CN109777948A - Technological method for extracting rubidium by flash cycle leaching of silicate - Google Patents
Technological method for extracting rubidium by flash cycle leaching of silicate Download PDFInfo
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- CN109777948A CN109777948A CN201910138678.9A CN201910138678A CN109777948A CN 109777948 A CN109777948 A CN 109777948A CN 201910138678 A CN201910138678 A CN 201910138678A CN 109777948 A CN109777948 A CN 109777948A
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- rubidium
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Abstract
The invention discloses a process method for extracting rubidium by flash cycle leaching of silicate, which is characterized in that solid ore raw materials are roasted and then subjected to flash cycle leaching-rapid dehydration process, so that the leaching rate of rubidium and the content concentration of rubidium are effectively improved; and in the subsequent extraction process, the extraction efficiency is improved and the loss rate is reduced, so that the technical index of rubidium is obviously improved, and the waste of mineral resources is effectively reduced. The process method has simple treatment flow and low production cost, and is favorable for popularization and application.
Description
Technical field
The process for extracting rubidium is leached the present invention relates to mineral processing technique field more particularly to a kind of silicate.
Background technique
Metal rubidium is a kind of extremely active and high degree of dispersion rare alkaline metal, in space technology, electronic industry, biological work
The fields such as journey, material science have a wide range of applications.So far, the mine for individually having commercial mining to be worth of rubidium is not found
Object, the main association of rubidium is in Cs lepidolite, pollucite, natural carnallite, potassium mine seawater and salt lake bittern.Discovered in recent years is a large amount of
Silicate mineral containing rubidium, currently available technology mainly extract rubidium from solid silicate, but technical process it is relatively complicated and
The loss late of rubidium is big, causes serious waste to mineral resources.Therefore, the leaching extractive technique technique for how optimizing rubidium is
It is badly in need of the technical problem urgently solved at present.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of silicate flash circulating leachings to extract rubidium
Process is leached by optimization solid silicate and extracts rubidium technical matters, while simplifying process flow, significantly improves rubidium
Leaching rate and leachate in rubidium concentration and greatly reduce the loss late of rubidium, so that the quality for significantly improving rubidium product refers to
Mark, effectively reduces the waste of mineral resources.
The purpose of the present invention is achieved by the following technical programs:
A kind of silicate flash circulating leaching provided by the invention extracts the process of rubidium, comprising the following steps:
(1) extract the preparation of stoste
(1-1) silicate ore raw material is added calcium chloride and carries out chloridising roasting, obtains fired slags, and generate chlorine；It is described
Chlorine enters chlorine gas absorption tower processing；
(1-2) described fired slags are added water and carry out flash circulating leaching and dehydration, obtain leachate and leached mud；Wherein,
Each extraction time is less than 5min, and leachate is recycled number and is greater than 8 times, and 85~90% is de- using screening in leached mud
Water, remaining 10~15% use filter-press dehydration；
(1-3) described leachate is added sodium carbonate and carries out precipitation reaction, obtains filtrate and precipitation of calcium carbonate after filtering；It is described
Precipitation of calcium carbonate carries out calcination processing and decomposes generation carbon dioxide and calcium oxide；The carbon dioxide returns to leachate and carbonic acid
In the precipitation reaction of sodium, the calcium oxide is entered step in the chlorine gas absorption tower in (1-1) to form calcium chloride back to roasting
In operation；
It is 1/7~1/10 that (1-4) described filtrate, which is concentrated by evaporation to cocnentration factor, to improve rubidium concentration, obtains concentrate, saltouts
