CN104789800A - Method for extracting rubidium from saline lake brine - Google Patents
Method for extracting rubidium from saline lake brine Download PDFInfo
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- CN104789800A CN104789800A CN201510234040.7A CN201510234040A CN104789800A CN 104789800 A CN104789800 A CN 104789800A CN 201510234040 A CN201510234040 A CN 201510234040A CN 104789800 A CN104789800 A CN 104789800A
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Abstract
The invention provides a method for extracting rubidium from saline lake brine. The method comprises the following steps: (1) adding water-soluble carbonate precipitated magnesium ions into the saline lake brine, carrying out solid-liquid separation to obtain a first filtrate and a second filtrated cake, and enabling the content of magnesium ions in the first filtrate to be lower than 50mg/L; (2) extracting rubidium from the first filtrate by using 4-tert-butyl-2-(alpha-methylbenzyl) phenol as an extractant and using an extraction-backextraction alternate countercurrent extraction process in an environment that the amount-of-substance concentration of [OH-] is 0.8-1mol/L, wherein the concentration of 4-tert-butyl-2-(alpha-methylbenzyl) phenol in the extractant is 0.5-1mol/L. According to the method, rubidium is effectively obtained from brine with high concentration of potassium, and the efficiency of rubidium extraction is increased.
Description
Technical field
The present invention relates to salt lake extractive technique, the especially extraction of rubidium element in salt lake.
Background technology
The reasons such as the areal variation of the appearance due to world wide energy dilemma and the growth to rubidium product demand and the distribution of rubidium ore resources is large, cause rubidium ore price to go up.The production cost extracting rubidium from solid mineral is very high, salt lake brine rubidium aboundresources, but up to the present develop still for blank, salt lake rubidium resource exploration data is few and outmoded, the research that salt lake brine puies forward rubidium method has no system report always, and the precedent of rubidium resource is not also exploited in Salt Lake Area.
Along with continually developing of Qinghai Salt Lake resource, the comprehensive utilization of salt lake resources more and more receives the concern of people, and wherein the exploitation of rubidium rare and scatter element obtain very large attention.And mostly the Bian that opens of salt lake resources is a certain mineral of single exploitation, gets richness and abandons poor, cause the huge waste of resource.The rubidium existed with bittern form, the salt lake being extensively distributed in the ground such as Qinghai, Tibet, GEOTHERMAL WATER, the rubidium resource in salt lake brine will be the emphasis of following exploitation, and from salt lake brine, Extraction and separation rubidium is significant and become extremely urgent task.
Extraction process separation and Extraction rubidium has certain superiority in production.It is substituted phenol that current extraction process applies maximum extraction agents, and substituted phenol is more with t-BAMBP research.It is comparatively easy that t-BAMBP has synthesis, steady sources, and studies in China is more, technology relative maturity, and the advantage such as can to produce in batches, industrially has broad application prospects.T-BAMBP in the basic conditions to the coordination selectivity of rubidium far away higher than neutral or acidic conditions, thus the basicity of extraction system is very important.Regulate the alkalescence of bittern must produce a large amount of magnesium hydrate precipitates, therefore, need before extraction to add technology for removal of magnesium from phosphorous.Current Hunan University Liu and brightness
[1]propose except magnesium method be add sodium hydroxide demagging, there is a lot of limitation, because of produce magnesium hydrate precipitate itself there is adsorptivity, a large amount of rubidiums can be taken away in precipitation process, cause the rate of recovery to reduce; And magnesium hydroxide exists the problem of filtration difficulty, be difficult to be applied in actual production, limit extraction process application industrially.Develop the new magnesium method that removes and become the key issue solving extraction process separation and Extraction rubidium from bittern.
The extraction of rubidium is not difficult to itself, and difficulty is the extracting and separating of carrying out Rubidium from the bittern of the potassium ion of high-content.T-BAMBP is while extraction rubidium, and K, Na are also extracted simultaneously, and when improving the rate of recovery of rubidium by the mode of multi-stage solvent extraction, the percentage extraction of potassium also can correspondingly improve, and is difficult to the object reaching the separation of rubidium potassium.Although t-BAMBP is to the existing research of the extraction of rubidium ion, but from the true salt lake brine of high density K, Na, extract the research report of Rubidium seldom, there is twice level Four extraction of bibliographical information at present, the washing of Pyatyi, within the mass concentration carrying potassium in rubidium technical process of twice two-stage back extraction is only 10 times of rubidium mass concentration
[2].Mass concentration for potassium is that the extraction process of the high potassium content bittern of the 800-3000 scope of rubidium mass concentration have not been reported so far.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of method extracting rubidium from salt lake brine, comprising the steps:
Step one: add water soluble carbonate precipitation magnesium ion in salt lake brine, obtain the first filtrate and the second filter cake after solid-liquid separation, to make in described first filtrate magnesium ion content at below 50mg/L;
Step 2: at [OH
-] substance withdrawl syndrome is under the environment of 0.8 ~ 1mol/L, with the 4-tertiary butyl-2-(α-methylbenzyl) phenol for extraction agent, utilize extraction reciprocal cross for counter-current extraction technique, from described first filtrate, extract rubidium;
Wherein, in described extraction agent, the concentration of the 4-tertiary butyl-2-(α-methylbenzyl) phenol is 0.5 ~ 1mol/L; Described extraction reciprocal cross for counter-current extraction processing condition is: be in a ratio of 0.5 ~ 2:1; Temperature 5 ~ 30 DEG C; Rotating speed 3000 ~ 4000r/min; Back extraction condition is: be in a ratio of 0.5 ~ 2:1; Temperature 15 ~ 30 DEG C; Rotating speed 3000 ~ 4000r/min; Mineral acid substance withdrawl syndrome is 0.02 ~ 0.5mol/L.
