effect is remarkable, and the method is worthy of popularization and application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (6)
1. A method for recovering organic and rare earth from a bastnaesite extraction three-phase is characterized by comprising the following steps:
s1, separately collecting three-phase emulsion according to different formation mechanisms of the three-phase emulsion, and then separating the three-phase emulsion from a liquid phase in a centrifugal separation mode to obtain filter residue and filtrate, wherein when the collected three-phase emulsion is formed by organic supersaturated emulsification, a cosolvent for changing the hydrophilicity of the three-phase emulsion is added into the three-phase emulsion, and then the three-phase emulsion is subjected to centrifugal separation treatment;
s2, transferring the filter residue into a reaction tank, and adding industrial sulfuric acid into the reaction tank until the filter residue is completely carbonized;
s3, after the carbonization reaction is finished, adding water into the reaction tank to ensure that the acidity in the reaction tank is 0.5-1.2mol/L, then heating to above 80 ℃, and stirring for reaction for 1-2 hours;
s4, after the stirring reaction is finished, filtering and separating to obtain carbon-containing waste residues and carbonized filtrate, and transferring the carbon-containing waste residues to a waste residue treatment process; adding soluble sodium salt or soluble potassium salt into the carbonized filtrate to carry out double-salt precipitation treatment, filtering and washing the filtrate to obtain rare earth sulfate double salt;
and clarifying and fractionating the filtrate in S5 and S2 to obtain an organic phase and a rare earth water phase.
2. The method of claim 1 wherein the three-phase emulsion is collected and then subjected to static fractionation to remove the organic phase followed by centrifugal separation, and in the case where the three-phase emulsion is formed by supersaturated emulsification of organic phase, the organic phase is subjected to static fractionation, then the co-solvent is added, and finally the organic phase is subjected to centrifugal separation.
3. The method for recovering organics and rare earths from a bastnaesite extraction three-phase system of claim 2 wherein the co-solvent is hydrochloric acid, a soluble organic or a soluble carbonate.
4. The method for recovering organic and rare earth from a bastnaesite extraction three-phase as claimed in claim 3, wherein the soluble sodium salt or soluble potassium salt is one of sodium carbonate, sodium bicarbonate, sodium chloride, sodium hydroxide, potassium carbonate, potassium chloride, and potassium hydroxide.
5. The process for the recovery of organic and rare earths from the bastnaesite extraction three-phase according to claim 4, wherein the soluble sodium salt is sodium carbonate.
6. The method for recovering organic and rare earth from the bastnaesite extraction three-phase as claimed in claim 1, wherein the filtered water and the washed water are transferred to a wastewater treatment process for standard treatment and then discharged at S4.
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