Potassium chloride sodium chloride, distilled water；
(1-5) described concentrate is added sodium hydroxide and is prepared, and sodium hydroxide concentration is 30~40g/L concentrate, obtains
To extraction stoste；
(2) preparation of rubidium chloride product
(2-1) described extraction stoste is added t-BAMBP+ dimethylbenzene and is extracted as extractant, obtains organic phase and raffinate
Liquid；The raffinate enters step in the leaching operation of (1-2)；
(2-2) described organic phase uses concentration to be washed for the sodium hydroxide of 1.5N, and cleaning solution becomes yellow from black
When extremely colourless, washing is finished；The cleaning solution enters step in the leaching operation of (1-2)；
(2-3) it is described it is washed after it is organic be added to the hydrochloric acid that concentration is 4N and be stripped, obtain strip liquor and again
Raw organic phase；Wherein, the strip liquor is evaporated the reaction solution after being concentrated to get concentration, and the regeneration organic phase enters step
In the extraction operation of (2-1)；
Reaction solution after (2-4) described concentration is added stannic chloride pentahydrate and carries out precipitation reaction, obtains chloro-stannic acid after filtering
Rubidium and mother liquor of precipitation of ammonium；
(2-5) described rubidium chlorostannate uses the solution formed by hydrochloric acid, pink salt addition water to be washed as washing solution；
Cleaning solution after washing is successively evaporated crystallization, volatilization stannic chloride processing together with the mother liquor of precipitation of ammonium in step (2-4), obtains
Potassium chloride, sodium chloride, volatile chlorinated tin；Wherein, the potassium chloride, sodium chloride enter step in the roasting operation of (1-1), institute
Volatile chlorinated tin is stated to enter step in the adsorption operation of (2-6) absorption bottle；
Rubidium chlorostannate after (2-6) described washing carries out calcining and decomposing, obtains rubidium chloride product；Generated tin tetrachloride
Gas carries out adsorption treatment by absorption bottle.
Further, chloridising roasting temperature is 860~980 DEG C in step (1-1) of the present invention.The step (1-2)
Middle fired slags are according to weight ratio fired slags: water=1: 8~12, which are added water, carries out flash circulating leachings and dehydration, when each leaching
Between be 3~5min, leachate be recycled number be 8~15 times.The leaching rate > 85% after the processing of the step (1-2).
The concentration of t-BAMBP is 1.0mol/L in step (2-1) extractant；To be extracted compared to O/A=1~3.The step
It is 6~8N that strip liquor, which is concentrated by evaporation to acidity, in (2-3).The concentration difference of hydrochloric acid, pink salt in step (2-5) the washing solution
For 4N, 0.1N；The dosage for washing solution is 8~15mL/g.Rb/ times, and washing times are 2~5 times.Step (2-6) washing
The temperature of rubidium chlorostannate its calcining and decomposing afterwards is 650~720 DEG C.
The invention has the following advantages:
(1) present invention optimizes solid silicates to extract rubidium technical matters, at flash circulating leaching-fast dewatering
Reason, fired slags leach coarse size by flash, quick filtering means dehydration may be implemented, and rubidium loses less in leached mud.In this way, not
Only process is simple, highly shortened processing time (prior art leaches dehydration and needs 3h or more), and multiple circulating leaching
It ensure that higher rubidium leaching rate (leaching rate > 85%), also effectively increase rubidium concentration in leachate, be subsequent extraction work
Cost is saved, is also the processing of subsequent extraction efficiency and byproduct, the quality index of rubidium product provides guarantee.
(2) present invention decomposites calcium oxide, flue gas CO in the preparatory phase for extracting stoste, byproduct calcination of calcium carbonate2.The former
Calcium oxide enters chlorine adsorption tower absorption chlorine as adsorbent, and the calcium chloride of formation is used for the chlorination of roasting operation of the present invention
Agent；The latter's flue gas CO2Into solution purification is used in the precipitation reaction of leachate and sodium carbonate, to realize environmental protection and synthesis
Utilize Double-linkage.
