Process of preparing atomic energy level zirconium dioxide and hafnium oxide by methyl isobutanone double solvent extraction method

A technology of methyl isobutyl ketone and atomic energy level, applied in the direction of zirconia, etc., can solve the problems of not very stable system, low extraction efficiency, bad smell, etc., to improve system stability, increase extraction efficiency, and improve extraction performance effect

Inactive Publication Date: 2007-03-14
JIANGXI KINGAN HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the end of the 1970s, the situation changed a lot. The outstanding disadvantage of the first process is that the solubility of MIBK in water is 1.7%, the loss in water is large, and thiocyanic acid is easy to decompose. At the same time, MIBK and thiocyanic acid are volatile and smell Unpleasant smell, worsening working enviro

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 1: prepare 2.65N and 7.48 hydrochloric acid, 5.35N dilute sulfuric acid, 6.65N ammonia water, 235g / L zirconium oxychloride, and 5.85M ammonium thiocyanate solutions respectively, pour them into corresponding high-level tanks, and extract them in the washing section Pump 220L2.50N acid wash into the tank, and pump 140L5.55N acid back into the stripping section; the second step: mix 950 liters of 15% butyl acetate extractant with methyl isobutyl ketone, and then After three-stage extraction with 3.10N hydrochloric acid and 2.86M ammonium thiocyanate mixed solution, put it into the extraction tank. Step 3: measure the ammonium thiocyanate solution, zirconium oxychloride solution, and hydrochloric acid solution into the feed liquid configuration barrel and stir evenly to control the ZrO in the feed liquid 2 Concentration: 180 g / L, acidity of hydrochloric acid: 2.52N, CNS - Concentration: 1.95 mol / L, put into the high tank for standby. The fourth step is to turn on th...

Embodiment 2

[0023] Step 1: Prepare 2.35N and 8.10N hydrochloric acid, 5.46N dilute sulfuric acid, 6.64N ammonia water, 235g / L zirconium oxychloride, and 5.73M ammonium thiocyanate solutions respectively, put them into the corresponding high-level tanks, and put them in the washing section Pump 220L of 2.25N acid wash into the extraction tank, and pump 140L of 5.65N acid back into the stripping section; the second step: after mixing 960 liters of 15% amyl acetate extractant with methyl isobutyl ketone, Then carry out three-stage extraction with 2.90N hydrochloric acid and 3.15M ammonium thiocyanate mixed solution, and then put it into the extraction tank. Step 3: measure the ammonium thiocyanate solution, zirconium oxychloride solution, and hydrochloric acid solution into the feed liquid configuration barrel and stir evenly to control the ZrO in the feed liquid 2 Concentration: 180 g / L, acidity of hydrochloric acid: 2.76N, CNS - Concentration: 1.85 mol / L, put into high tank for standby. ...

Embodiment 3

[0025] Step 1: Prepare 2.45N and 7.80N hydrochloric acid, 5.12N dilute sulfuric acid, 6.15N ammonia water, 255g / L zirconium oxychloride, and 5.38M ammonium thiocyanate solutions respectively, pour them into corresponding high-level tanks, and extract in the washing section Pump 220L2.25N acid wash into the tank, and pump 140L5.25N acid back into the stripping section; the second step: mix 1000 liters of 12% dimethyl heptyl methyl phosphate extractant with methyl isobutyl ketone After homogenization, carry out three-stage extraction with a mixed solution of 2.68N hydrochloric acid and 3.22M ammonium thiocyanate, and then put it into the extraction tank. Step 3: measure the ammonium thiocyanate solution, zirconium oxychloride solution, and hydrochloric acid solution into the feed liquid configuration barrel and stir evenly to control the ZrO in the feed liquid 2 Concentration: 185 g / L, acidity of hydrochloric acid: 2.32N, CNS - Concentration: 1.45 mol / L, put into high tank for ...

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PUM

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Abstract

The methyl isobutyl ketone (MIBK) double solvent extraction process of prepare zirconia and hafnium oxide in atomic energy level includes the following steps: 1. preparing dilute hydrochloric acid solution, dilute sulfuric acid solution, ammonia solution, zirconium oxychloride solution and ammonium thiocyanate solution; setting in high-level tanks separately; washing and reverse extracting; 2. mixing MIBK and extractant and extracting; 3. mixing ammonium thiocyanate solution, zirconium oxychloride solution and dilute hydrochloric acid solution; and setting the mixture in high-level tank; 4. reaction through stirring for 8 hr and multistage extraction to obtain zirconium hydroxide solution and hafnium hydroxide solution; 5. depositing zirconium hydroxide and hafnium hydroxide in ammonia water; and 6. high temperature roasting zirconium hydroxide and hafnium hydroxide to obtain zirconia and hafnium oxide. The process has high separating effect and less environmental pollution.

Description

technical field [0001] The invention relates to a process for preparing atomic-level zirconia and hafnium oxide, in particular to a process for preparing atomic-level zirconia and hafnium oxide by methyl isobutyl ketone dual-solvent extraction. Background technique [0002] The chemical behaviors of zirconium and hafnium are very similar, and their aqueous solution chemistry is also very complex, and it is very difficult to separate each other. They are considered to be one of the most difficult elements in the periodic table to separate. The content of zirconium in the earth's crust is 162ppm, and that in seawater is 2.6×10 -5 ppm, more than copper, zinc and lead, but the distribution is very scattered. The main mineral is baddeleyite (ZrO 2 ) and zircon (ZrSiO 4 ). The content of hafnium in the earth's crust is 2.8ppm, and <0.008ppm in seawater. There is no independent mineral. It often coexists with zirconium in nature and exists in zirconium ore. Zircon and baddel...

Claims

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Application Information

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IPC IPC(8): C01G25/02C01G27/02
Inventor 罗方承陈忠锡孙小龙谌美玲吴江罗新文邱才华李泉华万桂平邬红娣杨丽樊小妹
Owner JIANGXI KINGAN HI TECH
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