CS201956B1 - Method of preparing pure lithium carbonate for single crystals - Google Patents
Method of preparing pure lithium carbonate for single crystals Download PDFInfo
- Publication number
- CS201956B1 CS201956B1 CS191279A CS191279A CS201956B1 CS 201956 B1 CS201956 B1 CS 201956B1 CS 191279 A CS191279 A CS 191279A CS 191279 A CS191279 A CS 191279A CS 201956 B1 CS201956 B1 CS 201956B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- lithium carbonate
- single crystals
- lithium
- preparing pure
- pure lithium
- Prior art date
Links
- 239000013078 crystal Substances 0.000 title claims description 12
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 title claims description 11
- 229910052808 lithium carbonate Inorganic materials 0.000 title claims description 11
- 238000000034 method Methods 0.000 title description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- 229910003002 lithium salt Inorganic materials 0.000 claims description 2
- 159000000002 lithium salts Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- WMFOQBRAJBCJND-UHFFFAOYSA-M lithium hydroxide Inorganic materials [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Vynález se týká způsobu přípravy čistého uhličitanu lithného pro monokrystaly. Pro pěstování monokrystalů, obsahujících lithium, jako jsou například monokrystaly lithiumniobátu, je nezbytný vysoký stupeň čistoty výchozích lithnýoh surovin, obvykle uhličitanu lithnéhoThe invention relates to a process for preparing pure lithium carbonate for single crystals. For the cultivation of lithium-containing single crystals, such as lithium niobate single crystals, a high degree of purity of the starting lithium raw materials, usually lithium carbonate, is necessary
Běžné lithné sloučeniny věak nedosahují této vysoké potřebná čistoty a známá způsoby jejioh čištění, například přesrážení uhličitanem amonným neposkytuje surovinu dostatečná jakosti.However, conventional lithium compounds do not achieve this high purity and the known methods of purification thereof, for example by precipitation with ammonium carbonate, do not provide the raw material of sufficient quality.
Tyto nedoetatky nemá způsob přípravy čistého uhličitanu lithného pro monokrystaly podle vynálezu, jehož podstata spočívá v tom, že lithná sůl, převedená na dusičnan, se rozpustí v nižším alkoholu nebo ketonu, zatepla se filtruje, filtrát se zahustí ke krystalizaci a vzniklé krystaly, rozpuštěné v redestilované vedš, se sráží uhličitanem amonným.There is no method for the preparation of pure lithium carbonate for the single crystals of the present invention, which consists in dissolving the lithium salt converted to nitrate in a lower alcohol or ketone, filtering it warm, concentrating the filtrate to crystallize and the crystals formed redistilled, and is precipitated with ammonium carbonate.
Výhodou způsobů podle vynálezu je, že se získá produkt vysoké čistoty.An advantage of the methods of the invention is that a high purity product is obtained.
Vynález je založen na poznatku rozpustnosti dusičnanu lithného ve zmínšnýoh nižšíoh alkoholech nebo ketonech, které současně snižují a potlačují rozpustnost řady iontových sloučenin, přítomných jako nečistoty v použité soli. Jako výhodný se ukazuje přídavek kyseliny šňavelové·The invention is based on the recognition of the solubility of lithium nitrate in the lower alcohols or ketones mentioned, which simultaneously reduce and suppress the solubility of a number of ionic compounds present as impurities in the salt used. The addition of oxalic acid proves advantageous.
V dalším jsou uvedeny příklady, vynález dále osvětlující.The following examples are provided to further illustrate the invention.
201 9 56201 9 55
Příklad 1Example 1
Roztok dusičnanu lithného, připravený rozpuštěním výchozího uhličitanu nebo hydmoxidu lithného čistoty p.a. v kyselině dusičně byl neutralizován amoniakem do slabě zásaditě reakce a potě upraven přídavkem 2 % hmot., vztaženo na výohozí surovinu, kyselého fosforečnanu amonného. Vzniklé krystgly dusičnanu lithného byly poté rozpuštěny v ethylalkoholu s pří davkem 1 % hmot* dihyárofobíorečmanu amonného za teploty varu rozpouštědla. Zakalený roztok byl filtrován hustým filtrem a filtrát zahuštěn ks krystalizaci. Krystaly byly odsáty, promyty ethylalkoholem a rozpuštěny v redeetilované vodě na 15 až 20 %ní roztok* Uhličitanem amonným bylo provedeno srážení, přičemž první podíly vysráženého uhličitanu lithněho byly odfiltrovány a vráceny zpět do prvního stupně čištění. Vzniklý uhličitan lithný byl odsát, promyt redestilovanou vodou a po vysušení přsžíhán na 500 °C. Takto připravený uhličitan lithný vykazoval vysokou čistotu a monokrystaly lithiumniobátu z něj vypěstovaně byly bezvadné.Lithium nitrate solution, prepared by dissolving the starting lithium carbonate or hydroxide, p.a. in nitric acid was neutralized with ammonia to a slightly alkaline reaction and treated with the addition of 2% by weight, based on the feedstock, of ammonium acid phosphate. The resulting lithium nitrate crystals were then dissolved in ethyl alcohol with the addition of 1% by weight ammonium dihydrofoborate at the boiling point of the solvent. The cloudy solution was filtered through a thick filter and the filtrate was concentrated to crystallize. The crystals were sucked off, washed with ethanol and dissolved in redeetilized water to a 15-20% solution. Ammonium carbonate was precipitated, the first portions of precipitated lithium carbonate being filtered off and returned to the first purification step. The resulting lithium carbonate was aspirated, washed with redistilled water, and dried to 500 ° C after drying. The lithium carbonate thus prepared was of high purity and the single crystals of lithium niobate grown from it were impeccable.