Further, described step one comprises following operation:
First, described water soluble carbonate is made into 20 ~ 25% carbonate aqueous solutions, adds in described salt lake brine and stir more than 10min, after solid-liquid separation, obtain filtrate A, filter cake A; Wherein, the amount of substance of described water soluble carbonate is 1 ~ 1.5:1 with the ratio of the amount of substance of described magnesium ion;
Then, get described carbonate aqueous solution and be added in described filtrate A, stir more than 10min, after solid-liquid separation, obtain described first filtrate, filter cake B; Wherein, the amount of substance of described water soluble carbonate is 0.25 ~ 0.5:1 with the ratio of the amount of substance of described magnesium ion; Described filter cake A, filter cake B merge into described first filter cake.
Further, also comprise step 3: from described first filter cake, reclaim rubidium, comprise following operation:
First, at 500 ~ 900 DEG C of temperature lower calcination 30 ~ 60min after being dried by described first filter cake, calcinate is obtained;
Then, with water cleaning after described calcinate cooling, the second filtrate and the second filter cake is obtained by solid-liquid separation;
Wherein, described second filtrate repeating said steps two carries out the extraction of rubidium.
Further, in described step 3, for cleaning 0.5 ~ 2 times that the quality of the water of described calcinate is described calcinate quality.
Further, be also included in before carrying out described step one and described salt lake brine is diluted, make Mg content lower than 25g/L.
Further, described carbonate selects sodium carbonate.
Beneficial effect:
The present invention effectively obtains rubidium from containing the salt lake brine of high potassium concentration, improves the extraction efficiency of rubidium.Especially for the existing limitation except magnesium method, select water soluble carbonate demagging, the precipitation precipitation of generation is easily filtered; The add-on of water soluble carbonate, without the need to strictly controlling, regulates almost without impact follow-up extraction basicity.Carry out the filtrate Mg content after twice demagging and be down to below 50mg/L, directly can extract rubidium under alkaline environment.And be deposited in certain temperature lower calcination after washing by what produce, reclaim the rubidium precipitating and take away.Bittern after demagging is through the technique of extraction reciprocal cross for counter-current extraction, and effectively improve the separation efficiency of rubidium, potassium, realize the separation and concentration of rubidium, the comprehensive recovery of rubidium reaches more than 95%.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the embodiment of the present invention 1.
Embodiment
Below, will describe in detail various embodiments of the present invention by reference to the accompanying drawings.
The invention provides a kind of method extracting rubidium from salt lake brine, preferentially eliminate the interference of magnesium ion, the raising for the extraction efficiency of follow-up neodymium element provides effective guarantee.
The inventive method comprises the steps:
Step one: the sedimentation of magnesium ion.
(1) dilution of salt lake brine
Measure the salt lake brine Mg content after sampling.If magnesium ion content is higher than 25g/L, then add distilled water diluting to below 25g/L.
(2) water soluble carbonate precipitation is adopted to remove magnesium ion.
First, carbonate aqueous solution is prepared.According to the magnesium ion content measured in described salt lake brine, calculate the amount n (unit is mol/L) of the carbonate material that magnesium ion is precipitated completely.Take carbonate n ~ 1.5n according to the calculation result of magnesium ion content, be made into by water dissolution the carbonate aqueous solution that massfraction is 20 ~ 25%.
First time is precipitated: slowly joined by described carbonate aqueous solution in the above-mentioned salt lake brine sample diluted, and stirs 10min, filters, and collects filtrate A and filter cake A respectively.
Second time precipitation: get described carbonate aqueous solution again and be added in described filtrate A, stirs more than 10min, filters and obtains the first filtrate, filter cake B; Wherein, the amount of substance of described water soluble carbonate is 0.25 ~ 0.5:1 with the ratio of the amount of substance of described magnesium ion.
