CN112759512A - Method for producing high-purity cesium formate - Google Patents
Method for producing high-purity cesium formate Download PDFInfo
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- ATZQZZAXOPPAAQ-UHFFFAOYSA-M caesium formate Chemical compound [Cs+].[O-]C=O ATZQZZAXOPPAAQ-UHFFFAOYSA-M 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 51
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000000605 extraction Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001744 pollucite Inorganic materials 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000002386 leaching Methods 0.000 claims abstract description 8
- 239000002893 slag Substances 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000003113 alkalizing effect Effects 0.000 claims abstract description 6
- 235000019253 formic acid Nutrition 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000012074 organic phase Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000008346 aqueous phase Substances 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 5
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 3
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 34
- 239000012530 fluid Substances 0.000 description 9
- 238000005553 drilling Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- VHUJINUACVEASK-UHFFFAOYSA-J aluminum;cesium;disulfate;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[Cs+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VHUJINUACVEASK-UHFFFAOYSA-J 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 229910052601 baryte Inorganic materials 0.000 description 2
- 239000010428 baryte Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- -1 aluminum ions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali 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
- 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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- 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
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- Environmental & Geological Engineering (AREA)
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- Manufacturing & Machinery (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention discloses a method for producing high-purity cesium formate. The method for producing high-purity cesium formate comprises the following steps: (1) grinding pollucite, and acidifying to leach cesium; (2) adding water into the cesium-containing leaching solution or the slag washing water obtained in the step (1) to mix and dilute the concentration; (3) adding alkali into the cesium-containing solution with the concentration in the step (2) to adjust the pH value to 11-14, alkalizing, removing impurities and filtering; (4) and (4) extracting cesium from the cesium-containing alkalization impurity-removal liquid filtered in the step (3) by using a cesium special extracting agent, and performing back extraction on the cesium-containing alkalization impurity-removal liquid by using a formic acid solution with concentration to obtain a cesium formate back-extraction liquid. The method for producing the high-purity cesium formate does not introduce harmful metal elements in the production process, is environment-friendly, safe and environment-friendly, and is simple in process, free of complex impurity removal process, good in extraction and separation effect, high in cesium yield, high in purity of the produced product, high in capacity and suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of energy exploitation, and particularly relates to a method for producing high-purity cesium formate.
Background
With the development of oil and gas exploration and development, high-temperature and high-pressure wells are increased day by day, when conventional drilling fluid and completion fluid containing barite and other weighting materials are used for operation in the high-temperature and high-pressure wells, high pressure drop is easy to generate, so that the equivalent circulating density is overhigh, the solid-phase bearing capacity of the drilling fluid and the completion fluid can be reduced due to high downhole temperature, dynamic and static settlement of the barite is caused, oil and gas layers are damaged, and well control risks are increased, so that the high-temperature and high-pressure wells have serious safety and economic problems due to the influence of the conventional drilling fluid on the drilling.
Cesium is most electropositive among all stable metals. The 80% cesium formate solution is a liquid with the appearance of water, the density can reach 2.3g/cm3, and the cesium formate solution can be used as an oil drilling fluid and a completion fluid due to the advantages that the cesium formate solution can completely maintain various physical and chemical properties of cesium formate brine under the condition of high density, the solution viscosity is much lower than other solutions with the same density, the solid content is low, the transportation is safer, the toxicity is low, and the like. The cesium formate solution is used as the drilling fluid and the completion fluid, so that the environmental pollution is reduced, good temperature and pressure characteristics can be provided, the cesium formate solution has natural lubricity, and the cesium formate solution is beneficial to improving the drilling rate and reinforcing shale. Therefore, the large-scale production of 80% cesium formate solution is necessary.
In recent years, there have been few reports on the production preparation of 80% cesium formate solutions.
