CN215559047U - Device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater - Google Patents
Device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater Download PDFInfo
- Publication number
- CN215559047U CN215559047U CN202123078530.2U CN202123078530U CN215559047U CN 215559047 U CN215559047 U CN 215559047U CN 202123078530 U CN202123078530 U CN 202123078530U CN 215559047 U CN215559047 U CN 215559047U
- Authority
- CN
- China
- Prior art keywords
- ruthenium
- oxidation reactor
- storage tank
- containing wastewater
- booster pump
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The utility model relates to a device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater, belonging to the technical field of special chemical production devices. The device comprises a primary oxidation reactor, a ruthenium tetroxide gas storage tank, a booster pump and a hydrochloric acid atomizer; a discharge pipeline of the primary oxidation reactor is connected with a ruthenium tetroxide gas storage tank; a discharge pipeline of the ruthenium tetroxide gas storage tank is connected with a booster pump; the hydrochloric acid atomizer and the booster pump are respectively connected with the secondary oxidation reactor through discharge pipelines. The device provided by the utility model is adopted for production, has the advantages of high production efficiency, high product yield, low energy consumption, environmental friendliness and easy realization of industrial production.
Description
Technical Field
The utility model belongs to the technical field of special chemical production devices, and particularly relates to a device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater.
Background
Ruthenium trichloride is one of the most important compounds of ruthenium, and is an important chemical raw material in the fields of heterogeneous catalysis, homogeneous catalysis, electroplating, coating and the like. However, ruthenium resources in China are scarce, and the annual output is only kilogram and less than 1% of the demand. Therefore, it is necessary to realize recycling of ruthenium.
Currently, ruthenium is generally recovered from spent catalysts by an alkali fusion method, an ion exchange method, activated carbon adsorption, and a membrane separation method. Among them, the most common is the oxidative distillation method, which comprises the following processes: oxidation-absorption-concentration crystallization-drying and packaging, while the oxidative distillation method has high energy consumption and complex working procedures. For example, patent CN 106335932B adopts a conventional method, namely an oxidative distillation method, and the ruthenium trichloride powder is obtained by absorbing and reducing the ruthenium trichloride solution into a chlororuthenate solution by dilute hydrochloric acid, dispersing the chlororuthenate solution by a dispersion solvent, and then performing spray drying.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects in the related technology, the utility model provides the device for preparing ruthenium trichloride by utilizing the ruthenium-containing wastewater, and the device is adopted for production, so that the production efficiency is high, the product yield is high, the energy consumption is low, the environment is friendly, and the industrial production is easy to realize.
The utility model provides a device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater, which comprises a primary oxidation reactor, a ruthenium tetroxide gas storage tank, a booster pump and a hydrochloric acid atomizer; a discharge pipeline of the primary oxidation reactor is connected with a ruthenium tetroxide gas storage tank; a discharge pipeline of the ruthenium tetroxide gas storage tank is connected with a booster pump; the hydrochloric acid atomizer and the booster pump are respectively connected with the secondary oxidation reactor through discharge pipelines; the secondary oxidation reactor is a reaction and drying integrated machine and comprises an oxidation device and a drying device.
Preferably, the drying device is a vacuum freezer.
Preferably, the drying device further comprises a waste liquid storage tank connected with the drying device.
Preferably, the device also comprises a tail gas absorption device connected with the secondary oxidation reactor.
Preferably, the device also comprises a ruthenium-containing wastewater storage tank; the ruthenium-containing wastewater storage tank is connected with the primary oxidation reactor through a discharge pipeline.
Preferably, the device further comprises an oxidant storage tank; and the oxidant storage tank is connected with the primary oxidation reactor through a discharge pipeline.
Preferably, a stirrer is arranged in the primary oxidation reactor.
Preferably, valves are respectively arranged on pipelines connected with the primary oxidation reactor, the ruthenium tetroxide gas storage tank, the booster pump, the hydrochloric acid atomizer and the secondary oxidation reactor.
According to the device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater, which is provided by the utility model, the gas phase method is adopted for reaction, the ruthenium tetroxide gas is pressurized, the pressurized ruthenium tetroxide gas and the atomized hydrochloric acid gas are mixed for reaction, and the gas-gas reaction mode is adopted, so that the ruthenium tetroxide and the atomized hydrochloric acid are fully contacted, the reaction speed is high, the reaction is full, the production efficiency and the yield are improved, a multi-stage absorption device is not required, and the energy consumption is low.
