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Method for preparing ruthenium trichloride hydrate by adopting ruthenium-containing wastewater

A technology of ruthenium trichloride hydrate and ruthenium trichloride, which is applied in the field of preparing ruthenium trichloride hydrate, can solve the problems of long reaction time, low ruthenium enrichment rate, difficult product quality, etc., and achieve improved absorption rate and Reaction efficiency, increased gas-liquid contact area, and effective recycling effects

Pending Publication Date: 2021-12-31
HAIKE GRP RES INST OF INNOVATION & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these two methods have disadvantages such as complex process, high energy consumption, low ruthenium enrichment rate, many impurity elements and environmental pollution.
At the same time, when preparing ruthenium trichloride, sodium chlorate plus sulfuric acid system is usually used, which has problems such as many times of distillation, long reaction time, difficult product quality, and low product yield.
[0004] Patent CN103540760A discloses a method for recovering ruthenium from waste ruthenium hydroxide / diatomite catalyst, but this method uses highly toxic chemical hydrazine hydrate in the recovery process, which has potential safety hazards
And the obtained ruthenium sulfide precipitate is difficult to remove the S element during subsequent catalyst regeneration, which increases the difficulty and cost of the process

Method used

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  • Method for preparing ruthenium trichloride hydrate by adopting ruthenium-containing wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) According to figure 1 Build the reaction device as shown, and check the air tightness of the device (two absorption devices are installed, and two layers of microporous sand core glass plates are installed in each absorption device, and the pore diameter of the microporous sand core is 1 μm).

[0049] (2) Accurately weigh 30 kg of ruthenium-containing spent catalyst solution (brown black, use ICP-OES to detect Ru content 500 ppm), add it to the distillation reactor, weigh 200 g of hypochlorous acid (mass concentration 20%) and add it to the oxidant storage bottle ;

[0050] (3) 3L of HCl with a mass concentration of 15% is respectively configured in the 1st to 2nd-stage absorption bottles, and 30g of absolute ethanol is added;

[0051] (4) Turn on the gas cylinder switch and set the gas purge rate to 0.4L / min;

[0052] (5) Turn on the dropping funnel switch and set the pump speed to 10mL / min;

[0053] (6) Oxidation reaction at 50°C, the liquid in the primary abso...

Embodiment 2

[0064] (1) According to figure 1 Build the reaction device as shown, and check the air tightness of the device (there are 3 absorption devices, and each absorption device is equipped with 2 layers of glass plates with microporous sand cores, and the pore diameter of the microporous sand cores is 1 μm).

[0065] (2) Accurately take by weighing 30kg of spent catalyst solution containing ruthenium (brown yellow, after detecting Ru content 30ppm), add in the distillation reactor, take by weighing 300g sodium chlorate (available chlorine content 10%), add in the oxidant storage bottle;

[0066] (3) Prepare 1 L of HCl absorption solution with a mass concentration of 5% in 1-3 absorption bottles, and add 10 g of absolute ethanol;

[0067] (4) Turn on the gas cylinder switch and set the gas purge rate to 0.4L / min;

[0068] (5) Turn on the dropping funnel switch and set the pump speed to 5mL / min;

[0069] (6) Oxidation reaction at 50°C, the liquid in the first-level absorption bottle...

Embodiment 3

[0073] (1) According to figure 1 Build the reaction device as shown, and check the air tightness of the device (two absorption devices are installed, and 5 layers of microporous sand core glass plates are installed in each absorption device, and the pore diameter of the microporous sand core is 100 μm).

[0074] (2) Accurately weigh 30 kg of ruthenium-containing spent catalyst solution (brownish yellow, 30 ppm of Ru content after detection), add it to the distillation reactor, weigh 300 g of hydrogen peroxide (mass concentration 30%), and add it to the oxidant storage bottle;

[0075] (3) Prepare 1 L of HCl absorption solution with a mass concentration of 5% in 1-2 absorption bottles, and add 10 g of absolute ethanol;

[0076] (4) Turn on the gas cylinder switch and set the gas purge rate to 1.0L / min;

[0077] (5) Turn on the dropping funnel switch and set the pump speed to 5mL / min;

[0078] (6) Oxidation reaction at 30°C, the liquid in the primary absorption bottle turns li...

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Abstract

The invention provides a method for preparing ruthenium trichloride hydrate by adopting ruthenium-containing wastewater, and belongs to the technical field of special chemicals. The method comprises the following steps: mixing ruthenium-containing wastewater and an oxidizing agent, reacting at 25-50 DEG C to obtain ruthenium tetroxide gas, introducing compressed gas into the ruthenium-containing wastewater to transfer the ruthenium tetroxide gas into an absorption device containing an absorption liquid, and reacting ruthenium tetroxide with the absorption liquid to obtain the absorption liquid containing ruthenium trichloride or H2RuCl5; and carrying out reduced pressure evaporation on the absorption liquid containing ruthenium trichloride or H2RuCl5 to obtain the ruthenium trichloride hydrate. The method provided by the invention is low in energy consumption and mild in reaction, and can realize recovery of trace (ppm level) Ru in the aqueous solution.

Description

technical field [0001] The invention belongs to the technical field of special chemicals, and in particular relates to a method for preparing ruthenium trichloride hydrate by using ruthenium-containing wastewater. Background technique [0002] Ruthenium (Ru) belongs to specialty chemicals because of its unique, stable and efficient catalytic properties. Ruthenium has shown great industrial value in industrial catalysis and organic synthesis. However, my country's ruthenium resources are scarce, and the distribution is sparse, and it is associated with other metal minerals, which makes the smelting of ruthenium difficult and costly. At the same time, my country's chemical industry produces a large number of invalid ruthenium-based catalysts every year, and the content of ruthenium in these invalid ruthenium-based catalysts is much higher than that of primary primary mineral resources. In addition, in recent years, the price of ruthenium has been rising continuously. Therefor...

Claims

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Application Information

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IPC IPC(8): C02F9/10B01D53/78B01D53/68C01G55/00C02F101/20
CPCC02F1/72C02F1/04B01D53/78B01D53/68C01G55/005C01G55/001C02F2101/20
Inventor 谢芳苗力孝刘天雷魏志凯
Owner HAIKE GRP RES INST OF INNOVATION & TECH
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