Chinese patent No. CN110256232A reports a method for producing cesium formate solid, which discloses a method for preparing cesium alum conversion solution by using cesium alum as a raw material, removing aluminum ions in the cesium alum conversion solution, performing double decomposition with formate to obtain cesium formate solution, and removing sulfate ions in the cesium formate solution by using hydroxide. Removing metal ions in the hydroxide by carbonation, and finally drying to obtain the cesium formate finished product with the purity of 99.9 percent. In the production process, waste water and waste gas which pollute the environment are generated by kerosene, and waste residues are mainly calcium sulfate, but the method has higher cost and more complicated impurity removal process.
Disclosure of Invention
In view of the above, it is necessary to provide a method for producing high-purity cesium formate in view of the above problems.
In order to achieve the purpose, the invention provides the following technical scheme:
a method of producing high purity cesium formate, said method comprising the steps of:
(1) grinding pollucite, and acidifying to leach cesium;
(2) adding water into the cesium-containing leaching solution or the slag washing water obtained in the step (1) to mix and dilute the concentration;
(3) adding alkali into the cesium-containing solution with the concentration in the step (2) to adjust the pH value to 11-14, alkalizing, removing impurities and filtering;
(4) extracting cesium from the cesium-containing alkalization impurity-removal liquid filtered in the step (3) by using a cesium special extracting agent, and performing back extraction on the cesium-containing alkalization impurity-removal liquid by using a formic acid solution with concentration to obtain a cesium formate back-extraction liquid;
(5) and (4) adsorbing and removing oil from the back extraction solution obtained in the step (4) by adopting activated carbon, adding a pH regulator to regulate the pH value to be neutral, concentrating and filtering to obtain an 80% cesium formate solution.
Further, the acid used in the step (1) is concentrated hydrochloric acid, and the concentration of the concentrated hydrochloric acid is 25-32%.
Further, the cesium concentration in the step (2) is diluted to 30-120 g/L.
Further, the alkali in the step (3) is at least one of sodium hydroxide, potassium hydroxide or calcium hydroxide.
Furthermore, the special extracting agent for cesium in the step (4) adopts t-BAMBP, and the adopted extracting equipment is a continuous mixing and clarifying extraction tank.
Further, OH in the pre-extraction liquid in the step (4)-The concentration is 0.1-1.5 mol/L.
Further, the ratio of the organic phase to the aqueous phase extracted in the step (4) is 0.1-8: 1.
Further, the cesium-loaded organic phase in the step (4) is washed and back-extracted, wherein the phase ratio of the washed organic phase to the aqueous phase is 0.1-8:1, the pH value of the back-extraction is 3-5, and the phase ratio of the back-extraction is 0.1-8: 1.
Further, the pH regulator added in the step (5) is at least one of cesium hydroxide or cesium carbonate, and the concentration end point is 100-120 ℃.
The method for producing the high-purity cesium formate comprises the steps of firstly, acid leaching of pollucite; secondly, alkalizing and removing impurities; thirdly, extracting cesium by a cesium extracting agent; fourthly, carrying out back extraction by using a formic acid solution with a certain concentration; fifthly, concentrating and filtering the back extraction solution. The method comprises the steps of leaching cesium in pollucite ore by using acid, and separating by using an extraction method to obtain a high-purity cesium formate solution. The method for producing the high-purity cesium formate does not introduce harmful metal elements in the production process, is environment-friendly, safe and environment-friendly, and is simple in process, free of complex impurity removal process, good in extraction and separation effect, high in cesium yield, high in purity of the produced product, high in capacity and suitable for large-scale production.
Drawings
Fig. 1 is a process flow diagram of a method for producing high-purity cesium formate according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, the present invention provides a method for producing high-purity cesium formate, comprising the steps of:
(1) grinding pollucite, and acidifying to leach cesium;
(2) adding water into the cesium-containing leaching solution or the slag washing water obtained in the step (1) to mix and dilute the concentration;
(3) adding alkali into the cesium-containing solution with the concentration in the step (2) to adjust the pH value to 11-14, alkalizing, removing impurities and filtering;
(4) extracting cesium from the cesium-containing alkalization impurity-removal liquid filtered in the step (3) by using a cesium special extracting agent, and performing back extraction on the cesium-containing alkalization impurity-removal liquid by using a formic acid solution with concentration to obtain a cesium formate back-extraction liquid;
(5) and (4) adsorbing and removing oil from the back extraction solution obtained in the step (4) by adopting activated carbon, adding a pH regulator to regulate the pH value to be neutral, concentrating and filtering to obtain an 80% cesium formate solution.