Furthermore, the secondary oxidation reactor adopts a reaction and drying integrated machine, can realize continuous production, directly dries and removes by-product water and the like in the product, does not need concentration and crystallization, and further reduces energy consumption. And the secondary oxidation reactor is connected with a tail gas absorption device, so that the environment is not polluted.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the utility model and together with the description serve to explain the utility model without limiting the utility model. In the drawings:
FIG. 1 is a schematic structural diagram of an apparatus for producing ruthenium trichloride from ruthenium-containing wastewater according to the present invention;
wherein, the device comprises a 1-first-stage oxidation reactor, a 2-ruthenium tetroxide gas storage tank, a 3-booster pump, a 4-hydrochloric acid atomizer, a 5-second-stage oxidation reactor, a 6-tail gas absorption device, a 7-waste liquid storage tank, an 8-ruthenium-containing wastewater storage tank, a 9-oxidant storage tank, a 10-stirrer and a 11-valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the utility model provides a device for preparing ruthenium trichloride by using ruthenium-containing wastewater, which comprises a primary oxidation reactor 1, a ruthenium tetroxide gas storage tank 2, a booster pump 3 and a hydrochloric acid atomizer 4; a discharge pipeline of the primary oxidation reactor 1 is connected with a ruthenium tetroxide gas storage tank 2; a discharge pipeline of the ruthenium tetroxide gas storage tank 2 is connected with a booster pump 3; the hydrochloric acid atomizer 4 and the booster pump 3 are respectively connected with the secondary oxidation reactor 5 through discharge pipelines; the secondary oxidation reactor 5 is a reaction and drying integrated machine and comprises an oxidation device and a drying device.
When the device works, ruthenium-containing wastewater and an oxidant react in a primary oxidation reactor 1 to obtain ruthenium tetroxide gas, the ruthenium tetroxide gas enters a ruthenium tetroxide gas storage tank 2, hydrochloric acid atomized by a hydrochloric acid atomizer 4 and ruthenium tetroxide gas pressurized by a booster pump 3 both enter a secondary oxidation reactor 5 to react (the ruthenium tetroxide gas and the hydrochloric acid are atomized and then sprayed into an oxidation device of the secondary oxidation reactor 5 by the booster pump 3 to carry out rapid reaction, and a product after the reaction is introduced into a drying device to be dried).
In order to realize continuous production, the drying device is preferably a vacuum freezer, and the by-product water and the tail gas are removed through vacuum freeze drying.
In order to facilitate the reception and treatment of the waste liquid after the drying treatment, the present invention preferably further comprises a waste liquid storage tank 7 connected to the drying device.
In order to avoid environmental pollution caused by the reaction by-product chlorine gas, the present invention preferably further comprises a tail gas absorption device 6 connected to the secondary oxidation reactor 5.
In order to facilitate the control of the reaction, the present invention preferably further comprises a ruthenium-containing wastewater storage tank 8; the ruthenium-containing wastewater storage tank 8 is connected with the primary oxidation reactor 1 through a discharge pipeline.
To facilitate control of the reaction, the present invention preferably further comprises an oxidant storage tank 9; the oxidant storage tank 9 is connected with the primary oxidation reactor 1 through a discharge pipeline.
In order to achieve sufficient reaction, it is preferable that the primary oxidation reactor 1 of the present invention is provided with a stirrer 10.
In order to facilitate the control of the reaction, it is preferable that valves 11 are provided in the lines connected to the primary oxidation reactor 1, the ruthenium tetroxide gas tank 2, the booster pump 3, the hydrochloric acid atomizer 4, and the secondary oxidation reactor 5, respectively.
Example 1
(1) 50g of hydrochloric acid is charged into a hydrochloric acid atomizer;
(2) adding 1kg of ruthenium-containing wastewater (the content of ruthenium in the wastewater is 500ppm through ICP-MS detection) into a primary oxidation reactor, dropwise adding 10g of hypochlorous acid into the primary oxidation reactor at room temperature, controlling the reaction temperature of the primary oxidation reactor to be 65 ℃, the reaction time to be 2 hours, and the magnetic stirring speed to be 100 r/min;
(3) introducing the gas reacted in the step (2) into a ruthenium tetroxide gas holder;
(4) introducing the gas in the ruthenium tetroxide gas holder in the step (3) after being pressurized by a booster pump (the pressure of a pressurized gas outlet is 1 MPa) and the hydrochloric acid atomized in the step (1) into a secondary oxidation reactor for reaction, and vacuum freeze-drying the reaction product to obtain a RuCl product30.45g of solid powder, the yield is 90 percent, and the obtained by-product chlorine is pumped into a tail gas absorption device.