In the first filtrate obtained after twice precipitation, the content of magnesium is down to below 50mg/L, directly can carry out extraction test.Described filter cake A, filter cake B merge into described first filter cake.
Step 2: the extraction of metal rubidium ion.
At [OH
-] substance withdrawl syndrome is under the environment of 0.8 ~ 1mol/L, with the 4-tertiary butyl-2-(α-methylbenzyl) phenol (being called for short t-BAMBP) for extraction agent, utilize extraction reciprocal cross for counter-current extraction technique, from described first filtrate, extract rubidium;
Wherein, using sulfonated kerosene as thinner in described extraction agent, the concentration of control t-BAMBP is 0.5 ~ 1mol/L.Described extraction reciprocal cross can reference for counter-current extraction technique: " Li Zhou. the new arrangement-extraction reciprocal cross of extraction tandem replaces multi-stage counter current extraction process, Journal of Chemical Industry and Engineering .1985 (2): 189-195 " introduction, be the extraction process that those skilled in the art commonly use.In the extraction of rubidium of the present invention, the reciprocal cross of concrete extraction for counter-current extraction processing condition is: comparing (that is, extraction agent and the ratio of described first filtrate, be also called oil: water) is 0.5 ~ 2:1; Temperature 5 ~ 30 DEG C; Rotating speed 3000 ~ 4000r/min; The extraction liquid obtained enters stripping process.Stripping process condition is: comparing (that is, reverse-extraction agent and the ratio of described extraction liquid, be also called oil: water) is 0.5 ~ 2:1; Temperature 15 ~ 30 DEG C; Rotating speed 3000 ~ 4000r/min; Mineral acid substance withdrawl syndrome is 0.02 ~ 0.5mol/L.
The present invention also comprises step 3: for reclaiming rubidium from described first filter cake, will effectively improve the extraction efficiency of rubidium.Step 3 comprises following operation:
(1) first, by described first filter cake dry after in retort furnace 500 ~ 900 DEG C of temperature lower calcination 30 ~ 60min, obtain calcinate;
(2) treat that described calcinate is cooled to room temperature, weighing described calcinate quality is that (unit is g) to M.
First time cleaning: clean described calcinate with the distilled water of 0.5M ~ 2M, obtains liquor C and filter cake C after filtering.
Second time cleaning, the distilled water of continuation 0.5M ~ 2M cleans described filter cake C, obtains filtrate D and filter cake D after filtering.
Described liquor C and filtrate D merge into the second filtrate, and described like this second filtrate can enter the extraction carrying out rubidium in described step 2.
Specific embodiment will be introduced below.
Embodiment 1
Anhydrous sodium carbonate 98g, dissolves with 350mL distilled water, slowly joins (content of magnesium is 21.98g/L) in 1L salt lake brine sample, stirs 10min, filters, and collects filtrate A and filter cake A respectively.
Take anhydrous sodium carbonate 25g 88mL distilled water to dissolve, slowly join in filtrate 1, stir 10min, filter, collect the first filtrate and filter cake B respectively.The content collecting magnesium in the first filtrate obtained is 43mg/L.
The filter cake A precipitate first time and second time and filter cake B merges into the first filter cake, in retort furnace 800 DEG C heating 40min, gross weight 180.7g after oven dry.Add the washing of 180mL distilled water after taking out cooling once, filter, collect liquor C and filter cake C respectively.
Filter cake C is added 180mL distilled water again and carries out secondary washing, filter, collect filtrate D and filter cake D respectively.The liquor C obtain twice washing and filtrate D merge into the second filtrate.
Described first filtrate and the second filtrate all enter the technical process of extraction reciprocal cross for counter-current extraction.
Weighing sodium hydroxide solid is added in the first filtrate and the mixed system of the second filtrate, and stirring and dissolving, makes OH
-concentration 0.8mol/L.Carry out after filtration extracting the technical process extraction rubidium of reciprocal cross for counter-current extraction.Extraction conditions is: compare (oil: water)=1:1, temperature: 5 DEG C, rotating speed: 3000r/min.Back extraction condition is: compare (oil: water)=1:1, temperature: 15 DEG C, concentration of hydrochloric acid: 0.05mol/L, rotating speed: 3000r/min.