Further, the acid used in the step (1) is concentrated hydrochloric acid, and the concentration of the concentrated hydrochloric acid is 25-32%.
Further, the cesium concentration in the step (2) is diluted to 30-120 g/L.
Further, the alkali in the step (3) is at least one of sodium hydroxide, potassium hydroxide or calcium hydroxide.
Furthermore, the special extracting agent for cesium in the step (4) adopts t-BAMBP, and the adopted extracting equipment is a continuous mixing and clarifying extraction tank.
Further, OH in the pre-extraction liquid in the step (4)-The concentration is 0.1-1.5 mol/L.
Further, the ratio of the organic phase to the aqueous phase extracted in the step (4) is 0.1-8: 1.
Further, the cesium-loaded organic phase in the step (4) is washed and back-extracted, wherein the phase ratio of the washed organic phase to the aqueous phase is 0.1-8:1, the pH value of the back-extraction is 3-5, and the phase ratio of the back-extraction is 0.1-8: 1.
Further, the pH regulator added in the step (5) is at least one of cesium hydroxide or cesium carbonate, and the concentration end point is 100-120 ℃.
The method for producing the high-purity cesium formate comprises the steps of firstly, acid leaching of pollucite; secondly, alkalizing and removing impurities; thirdly, extracting cesium by a cesium extracting agent; fourthly, carrying out back extraction by using a formic acid solution with a certain concentration; fifthly, concentrating and filtering the back extraction solution. The method comprises the steps of leaching cesium in pollucite ore by using acid, and separating by using an extraction method to obtain a high-purity cesium formate solution. The method for producing the high-purity cesium formate does not introduce harmful metal elements in the production process, is environment-friendly, safe and environment-friendly, and is simple in process, free of complex impurity removal process, good in extraction and separation effect, high in cesium yield, high in purity of the produced product, high in capacity and suitable for large-scale production.
The first embodiment is as follows:
the method comprises the following steps: milling pollucite ore to 200 meshes by ball milling;
step two: mixing the pollucite ore powder ground in the first step with 32% concentrated hydrochloric acid, and heating in a closed enamel reaction kettle at a temperature of more than 95 ℃ to react for 3 hours;
step three: adding water or slag washing water into the slurry reacted in the step two, and diluting the solubility of cesium to 80 g/L;
step four: adding sodium hydroxide into the diluted leachate to adjust the pH value to 11, performing filter pressing on impurity elements precipitated in the leachate by using a filter press, and washing slag by using water;
step five: adding sodium hydroxide into the material subjected to filter pressing and clearing in the fourth step to adjust the OH-concentration to 0.6moL/L, and entering a continuous mixing and clarifying extraction tank to perform extraction by using a special extracting agent t-BAMBP, wherein the extraction ratio is 1: 1. Then passing through pure water in a proportion of 3: washing is carried out compared with 1. Because the extracting agent preferentially extracts the cesium, the cesium formate strip liquor is obtained after strip extraction is carried out according to the ratio of 1:1, and the pH value of strip extraction is 3.5;
step six: and (4) adsorbing and removing oil from the back extraction solution in the fifth step by using active carbon, adding a proper amount of cesium hydroxide to adjust the pH value to be neutral, concentrating and filtering, wherein the concentration end point is 110 ℃. Thus obtaining 80% cesium formate solution.