Příklad 2Example 2
Výohozí uhličitan lithný byl rozpuštěn vo zředěné kyselině dusičně a pH roztoku bylo upraveno amoniakem do slabě zásadité reakce. Po přídavku 1 % hmot. ohelatonu I byl roztok filtrován a odpařen ke krystalizaci. Vzniklé krystaly dusičnanu lithněho byly podle vynálezu rozpuštěny v acetonu čistoty p.a* zároveň s přídavkem 1 % hmot. (vztaženo na výohezí surovinu) kyseliny šťavelové p.a. Kalný roztok byl zatepla zfiltrován hustým filtrem, filtrát odpařen ke rystalizaei a dále bylo postupováno jako v příkladu 1 * Docílené výsledky, tj. jakost připraveného uhličitanu lithněho a z něho vypěstovaná monokrystaly vykázaly obdobné hodnoty jako v příkladu 1.The lithium carbonate was dissolved in dilute nitric acid and the pH of the solution was adjusted with ammonia to a slightly basic reaction. After addition of 1 wt. ohelatone I, the solution was filtered and evaporated to crystallize. The resulting lithium nitrate crystals according to the invention were dissolved in acetone of p.a * purity together with the addition of 1 wt. (based on raw material yield) oxalic acid p.a. The turbid solution was hot filtered through a dense filter, the filtrate was evaporated to rystallization, and then proceeded as in Example 1. The results obtained, i.e. the quality of the prepared lithium carbonate and the monocrystals grown therefrom, were similar to those of Example 1.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS191279A CS201956B1 (en) | 1979-03-23 | 1979-03-23 | Method of preparing pure lithium carbonate for single crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS191279A CS201956B1 (en) | 1979-03-23 | 1979-03-23 | Method of preparing pure lithium carbonate for single crystals |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS201956B1 true CS201956B1 (en) | 1980-12-31 |
Family
ID=5354671
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS191279A CS201956B1 (en) | 1979-03-23 | 1979-03-23 | Method of preparing pure lithium carbonate for single crystals |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS201956B1 (en) |
-
1979
- 1979-03-23 CS CS191279A patent/CS201956B1/en unknown
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0161704B1 (en) | Process for the production of water soluble ammonium phosphates | |
| DK173272B1 (en) | Process for recovering 2-keto-L-gulonic acid from a fermentation medium | |
| SU668608A3 (en) | Method of obtaining gamma-crystalline form of sodium salt of 7-(d-2-formiloxy-2-phenyl-acetamido)-3-(1-methyl-1n-tetrazolil-5-thomethyl)-cephem-4-carboxylic acid | |
| JPS62502683A (en) | chemical purification method | |
| US5618936A (en) | Process for preparing (S) (+)-4,4'-(1-methyl-1,2-ethanediyl)-bis (2,6-piperazinedione) | |
| CS201956B1 (en) | Method of preparing pure lithium carbonate for single crystals | |
| US4203903A (en) | Process for the recovery of spectinomycin | |
| US2797215A (en) | Production of type a riboflavin crystals | |
| GB909933A (en) | Process for the recovery of concentrated sulphuric acid from salt-containing dilute waste acids | |
| RU2044730C1 (en) | PROCESS FOR PREPARING N-(β-HYDROXYETHYL)-4,6-DIMETHYLDIHYDROPYRIMIDON-2 | |
| US2435125A (en) | Purification of tryptophane | |
| US2567955A (en) | Preparation of guanidine thiocyanate | |
| US2309739A (en) | Z-aminopykimtoines | |
| US3932386A (en) | Sodium 6-(L-aminocyclohexane carboxamido)penicillanic acid | |
| JPS6352620B2 (en) | ||
| US3226187A (en) | Method of obtaining insoluble basic aluminum ammonium alum | |
| RU2162439C1 (en) | Method of preparing disodium phosphate | |
| US2857375A (en) | Streptomycin and dihydrostreptomycin salts and method of recovering and purifying streptomycin and dihydrostrep tomycin by means thereof | |
| RU1792914C (en) | Method of calcium phosphate production | |
| SU465789A3 (en) | The way to get eburnamonine | |
| RU2776120C1 (en) | Method for producing potassium monoposphate | |
| JPS60151204A (en) | Manufacture of purified ammonium secondary phosphate in high yield | |
| US2764612A (en) | Process for preparing salts of glutamic acid | |
| SU485976A1 (en) | The method of obtaining octammine-m-amino-ol-dicobaltihloride | |
| US2744892A (en) | Crystallization of dihydrostreptomycin sulphate |