SU1175871A1 - Method of producing zirconium dioxide - Google Patents
Method of producing zirconium dioxide Download PDFInfo
- Publication number
- SU1175871A1 SU1175871A1 SU833658533A SU3658533A SU1175871A1 SU 1175871 A1 SU1175871 A1 SU 1175871A1 SU 833658533 A SU833658533 A SU 833658533A SU 3658533 A SU3658533 A SU 3658533A SU 1175871 A1 SU1175871 A1 SU 1175871A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- zirconium dioxide
- content
- zirconium
- ammonium hydroxide
- producing zirconium
- Prior art date
Links
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 9
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title description 3
- 239000000460 chlorine Substances 0.000 claims abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 6
- -1 chlorine ions Chemical class 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000004202 carbamide Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims 2
- 229910001928 zirconium oxide Inorganic materials 0.000 abstract description 2
- 235000013877 carbamide Nutrition 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000004062 sedimentation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001804 chlorine Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
СПОСОБ ПОЛУЧЕНИЯ ДИОКСИДА ЦИРКОНИЯ осаждением из раствора хлорокиси циркони гидроксидом аммони , фильтрахщей, промывкой и термообработкой , отличающийс тем, что. С; целью обеспечени получени продукта с содержанием .ионов хлора не более 1«10 мас.%,. осаждение ведут в присутствии карбамида , вз того в мольном соотношении к хлорокиси циркони A method for producing zirconium dioxide by precipitating ammonium hydroxide from a solution of zirconium oxychloride by ammonium hydroxide, fillers, washing and heat treatment, characterized in that. WITH; the purpose of ensuring the production of a product with the content of chlorine ions is not more than 1 "10 wt.% ,. sedimentation is carried out in the presence of carbamide, taken in a molar ratio to zirconium oxide
Description
ч елate
0000
ч Изобретение относитс к способу получени особо чистого диоксида цирко1ад , которьй находит применени в электронной промышленности, в оптическом стекловарении, где к диоксиду циркони предъ вл ют высокие требовани по содержанию как микропримесей катионов железа, марганца, кобальта и т. д., так и к содержанию ионов хлора, количество Которых не должно превышать 1-5 .%. Целью изобретени вл етсч обеспечение ролучени продукта с содержанием ионов хлора не более . %. Пример.В аппарат, снабженный рубашкой и перемешивающим устройством , загружают реакционную массу, состо щую из 1 г-моль (178 г) 75%-ного водного раствора хлорокиси циркони , 2,1 моль (73,5 г 25%-iioro раствора аммиака и 0,25 гмоль (1,6 г) 25%-ного водного раствора карбамида, что соответствует ,их .мольному соотношению 1:2,1:0,025 Взаимодействие загружаемых реаге тов Сопровождаетс небольшим вьщелением тепла. Температура реакции ;поддерзкиваетс на уровне . : Полученную суспензию гидроокиси циркони фильтруют, промывают обес:соленной водой, а отмытые кристаллы подвергают термической обработке при 550°С. В результате получают 0., 991 г-мол ( 121,9 г) целевого продукта, что со |ОТветствует выходу 99,1% с содержа нием основного вещества 99,6 мас.% и содержанием ионов хлора не более .%. Таким образом достигаетс необходимое качество по содержанию ионов хлора на уровне мас.% и сохранение на достигнутом уровне в способе (прототипе) катионов, мас.%: Fe - 5 -10-, Со - 5 1 -10 , Ni - 1 -10 , Сг - 1-10Получение диоксида циркони в примерах 1-3 осуществл ют по аналогичной методике. Экспериментальные данные, приведенные в примерах 1-3, представлены в таблице. Из таблицы видно, что уровень загр знени целевого продукта ионами хлора снижен с 1 -10 до 1-10 мас%1 Дозировка карбамида и аммиака в указанном соотношении обеспечиваетобразование кристаллов правильной формы, что приводит к интенсификации процесса фильтрации за счет сокращени времени фильтрации и отмывки в 5-6 раз за счет снижени температуры термообработки с 1200 до . Выход готового продукта увеличиВаетс на 19% вследствие более полного протекани реакции образовани диоксида циркони . Содержание основного вещества увеличиваетс с 99 до 99,6 мас.