Example two:
the method comprises the following steps: milling pollucite ore to 300 meshes by ball milling;
step two: mixing the pollucite ore powder ground in the first step with 32% concentrated hydrochloric acid, and heating in a closed enamel reaction kettle at a temperature of more than 95 ℃ to react for 2 hours;
step three: adding water or slag washing water into the slurry reacted in the step two, and diluting the solubility of cesium to 120 g/L;
step four: adding sodium hydroxide into the diluted leachate to adjust the pH value to 10, performing filter pressing on the impurity elements precipitated in the leachate by using a filter press, and washing slag by using water;
step five: adding sodium hydroxide into the material subjected to filter pressing and clearing in the fourth step to adjust the OH-concentration to 1.0moL/L, and entering a continuous mixing and clarifying extraction tank to perform extraction by using a special extracting agent t-BAMBP, wherein the extraction ratio is 2: 1. Passing through pure water to obtain a mixture of 4: washing is carried out compared with 1. Because the extracting agent preferentially extracts the cesium, the cesium formate strip liquor is obtained after strip extraction is carried out according to the ratio of 1:1, and the pH value of strip extraction is 4.8;
step six: and (4) adsorbing and removing oil from the back extraction solution in the fifth step by using active carbon, adding a proper amount of cesium hydroxide to adjust the pH value to be neutral, concentrating and filtering, wherein the concentration end point is 110 ℃. Thus obtaining 80% cesium formate solution.
The above description is only for the purpose of illustrating specific embodiments of the present invention, and should not be construed as limiting the scope of the present invention, and all equivalent changes and modifications made in accordance with the spirit of the present invention should be considered as falling within the scope of the present invention.
Claims (9)
1. A method for producing high-purity cesium formate is characterized by comprising the following steps: the method comprises the following steps:
(1) grinding pollucite, and acidifying to leach cesium;
(2) adding water into the cesium-containing leaching solution or the slag washing water obtained in the step (1) to mix and dilute the concentration;
(3) adding alkali into the cesium-containing solution with the concentration in the step (2) to adjust the pH value to 11-14, alkalizing, removing impurities and filtering;
(4) extracting cesium from the cesium-containing alkalization impurity-removal liquid filtered in the step (3) by using a cesium special extracting agent, and performing back extraction on the cesium-containing alkalization impurity-removal liquid by using a formic acid solution with concentration to obtain a cesium formate back-extraction liquid;
(5) and (4) adsorbing and removing oil from the back extraction solution obtained in the step (4) by adopting activated carbon, adding a pH regulator to regulate the pH value to be neutral, concentrating and filtering to obtain an 80% cesium formate solution.
2. The method for producing high-purity cesium formate according to claim 1, characterized in that: the acid used in the step (1) is concentrated hydrochloric acid, and the concentration of the concentrated hydrochloric acid is 25-32%.
3. The method for producing high-purity cesium formate according to claim 1, characterized in that: and (3) diluting the cesium concentration in the step (2) to 30-120 g/L.
4. The method for producing high-purity cesium formate according to claim 1, characterized in that: the alkali in the step (3) is at least one of sodium hydroxide, potassium hydroxide or calcium hydroxide.
5. The method for producing high-purity cesium formate according to claim 1, characterized in that: the special extracting agent for cesium in the step (4) adopts t-BAMBP, and the adopted extracting equipment is a continuous mixing clarification extracting tank.
6. The method for producing high-purity cesium formate according to claim 1, characterized in that: OH in the pre-extraction liquid in the step (4)-The concentration is 0.1-1.5 mol/L.
7. The method for producing high-purity cesium formate according to claim 1, characterized in that: the ratio of the organic phase to the aqueous phase extracted in the step (4) is 0.1-8: 1.
8. The method for producing high-purity cesium formate according to claim 1, characterized in that: and (4) washing and back-extracting the cesium-loaded organic phase in the step (4), wherein the phase ratio of the washed organic phase to the aqueous phase is 0.1-8:1, the pH value of the back-extraction is 3-5, and the phase ratio of the back-extraction is 0.1-8: 1.
9. The method for producing high-purity cesium formate according to claim 1, characterized in that: the pH regulator added in the step (5) is at least one of cesium hydroxide or cesium carbonate, and the concentration end point is 100-120 ℃.
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