Preparation method of cesium carbonate_Industrial additives

Background and overview of the preparation method of cesium carbonate

Cesium carbonate is an inorganic compound. It is a white solid under normal temperature and pressure. It is easily soluble in water and absorbs moisture quickly when placed in the air. Cesium carbonate aqueous solution is strongly alkaline and can react with acid to produce the corresponding cesium salt and water, and release carbon dioxide. Cesium carbonate is easy to transform and can be used as a precursor for other cesium salts, and is widely used in cesium salt varieties. Cesium carbonate can be used as a modification layer between the active layer of solar cells and the Al electrode to improve device conversion efficiency, generate Al-O-Cs compounds, reduce the series resistance of the battery, improve the short-circuit current and photoelectric conversion efficiency of the solar cell, and Due to the compactness of the cesium carbonate layer itself, the stability of the device has also been significantly improved. Due to the strong metallic n-type heavy doping effect of cesium in cesium carbonate, the Al/CsCO cathode modified with cesium carbonate nano-interface can greatly improve the injection of electrons and significantly improve the performance of inverted top-emission structure OLED devices. Cesium carbonate is also used as a catalyst in the synthesis of alkyl aryl ethers.

Preparation method of cesium carbonate

Report on the preparation method of cesium carbonate 1.

The method for preparing cesium carbonate using cesium alum as raw material is carried out as follows: the first step is to recrystallize the cesium alum, add the cesium alum into deionized water and heat to dissolve it, after dissolution, cool and crystallize and filter. Obtain refined cesium alum; the second step, transformation, add refined cesium alum into deionized water and heat to dissolve it. After dissolution, a refined cesium alum solution is obtained. Slowly add lime milk into the refined cesium alum solution, and obtain sulfuric acid after solid-liquid separation. Cesium pure liquid; the third step, causticization, the barium hydroxide solution is added into the cesium sulfate pure liquid in 2 to 3 times, and centrifuged to obtain the barium sulfate solid and causticizing liquid; the fourth step, carbonization, concentration and evaporation, to causticization Pour CO into the liquid for carbonization, carbonize until the pH of the carbonized liquid is 7 to 10, let it stand, concentrate the carbonized supernatant after standing, and obtain the concentrated liquid after cooling; the fifth step is to perform one-time fine filtration and drying , the concentrated liquid is filtered with a polymer filtration device. The filtered filtrate is concentrated, crystallized and dried at low temperature to obtain low-temperature material; the sixth step of trifluoromethylpyridine is high-temperature decomposition. After the low-temperature material is decomposed at high temperature, the high-temperature material is obtained; the seventh step , secondary fine filtration, the high-temperature material is dissolved in deionized water, and then filtered with a polymer filtration device. After filtration, the filtered clean liquid is obtained; the eighth step is to concentrate and dry the clean liquid. After the filtered clean liquid is concentrated and dried, Cesium carbonate is obtained. The purity of cesium carbonate obtained by this method is 99.90% to 99.99%; the yield of cesium is 92% to 96%, and the production cost is reduced by 30% to 50% compared with the existing technology.

Report on the preparation method of cesium carbonate 2.

A method for extracting high-purity cesium carbonate from cosmide garnet

(1) Ore grinding: grind the ore to 120 mesh using a ball mill.

(2) Acidification reaction: Mix the cosmonite ore powder ground in step (1) with 10 equivalents of concentrated hydrochloric acid (concentration: 32%), and heat to 100°C in a closed enamel reaction kettle The reaction was carried out for 2 hours.

(3) Add water to the slurry after the reaction in step (2), mix it at a liquid-to-solid ratio of 4:1, and heat to 80 to 100°C to perform a leaching reaction for 1 hour.

(4) Add sodium hydroxide to the material reacted in step (3) to adjust the pH to 10 to precipitate impurities such as aluminum, silicon, calcium and magnesium.

(5) Filter the material after step (4) with a filter press, and then wash the residue with water. The ratio of washing liquid to solid is 1:1.

(6) After adjusting the composition of the leachate in step (5), it enters the continuous mixing and clarification extraction tank for extraction with the special extraction agent “Secondary BAMBP”. Since this extraction agent has excellent selectivity for cesium and rubidium, it can also separate The coefficient is very large, and cesium is extracted first, and the cesium carbonate strip solution is obtained after stripping with carbon dioxide.

(7) Concentrate the cesium carbonate stripping solution produced in step (6), and introduce carbon dioxide for deep carbonization. The carbonization pressure is 0.2Mpa and the carbonization time is 1 hour. Further concentrate to precipitate crystals, and centrifuge the crystals and mother liquor.

(8) Dissolve the crystallized product produced in step (7) with pure water at a liquid-to-solid trifluorobenzene boric acid ratio of 2:1, filter, then concentrate and crystallize again, and centrifuge to obtain secondary crystallization.

(9) Put the secondary crystal obtained in step (8) into an oven to dry and pulverize to obtain a cesium carbonate product with a purity of 99.99%. The total yield of cesium is 94.59%.

References

[1] [Chinese invention] CN201811186015.6 Method for preparing cesium carbonate using cesium alum as raw material

[2] [Chinese invention] CN201910514959.X A method for extracting high-purity cesium carbonate from cosmite garnet