The partition ratio of the rubidium finally obtained is 49:1, and the partition ratio of potassium is 1:81, and the partition ratio of sodium is 1:506.If only rely in the present embodiment the rubidium extraction in the first filtrate, the rate of recovery of rubidium is about 85%; Add the recovery to rubidium in filter cake, so the comprehensive recovery of rubidium reaches 95.4%.The processing parameter of the present embodiment arranges as shown in table 1:
The processing parameter of table 1 embodiment 1 and result thereof
Embodiment 2
The operation steps of the present embodiment is similar to embodiment 1, and processing parameter is as shown in table 2:
The processing parameter of table 2 embodiment 2 and result thereof
Embodiment 3
The operation steps of the present embodiment is similar to embodiment 1, and processing parameter is as shown in table 3:
The processing parameter of table 3 embodiment 3 and result thereof
Embodiment 4
The operation steps of the present embodiment is similar to embodiment 4, and processing parameter is as shown in table 4:
The processing parameter of table 4 embodiment 4 and result thereof
From embodiment 1 ~ 4 all, present invention reduces the separation of rubidium, extraction process flow, improve rubidium, potassium separation efficiency.The rubidium partition ratio > 45:1 of embodiment 1 ~ 4, the partition ratio of potassium is less than 1:80, and the partition ratio of sodium is less than 1:500.The comprehensive recovery of rubidium reaches more than 95%, and illustrate that the inventive method obtains good effect, the primary products obtained meet the needs carrying out later separation extraction with additive method.
Claims (6)
1. from salt lake brine, extract a method for rubidium, it is characterized in that, comprise the steps:
Step one: add water soluble carbonate precipitation magnesium ion in salt lake brine, obtain the first filtrate and the second filter cake after solid-liquid separation, to make in described first filtrate magnesium ion content at below 50mg/L;
Step 2: at [OH
-] substance withdrawl syndrome is under the environment of 0.8 ~ 1mol/L, with the 4-tertiary butyl-2-(α-methylbenzyl) phenol for extraction agent, utilize extraction reciprocal cross for counter-current extraction technique, from described first filtrate, extract rubidium;
Wherein, in described extraction agent, the concentration of the 4-tertiary butyl-2-(α-methylbenzyl) phenol is 0.5 ~ 1mol/L; Described extraction reciprocal cross for counter-current extraction processing condition is: be in a ratio of 0.5 ~ 2:1; Temperature 5 ~ 30 DEG C; Rotating speed 3000 ~ 4000r/min; Back extraction condition is: be in a ratio of 0.5 ~ 2:1; Temperature 15 ~ 30 DEG C; Rotating speed 3000 ~ 4000r/min; Mineral acid substance withdrawl syndrome is 0.02 ~ 0.5mol/L.
2. from salt lake brine, extract the method for rubidium according to claim 1, it is characterized in that, described step one comprises following operation:
First, described water soluble carbonate is made into 20 ~ 25% carbonate aqueous solutions, adds in described salt lake brine and stir more than 10min, after solid-liquid separation, obtain filtrate A, filter cake A; Wherein, the amount of substance of described water soluble carbonate is 1 ~ 1.5:1 with the ratio of the amount of substance of described magnesium ion;
Then, get described carbonate aqueous solution and be added in described filtrate A, stir more than 10min, after solid-liquid separation, obtain described first filtrate, filter cake B; Wherein, the amount of substance of described water soluble carbonate is 0.25 ~ 0.5:1 with the ratio of the amount of substance of described magnesium ion; Described filter cake A, filter cake B merge into described first filter cake.
3. according to claim 1 or 2, from salt lake brine, extract the method for rubidium, it is characterized in that, also comprise step 3: from described first filter cake, reclaim rubidium, comprise following operation:
First, at 500 ~ 900 DEG C of temperature lower calcination 30 ~ 60min after being dried by described first filter cake, calcinate is obtained;
Then, with water cleaning after described calcinate cooling, the second filtrate and the second filter cake is obtained by solid-liquid separation;
Wherein, described second filtrate repeating said steps two carries out the extraction of rubidium.
4. from salt lake brine, extract the method for rubidium according to claim 3, it is characterized in that, in described step 3, for cleaning 0.5 ~ 2 times that the quality of the water of described calcinate is described calcinate quality.
5. from salt lake brine, extract the method for rubidium according to claim 1, it is characterized in that, be also included in before carrying out described step one and described salt lake brine is diluted, make Mg content lower than 25g/L.
6. from salt lake brine, extract the method for rubidium according to claim 1, it is characterized in that, described carbonate selects sodium carbonate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105256150A (en) * | 2015-10-26 | 2016-01-20 | 中国科学院青海盐湖研究所 | Method for extracting rubdium and cesium from acid brine |
| 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 |
| CN113307299A (en) * | 2021-06-22 | 2021-08-27 | 中国科学院青海盐湖研究所 | Method for extracting rubidium from high-potassium magnesium chloride brine |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105256150A (en) * | 2015-10-26 | 2016-01-20 | 中国科学院青海盐湖研究所 | Method for extracting rubdium and cesium from acid brine |
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| 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 |
| CN112239221B (en) * | 2020-10-19 | 2023-02-28 | 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 |
| CN113307299A (en) * | 2021-06-22 | 2021-08-27 | 中国科学院青海盐湖研究所 | Method for extracting rubidium from high-potassium magnesium chloride brine |
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