Method for preparing zirconium sulfate tetrahydrate with zirconium carbonate production wastewater

A technology of zirconium sulfate tetrahydrate and production wastewater, applied in zirconium sulfate and other directions, can solve the problems of poor consistency, serious equipment corrosion, long process, etc., and achieve the effect of reducing production cost, saving environmental resources and simple process

Active Publication Date: 2013-12-25
JIANGXI KINGAN HI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The first method has long process, low metal recovery rate, unstable product quality and high production cost
Due to the use of hydrochloric acid in the second method, the equipment is severely corroded and the operating environment is poor
Due to low-acid leaching and high-acid hydrolysis, the metal recovery rate is low, and the product contains high titanium content.
The third one uses zirconium oxychloride to produce zirconium sulfate, although the quality is very good, but the c

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  • Method for preparing zirconium sulfate tetrahydrate with zirconium carbonate production wastewater

Examples

Experimental program
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Effect test

Embodiment 1

[0014] A kind of method that utilizes zirconium carbonate production waste water to prepare zirconium sulfate tetrahydrate, its process step is:

[0015] (1) Adjust the pH value of 2000L zirconium carbonate production wastewater to 5 with dilute lye, and settle for 60 minutes;

[0016] (2) Then pump the waste water into the effective filtration area of ​​25m 2 A plate-and-frame filter press is used for press filtration, and after the press filtration is completed, it is purged with compressed air for 1 hour, and the plate is unloaded to obtain 41.8 kg of zirconium hydroxide;

[0017] (3) Dissolve zirconium hydroxide in 21L of 98% sulfuric acid at a mass:volume ratio of 1:0.5, heat the system to 40 degrees Celsius to completely dissolve zirconium hydroxide, and then filter to remove mechanical impurities;

[0018] (4) Add 98% concentrated sulfuric acid to the filtrate to adjust the sulfuric acid concentration of the system to 50%, naturally cool to 40 degrees Celsius, separate...

Embodiment 2

[0020] A kind of method that utilizes zirconium carbonate production waste water to prepare zirconium sulfate tetrahydrate, its process step is:

[0021] (1) Adjust the pH value of 3000L zirconium carbonate production wastewater to 6 with dilute lye, and let it settle naturally for 55 minutes;

[0022] (2) Then pump the waste water into the effective filtration area of ​​40m 2 Plate and frame filter press press filter, after the press filter is completed, use compressed air to blow for 1.2 hours, unload the plate, and obtain 63kg of zirconium hydroxide;

[0023] (3) Dissolve zirconium hydroxide in 63L of 98% sulfuric acid at a ratio of mass: volume of 1:1, heat the system to 50 degrees Celsius to completely dissolve zirconium hydroxide, and then filter to remove mechanical impurities;

[0024] (4) Add 98% concentrated sulfuric acid to the filtrate to adjust the sulfuric acid concentration of the system to 55%, naturally cool to 40 degrees Celsius, separate the mother liquor b...

Embodiment 3

[0026] A kind of method that utilizes zirconium carbonate production waste water to prepare zirconium sulfate tetrahydrate, its process step is:

[0027] (1) Adjust the pH value of 4000L zirconium carbonate production wastewater to 7 with dilute lye, and settle naturally for 50 minutes;

[0028] (2) Then pump the waste water into the effective filtration area of ​​30m 2 Plate and frame filter press press filter, after the press filter is completed, use compressed air to blow for 1.4 hours, unload the plate, and obtain 87kg of zirconium hydroxide;

[0029] (3) Dissolve zirconium hydroxide in 174L of 98% sulfuric acid at a ratio of mass:volume of 1:2, heat the system to 55 degrees Celsius to completely dissolve zirconium hydroxide, and then filter to remove mechanical impurities;

[0030] (4) Add 98% concentrated sulfuric acid to the filtrate to adjust the sulfuric acid concentration of the system to 60%, naturally cool to 40 degrees Celsius, separate the mother liquor by sucti...

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Abstract

The invention discloses a method for preparing zirconium sulfate tetrahydrate with zirconium carbonate production wastewater. The method comprises the technical steps of: (1) adjusting a pH (Potential of Hydrogen) value of the zirconium carbonate production wastewater with dilute alkali, performing sedimentation, (2) pumping the wastewater into a plate-and-frame filter press for press filtration, purging with compressed air after the press filtration, removing a plate, obtaining zirconium hydroxide, (3) dissolving zirconium hydroxide in sulfuric acid or zirconium sulfate tetrahydrate mother liquor at a mass-volume ratio of 1:(1-3), heating to 50-60 DEG C to completely dissolve zirconium acyl hydroxide, filtering off mechanical impurities, and (4) adding concentrated sulfuric acid into filtrate to adjust a system sulfuric acid concentration to 50-70%, naturally cooling to 40 DEG C for crystallization, centrifuging, and obtaining zirconium sulfate tetrahydrate. The method is simple in technology, prepares zirconium sulfate tetrahydrate with the zirconium carbonate production wastewater, and prevents the zirconium carbonate production wastewater from influencing an environment; obtained zirconium sulfate tetrahydrate is high in purity and is up to a national first grade standard; since the zirconium sulfate tetrahydrate mother liquor is recycled, the production cost is lowered effectively; and environmental resources are saved.

Description

technical field [0001] The invention belongs to the technical field of zirconium carbonate production wastewater treatment, in particular to a method for preparing zirconium sulfate tetrahydrate from zirconium carbonate production wastewater. Background technique [0002] At present, the domestic production of basic zirconium carbonate mainly adopts a two-step process, the steps are: zirconium oxychloride → basic zirconium sulfate → adding carbonate → zirconium carbonate. A large amount of industrial wastewater is produced during washing of basic zirconium carbonate, exceeding 15 tons / ton of product, and the mass content of ZrO2 is greater than 4g / L, which must be recycled. At present, some domestic enterprises neutralize the waste water with the waste alkali water produced in the production of zirconium oxychloride, and add water purifiers for sedimentation treatment. The resulting waste residue contains ZrO 2 It contains about 5% and contains a large amount of impuritie...

Claims

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Application Information

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IPC IPC(8): C01G25/06
Inventor 张尚吴江邱才华黎隆湖
Owner JIANGXI KINGAN HI TECH
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