(3) preparatory phase of the invention in rubidium chloride product, organic phase are washed using 1.5N sodium hydroxide solution, can
With the nonferrous metal ion in complete washing removal organic phase, and less than 10%, (prior art uses the washing loss rate of rubidium
Water washing is distilled, 35%) the washing loss rate of rubidium is greater than.In addition, the washing of rubidium chlorostannate, is the chlorine tin in order to deviate from co-precipitation
Sour potassium, sodium, but the prior art is adopted and is washed with distilled water, and the washing loss rate of rubidium is big (washing loss rate is 30% or more), and this
Invention, as cleaning solution, both can be washed completely using 4N hydrochloric acid 0.1N tin-salt solution and remove potassium chlorostannate, sodium, and rubidium is washed
Washing loss late can control 0.15%.The subsequent carrying out washing treatment process of the present invention also provides for the raising of the rubidium rate of recovery into one
The guarantee of step.
(4) present invention significantly improves the technical indicator of rubidium, thus effectively by the leaching extractive technique technique of optimization rubidium
Reduce the waste of mineral resources.And process flow is simple, production cost is low, is conducive to promotion and application.
Detailed description of the invention
Below in conjunction with embodiment and attached drawing, the present invention is described in further detail:
Fig. 1 is that silicate flash circulating leaching of the embodiment of the present invention extracts the preparation process for extracting stoste in the process of rubidium
Flow chart；
Fig. 2 is the preparation that silicate flash circulating leaching of the embodiment of the present invention extracts rubidium chloride product in the process of rubidium
Process flow chart.
Specific embodiment
The embodiment of the present invention is respectively using the mixture of mica and mica and feldspar as ore raw materials, Rb2O3Content
For 0.08~1.2% (being shown in Table 1).
As shown in Figure 1 and Figure 2, a kind of silicate flash circulating leaching of the embodiment of the present invention extracts the process of rubidium, step
It is rapid as follows:
(1) extract the preparation of stoste
(1-1) silicate ore raw material is added calcium chloride and carries out chloridising roasting at a temperature of 900 DEG C, and the dosage of calcium chloride is
The 70wt% of silicate ore raw material, calcining time 90min obtain fired slags, and generate chlorine；Wherein, chlorine enters chlorine
The processing of aspiration tower；
(1-2) above-mentioned fired slags are according to weight ratio fired slags: water=1: 10, which are added water, carries out flash circulating leaching and dehydration,
Obtain leachate and leached mud；Wherein, each extraction time is 4min, and it is 10 times that number, which is recycled, in leachate, leached mud
In 87% using screening and dewatering, remaining 13% use filter-press dehydration；The leaching rate of each embodiment is as shown in table 1.
(1-3) above-mentioned leachate is added sodium carbonate and carries out precipitation reaction, obtains filtrate and precipitation of calcium carbonate after filtering；Carbonic acid
Calcium precipitate carries out calcination processing and decomposes generation carbon dioxide and calcium oxide, wherein carbon dioxide returns to leachate and sodium carbonate
Precipitation reaction in be used for solution purification, calcium oxide enter step in the chlorine gas absorption tower in (1-1) as adsorbent adsorb chlorine
Gas is returned in roasting operation with forming calcium chloride；
It is 1/8 that (1-4) above-mentioned filtrate, which is concentrated by evaporation to cocnentration factor, to improve rubidium concentration, obtains concentrate, potassium chloride of saltouing
Sodium chloride, distilled water；
(1-5) above-mentioned concentrate is added sodium hydroxide and is prepared, and the dosage of sodium hydroxide is 35g/L concentrate, obtains
Extract stoste；
(2) preparation of rubidium chloride product
T-BAMBP+ dimethylbenzene is added in (2-1) above-mentioned extraction stoste, and as extractant, (concentration of t-BAMBP is in extractant
It 1.0mol/L) is extracted, compares O/A=2, obtain organic phase and raffinate；Raffinate enters step the leaching operation of (1-2)
In；
