Zirconium → Zirconyl nitrate

HRID 634569

反応式

HRID 634569 の反応式
[NH4+:1].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[OH2:7].[OH-:8].[OH-:9].[OH-].[OH:11][W:12]([O:15][W:16]([O:19][W:20]([O-:23])(=[O:22])=[O:21])(=[O:18])=[O:17])(=[O:14])=[O:13].[OH:24][W:25]([O:28][W:29]([O:32][W:33]([O:36][W:37]([O-:40])(=[O:39])=[O:38])(=[O:35])=[O:34])(=[O:31])=[O:30])(=[O:27])=[O:26].[OH:41][W:42]([O:45][W:46]([O:49][W:50]([O:53][W:54]([O-:57])(=[O:56])=[O:55])(=[O:52])=[O:51])(=[O:48])=[O:47])(=[O:44])=[O:43].[W:58].[Zr:59]>>[N+:1]([O-:9])([OH:8])=[O:7].[N+:1]([O-:9])([OH:8])=[O:7].[O:7]=[Zr:59].[NH4+:1].[NH4+:1].[NH4+:1].[NH4+:1].[NH4+:1].[NH4+:1].[OH2:11].[OH-:24].[OH-:41].[OH-:11].[OH:23][W:20]([O:19][W:16]([O:15][W:12]([O-:14])(=[O:11])=[O:13])(=[O:18])=[O:17])(=[O:21])=[O:22].[OH:27][W:25]([O:28][W:29]([O:32][W:33]([O:36][W:37]([O-:40])(=[O:38])=[O:39])(=[O:35])=[O:34])(=[O:30])=[O:31])(=[O:24])=[O:26].[OH:44][W:42]([O:45][W:46]([O:49][W:50]([O:53][W:54]([O-:57])(=[O:55])=[O:56])(=[O:52])=[O:51])(=[O:47])=[O:48])(=[O:41])=[O:43].[W:58]

参加物

4

反応物 2

HCID 23995ZirconiumHCID 25113228Ammonium tungsten oxide

生成物 2

HCID 83761Zirconyl nitrateHCID 25113228Ammonium tungsten oxide

反応条件

温度
60 °C

実験手順

This example describes a low temperature method for the bulk synthesis of fine particle, crystalline ZrW2O8. 0.5M solutions of zirconium oxynitrate and ammonium metatungstate were prepared. 200ml of ammonium metatungstate solution were heated to 60° C. in a 2.0 L beaker. 100 ml of the zirconium salt solution were added to the breaker with a burette, and the mixture was stirred using mechanical stirring. The addition took approximately 1.5 hours. The addition was drop wise with very good stirring and simultaneous heating (60° C.). After the addition was complete, stirring was continued magnetically until the solution was concentrated (for one more hour). Then 250 ml of 6M HCl were added and the heating and stirring were continued until the solution was concentrated once again into a slurry (for about three hours). The slurry was transferred to a Parr bomb and was heated at 180° C. over night (for about fifteen hours) for a fast setting of gel under hydrothermal pressures. The hydrate gel was then filtered, washed with deionized water and dried in the oven (ZWO-HT-1) for three hours. This gel was then fired at 650° C. for 2.5 hours. The product obtained (ZWO-HT-2) was analyzed by XRD. The gel also was sintered at 1473K (ZWO-HT-3) for thirty minutes and was analyzed for its phase purity and bulk density. The X-ray diffractograms of the samples prior to and subsequent to sintering are presented in FIGS. 12-13.

後処理

  1. additionThe addition
  2. additionThe addition
  3. stirringwith very good stirring
  4. additionAfter the addition
  5. stirringstirring
  6. concentrationwas concentrated (for one more hour)
  7. additionThen 250 ml of 6M HCl were added
  8. stirringthe heating and stirring
  9. concentrationwas concentrated once again into a slurry (for about three hours)
  10. temperaturewas heated at 180° C. over night (for about fifteen hours) for a fast setting of gel under hydrothermal pressures
  11. filtrationThe hydrate gel was then filtered
  12. washwashed with deionized water
  13. customdried in the oven (ZWO-HT-1) for three hours
  14. waitThis gel was then fired at 650° C. for 2.5 hours
  15. customThe product obtained (ZWO-HT-2)

出典と根拠

ORDレコード
ord-b58ae6d8fe7246388853a7db8d942a6d
出典データセット
uspto-grants-2001_02
特許番号
US06183716B2

関連ノート

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