SU180572A1 - Method of producing fine-dispersed powder of triplicate and double carbonates of alkaline-earth elements - Google Patents
Method of producing fine-dispersed powder of triplicate and double carbonates of alkaline-earth elementsInfo
- Publication number
- SU180572A1 SU180572A1 SU809296A SU809296A SU180572A1 SU 180572 A1 SU180572 A1 SU 180572A1 SU 809296 A SU809296 A SU 809296A SU 809296 A SU809296 A SU 809296A SU 180572 A1 SU180572 A1 SU 180572A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- triplicate
- alkaline
- earth elements
- producing fine
- double
- Prior art date
Links
- 150000004649 carbonic acid derivatives Chemical class 0.000 title description 6
- 239000000843 powder Substances 0.000 title description 3
- 239000000243 solution Substances 0.000 description 11
- 229910052791 calcium Inorganic materials 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N edta Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 6
- 229910052712 strontium Inorganic materials 0.000 description 6
- 229910052788 barium Inorganic materials 0.000 description 5
- 150000002823 nitrates Chemical class 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N Barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- DHEQXMRUPNDRPG-UHFFFAOYSA-N Strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 102000037197 Anion exchangers Human genes 0.000 description 1
- 108091006437 Anion exchangers Proteins 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate dianion Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- OPCMAZHMYZRPID-UHFFFAOYSA-J Potassium tetraiodomercurate(II) Chemical compound [K+].[K+].I[Hg-2](I)(I)I OPCMAZHMYZRPID-UHFFFAOYSA-J 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium(0) Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- -1 nitrate salts Chemical class 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Description
Двойной и тройной карбонаты бари , стронци и кальци примен ютс в SvieKTpOBaKyyMной технике дл производства оксидных катодов .Double and triple carbonates of barium, strontium and calcium are used in the SvieKTpOBaKyyM technique for the production of oxide cathodes.
Известно получение мелкодисперсных порошков Ва, Sr, Са тройных и двойных карбонатов карбонизацией раствора нитратов щелочноземельных элементов с добавлением водного раствора аммиака и с последующей отмывкой от ионов гор чей дистиллированной водой. Такие порощкн нельз использовать дл получени веществ высокой :тепени чистоты из-за загр знени соединений органическими и неорганическими примес ми. Между тем дл производства оксидных катодов сверхминиатюрных приборов тройной и двойной карбонаты Ва, Sr и Са должны отвечать высоким требовани м как по размеру зерна, так и по химической чистоте материала.It is known to obtain finely dispersed Ba, Sr, Ca powders of ternary and double carbonates by carbonizing a solution of nitrates of alkaline earth elements with the addition of an aqueous solution of ammonia and subsequent washing of ions with hot distilled water. Such powders cannot be used to obtain substances of high: warm purity due to contamination of the compounds with organic and inorganic impurities. Meanwhile, for the production of oxide cathodes of subminiature triple and double carbonates, Ba, Sr, and Ca must meet the high requirements of both grain size and chemical purity of the material.
Согласно лредложенному способу мож}1о получать тройной и двойной карбонаты Ва, Sr и Са размером зерна до 2 мк с содержанием примесей не более 2- % дл железа или меди, или цинка, или свиица, % дл сульфидов, % - нерастворимых в НС1 веществ (в виде сульфатов), 1 10 % дл хлоридов, 110 % дл натри или кали , 0,053/0 дл нитратов.According to the proposed method, we can obtain ternary and double carbonates Ba, Sr, and Ca with a grain size of up to 2 microns with an impurity content of not more than 2% for iron or copper, or zinc, or pigment,% for sulfides,% is HC1 insoluble (as sulphates), 1 10% for chlorides, 110% for sodium or potassium, 0.053 / 0 for nitrates.
Sr и Са при помощи св зывани примесей этилендиаминтетрауксусной кислотой в этилендиаминтетраацетатные комплексы (ЭДТА) и последующей сорбции последних на анионитовых смолах. Очищенный раствор подвергают карбонизации при температуре С при медленном приливании аммиака.Sr and Ca by binding impurities with ethylene diamine tetraacetic acid in ethylenediamine tetraacetate complexes (EDTA) and subsequent sorption of the latter on anion exchangers. The purified solution is subjected to carbonization at a temperature C with a slow addition of ammonia.
Пример. Смесь азотнокислых солей Ва, Sr и Са заданного состава раствор ют в дистиллированной воде и фильтруют от механических примесей. В качестве исходного сырь используют X. ч. азотнокислый барий и кальций и ч. д. а. азотнокислый стронций. К раствору азотнокислых солей приливают растворExample. A mixture of the nitrate salts of Ba, Sr, and Ca of a given composition is dissolved in distilled water and filtered from mechanical impurities. X. h. Barium nitrate and calcium and h.a. strontium nitrate. A solution is added to the solution of nitrate salts
этилендиаминтетрауксусной кислоты (0,15о/о ЭДТА от общего веса азотнокислых солей) н устанавливают рН 3-3,5 дл тройного и 3- 4 дл двойного карбоната. Затем раствор пропускают через ионообменную колонку, заполненную анионитом.ethylenediaminetetraacetic acid (0.15o / o EDTA based on the total weight of nitrate salts) and the pH is set to 3-3.5 for triple and 3-4 for double carbonate. Then the solution is passed through an ion exchange column filled with anion exchange resin.
Очищенный раствор азотнокислых солей фильтруют через капроновую ткань и охлаждают до 10°С. При данной температуре через раствор пропускают углекислый газ и одновременно приливают водный раствор аммиака. Скорость приливани аммиака должна быть такой, чтобы нитратные растворы во врем осаждени не нагревались. Осадок двойного или тройного карбонатов промывают гор чей 3 ронке Бюхнера до отсутстви ионов NH4 по качественной реакции с реактивом Несслера. „ Предмет и з о о р е т е и и Способ получени мелкодисперсных порош-5 ков тройных и двойных карбонатов щелочноземельных элементов путем карбонизации раствора нитратов щелочноземельных элемен4 тов с добавлением водного раствора аммиака и с последующей отмывкой от ионов гор чей дистиллированной водой, отличающийс тем. . получени продукта высокой степени чистоты, перед карбонизацией к раствору добавл ют этилендиаминтетрауксусную кислоту и полученный при этом раствор нропускают через ионит.The purified solution of nitrate salts is filtered through a nylon cloth and cooled to 10 ° C. At this temperature, carbon dioxide is passed through the solution and at the same time an aqueous solution of ammonia is added. The flow rate of ammonia should be such that the nitrate solutions during the precipitation are not heated. The precipitate of double or triple carbonates is washed with a hot 3 Buchner tank until there are no NH4 ions for a qualitative reaction with Nessler's reagent. The Subject and Solution of the Process . . to obtain a product of high purity, ethylenediaminetetraacetic acid is added to the solution before carbonization, and the resulting solution is passed through an ion exchanger.
Publications (1)
Publication Number | Publication Date |
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SU180572A1 true SU180572A1 (en) |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4053572A (en) * | 1976-05-17 | 1977-10-11 | The Harshaw Chemical Company | Process for preparing essentially pure barium fluoride crystals |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4053572A (en) * | 1976-05-17 | 1977-10-11 | The Harshaw Chemical Company | Process for preparing essentially pure barium fluoride crystals |
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