%. Изобретение позвол ет исключить выброс в атмосферу большого количества хлорпроизводных продуктов реакции .The invention relates to a process for the production of highly pure zirconium dioxide, which is used in the electronics industry, in optical glassmaking, where zirconia is made of high demands on the content of trace amounts of iron, manganese, cobalt cations, etc., and the content of chlorine ions, the amount of which should not exceed 1-5.%. The aim of the invention is the provision of rolling of the product with the content of chlorine ions not more. % Example. In an apparatus equipped with a jacket and a stirrer, a reaction mass is loaded consisting of 1 g-mol (178 g) of a 75% aqueous solution of zirconium oxide, 2.1 mol (73.5 g of a 25% -iorior ammonia solution and 0.25 gmol (1.6 g) of a 25% aqueous solution of urea, which corresponds to their molar ratio of 1: 2.1: 0.025 The interaction of the loaded reagents is accompanied by a small heat release. The temperature of the reaction is maintained at the level of: The resulting zirconium hydroxide suspension is filtered, washed with saline water, and the washed crystals subjected to heat treatment at 550 ° C. The result is 0., 991 gmol (121.9 g) of the target product, which means Co | Responds to a yield of 99.1% with a basic substance content of 99.6% by weight and an ion content chlorine, not more than.%. Thus, the required quality of chlorine ion content at the level of wt.% and preservation of the cations in the method (prototype), wt.%: Fe - 5-10-, Co - 5 1 -10, Ni-1 -10, Cr-1-10. The preparation of zirconia in Examples 1-3 is carried out in a similar manner. The experimental data given in examples 1-3, are presented in the table. The table shows that the level of contamination of the target product with chlorine ions is reduced from 1 -10 to 1-10 wt% 1 The dosage of urea and ammonia in the specified ratio ensures the formation of crystals of the correct form, which leads to an intensification of the filtration process by reducing the filtration time and washing 5-6 times by reducing the heat treatment temperature from 1200 to. The yield of the finished product is increased by 19% due to a more complete reaction of the formation of zirconium dioxide. The content of the basic substance increases from 99 to 99.6% by weight. The invention makes it possible to eliminate the release into the atmosphere of a large amount of chlorine derivatives of the reaction products.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU833658533A SU1175871A1 (en) | 1983-11-03 | 1983-11-03 | Method of producing zirconium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU833658533A SU1175871A1 (en) | 1983-11-03 | 1983-11-03 | Method of producing zirconium dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1175871A1 true SU1175871A1 (en) | 1985-08-30 |
Family
ID=21087654
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU833658533A SU1175871A1 (en) | 1983-11-03 | 1983-11-03 | Method of producing zirconium dioxide |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU1175871A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719091A (en) * | 1986-07-01 | 1988-01-12 | Corning Glass Works | Preparation of mono-sized zirconia powders by forced hydrolysis |
| US5470550A (en) * | 1993-12-30 | 1995-11-28 | Westinghouse Electric Corporation | Zirconium sulfate precipitation |
-
1983
- 1983-11-03 SU SU833658533A patent/SU1175871A1/en active
Non-Patent Citations (1)
| Title |
|---|
| Авторское свидетельство СССР № 535219, кл. С 01 G 25/02, 1972.. Строение и свойство адсорбентов и катализаторов. Мир, 1973, с. 361364. * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719091A (en) * | 1986-07-01 | 1988-01-12 | Corning Glass Works | Preparation of mono-sized zirconia powders by forced hydrolysis |
| US5470550A (en) * | 1993-12-30 | 1995-11-28 | Westinghouse Electric Corporation | Zirconium sulfate precipitation |
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