(2-2) above-mentioned organic phase uses concentration to be washed for the sodium hydroxide of 1.5N, and cleaning solution becomes yellow from black
When extremely colourless, washing is finished；Cleaning solution enters step in the leaching operation of (1-2)；
(2-3) it is above-mentioned it is washed after organic phase according to compared to O/A=10 be added concentration be 4N hydrochloric acid be stripped,
Obtain strip liquor and regeneration organic phase；Wherein, it is the reaction after 6~8N is concentrated that strip liquor, which is evaporated and is concentrated into acidity,
Liquid, regeneration organic phase enter step in the extraction operation of (2-1)；
Reaction solution after (2-4) above-mentioned concentration is added stannic chloride pentahydrate and carries out precipitation reaction, obtains chloro-stannic acid after filtering
Rubidium and mother liquor of precipitation of ammonium；
(2-5) above-mentioned rubidium chlorostannate uses the solution formed by hydrochloric acid, pink salt addition water as washing solution (washing solution
Middle hydrochloric acid, pink salt concentration be respectively 4N, 0.1N) washed, wash solution dosage be 10mL/g.Rb/ times, washing times
It is 3 times；Cleaning solution after washing is successively evaporated crystallization, at the stannic chloride that volatilizees together with the mother liquor of precipitation of ammonium in step (2-4)
Reason, obtains potassium chloride, sodium chloride, volatile chlorinated tin；Wherein, potassium chloride, sodium chloride enter step the roasting operation of (1-1)
In, volatile chlorinated tin enters step in the adsorption operation of (2-6) absorption bottle；
Rubidium chlorostannate after (2-6) above-mentioned washing decompose in 680 DEG C of temperature lower calcinations, obtains rubidium chloride product；Institute
The tin tetrachloride gas of generation carries out adsorption treatment by absorption bottle.
1 various embodiments of the present invention ore raw materials of table, Rb2O3Content, leaching rate technical indicator
| Embodiment | Ore raw materials | Rb2O3Content % | Leaching rate % |
| Embodiment one | Mica 15%+ feldspar 85% | 0.082 | 86 |
| Embodiment two | Mica 100% | 0.51 | 93 |
| Embodiment three | Mica 80%+ feldspar 20% | 1.20 | 95 |
Its RbCl content of the rubidium chloride product that the embodiment of the present invention is prepared reaches 99.5% or more (being shown in Table 2), matter
Amount meets rubidium chloride industrial product quality standard (Q/TJTE 17-2004).Leached mud, which meets mixed mud consolidation waterproofing agent quality, to be wanted
It asks.The sodium chloride and potassium chloride saltoutd meets respective product quality requirement after FLOTATION SEPARATION.
The primary chemical for the rubidium chloride product that 2 embodiment of the present invention of table is prepared forms (%)
| Project | RbCl | Al | Fe | K | Na |
| Content | 99.64 | 0.00082 | 0.0002 | 0.0477 | 0.0091 |
| Project | Li | Cs | Mg | Ca | Pb |
| Content | 0.0081 | 0.1801 | 0.00070 | 0.00470 | 0.00036 |
Claims (8)
1. the process that a kind of silicate flash circulating leaching extracts rubidium, it is characterised in that the following steps are included:
(1) extract the preparation of stoste
(1-1) silicate ore raw material is added calcium chloride and carries out chloridising roasting, obtains fired slags, and generate chlorine；The chlorine
Into chlorine gas absorption tower processing；
(1-2) described fired slags are added water and carry out flash circulating leaching and dehydration, obtain leachate and leached mud；Wherein, every time
Extraction time be less than 5min, leachate be recycled number be greater than 8 times, in leached mud 85~90% using screening and dewaterings, its
Remaining 10~15% use filter-press dehydration；
(1-3) described leachate is added sodium carbonate and carries out precipitation reaction, obtains filtrate and precipitation of calcium carbonate after filtering；The carbonic acid
Calcium precipitate carries out calcination processing and decomposes generation carbon dioxide and calcium oxide；The carbon dioxide is back to leachate and sodium carbonate
In precipitation reaction, the calcium oxide is entered step in the chlorine gas absorption tower in (1-1) to form calcium chloride back to roasting operation
In；
It is 1/7~1/10 that (1-4) described filtrate, which is concentrated by evaporation to cocnentration factor, to improve rubidium concentration, obtains concentrate, chlorination of saltouing
Potassium sodium chloride, distilled water；
(1-5) described concentrate is added sodium hydroxide and is prepared, and sodium hydroxide concentration is 30~40g/L concentrate, is extracted
Stoste；
(2) preparation of rubidium chloride product
(2-1) described extraction stoste is added t-BAMBP+ dimethylbenzene and is extracted as extractant, obtains organic phase and raffinate；Institute
Raffinate is stated to enter step in the leaching operation of (1-2)；
(2-2) described organic phase uses concentration to be washed for the sodium hydroxide of 1.5N, and cleaning solution becomes yellow to nothing from black
When color, washing is finished；The cleaning solution enters step in the leaching operation of (1-2)；
(2-3) it is described it is washed after it is organic be added to concentration be 4N hydrochloric acid be stripped, obtaining strip liquor and regeneration has
Machine phase；Wherein, the strip liquor is evaporated the reaction solution after being concentrated to get concentration, and the regeneration organic phase enters step (2-
1) in extraction operation；
Reaction solution after (2-4) described concentration is added stannic chloride pentahydrate and carries out precipitation reaction, obtained after filtering rubidium chlorostannate and
Mother liquor of precipitation of ammonium；
(2-5) described rubidium chlorostannate uses the solution formed by hydrochloric acid, pink salt addition water to be washed as washing solution；Washing
Cleaning solution afterwards is successively evaporated crystallization, volatilization stannic chloride processing together with the mother liquor of precipitation of ammonium in step (2-4), obtains chlorination
Potassium, sodium chloride, volatile chlorinated tin；Wherein, the potassium chloride, sodium chloride enter step in the roasting operation of (1-1), described to wave
Hair property stannic chloride enters step in the adsorption operation of (2-6) absorption bottle；
Rubidium chlorostannate after (2-6) described washing carries out calcining and decomposing, obtains rubidium chloride product；Generated tin tetrachloride gas
Adsorption treatment is carried out by absorption bottle.
2. the process that silicate flash circulating leaching according to claim 1 extracts rubidium, it is characterised in that: the step
Suddenly chloridising roasting temperature is 860~980 DEG C in (1-1).
3. the process that silicate flash circulating leaching according to claim 1 extracts rubidium, it is characterised in that: the step
Suddenly in (1-2) fired slags according to weight ratio fired slags: water=1: 8~12 be added water carry out flash circulating leachings and dehydration, every time
Extraction time be 3~5min, leachate be recycled number be 8~15 times.
4. the process that silicate flash circulating leaching according to claim 1 or 3 extracts rubidium, it is characterised in that: warp
Leaching rate > 85% after the processing of the step (1-2).
5. the process that silicate flash circulating leaching according to claim 1 extracts rubidium, it is characterised in that: the step
Suddenly the concentration of t-BAMBP is 1.0mol/L in (2-1) extractant；To be extracted compared to O/A=1~3.
6. the process that silicate flash circulating leaching according to claim 1 extracts rubidium, it is characterised in that: the step
Suddenly it is 6~8N that strip liquor, which is concentrated by evaporation to acidity, in (2-3).
7. the process that silicate flash circulating leaching according to claim 1 extracts rubidium, it is characterised in that: the step
Suddenly (2-5) washs hydrochloric acid in solution, the concentration of pink salt is respectively 4N, 0.1N；The dosage for washing solution is 8~15mL/g.Rb/
Secondary, washing times are 2~5 times.
8. the process that silicate flash circulating leaching according to claim 1 extracts rubidium, it is characterised in that: the step
Suddenly the temperature of rubidium chlorostannate its calcining and decomposing after (2-6) washing is 650~720 DEG C.
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| CN111893309A (en) * | 2020-08-11 | 2020-11-06 | 广东省科学院资源综合利用研究所 | Comprehensive recycling method for full recycling of cigarette ash |
| CN112239221A (en) * | 2020-10-19 | 2021-01-19 | 广东省科学院资源综合利用研究所 | Method for extracting rubidium chloride from rubidium-containing high-salinity brine |
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