Comparative example 1
(1) 50g of hydrochloric acid is respectively filled into three-stage absorption devices which are connected in series;
(2) adding 1kg of ruthenium-containing wastewater (the content of ruthenium in the wastewater is 500ppm detected by ICP-MS) into a three-neck flask, and dropwise adding 10g of hypochlorous acid at room temperature, wherein the reaction temperature is 75 ℃, the reaction time is 1h, and the magnetic stirring speed is 200 r/min;
(3) introducing the gas reacted in the step (2) into an absorption device;
(4) introducing the by-product obtained in the step (3) into a tail gas treatment device for absorption;
(5) and (4) putting the ruthenic acid solution reduced by the three-stage absorption device in the step (3) into a rotating device for reduced pressure distillation at the temperature of 90 ℃ and the pressure of-0.01 MPa to obtain 0.2567g of solid powder with the yield of 51.34%.
TABLE 1 preparation of RuCl in example 1 and comparative example 13Performance and yield
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater is characterized by comprising a primary oxidation reactor, a ruthenium tetroxide gas storage tank, a booster pump and a hydrochloric acid atomizer; a discharge pipeline of the primary oxidation reactor is connected with a ruthenium tetroxide gas storage tank; a discharge pipeline of the ruthenium tetroxide gas storage tank is connected with a booster pump; the hydrochloric acid atomizer and the booster pump are respectively connected with the secondary oxidation reactor through discharge pipelines; the secondary oxidation reactor is a reaction and drying integrated machine and comprises an oxidation device and a drying device.
2. The apparatus according to claim 1, wherein the drying device is a vacuum freezer.
3. The apparatus for producing ruthenium trichloride according to claim 1, further comprising a waste liquid storage tank connected to the drying apparatus.
4. The apparatus for preparing ruthenium trichloride according to claim 1, further comprising a tail gas absorption unit connected to the secondary oxidation reactor.
5. The apparatus for preparing ruthenium trichloride by using ruthenium-containing wastewater according to claim 1, further comprising a ruthenium-containing wastewater storage tank; the ruthenium-containing wastewater storage tank is connected with the primary oxidation reactor through a discharge pipeline.
6. The apparatus for producing ruthenium trichloride using ruthenium-containing wastewater according to claim 1, further comprising an oxidizing agent storage tank; and the oxidant storage tank is connected with the primary oxidation reactor through a discharge pipeline.
7. The apparatus for preparing ruthenium trichloride according to claim 1, wherein a stirrer is provided in the primary oxidation reactor.
8. The apparatus for preparing ruthenium trichloride according to claim 1, wherein valves are provided in the lines connecting the primary oxidation reactor, the ruthenium tetroxide gas tank, the booster pump, the hydrochloric acid atomizer, and the secondary oxidation reactor, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123078530.2U CN215559047U (en) | 2021-12-09 | 2021-12-09 | Device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202123078530.2U CN215559047U (en) | 2021-12-09 | 2021-12-09 | Device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN215559047U true CN215559047U (en) | 2022-01-18 |
Family
ID=79853710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202123078530.2U Active CN215559047U (en) | 2021-12-09 | 2021-12-09 | Device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN215559047U (en) |
-
2021
- 2021-12-09 CN CN202123078530.2U patent/CN215559047U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102247871B (en) | Preparation method of solid acid catalyst used for biomass hydrolysis | |
| CN101485990B (en) | Solid supported heteropoly acid catalyst and preparation method thereof | |
| CN111254456B (en) | Electrochemical synthesis method of 2-nitro-4-methylsulfonylbenzoic acid | |
| CN102816045B (en) | Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production | |
| CN108822073B (en) | Preparation method and application of vinyl sulfate | |
| JP2020522530A (en) | System and process for co-producing dimethyl carbonate and ethylene glycol | |
| CN111330645A (en) | Preparation method and application of bifunctional MOF (metal organic framework) nano catalyst for degrading p-nitrophenol and fixing nitrogen at room temperature simultaneously | |
| CN1439599A (en) | Production for stable chlorinedioxide solution | |
| CN104998689A (en) | Anion resin-carried peroxyphosphotungstic acid, its preparation method and use, and epoxycycloparaffin synthesis method | |
| WO2020192477A1 (en) | Catalyst and method for preparing isopentyl diol | |
| CN215559047U (en) | Device for preparing ruthenium trichloride by utilizing ruthenium-containing wastewater | |
| CN103626681A (en) | Method for preparing 4,4'-dinitrostilbene-2,2'-disulfonic acid | |
| CN109550522A (en) | A kind of wet oxidizing catalyst, preparation method and its application handling refinery basic sewage | |
| CN108864030A (en) | A method of carbon dioxide synthesizing annular carbonate is catalyzed with new catalyst | |
| CN105013539A (en) | Solid phase catalyst for preparing methyl formate, preparation method therefor and application thereof | |
| CN113149827A (en) | Method for synthesizing alkynoic acid by using terminal alkyne and carbon dioxide | |
| CN104328150B (en) | A kind of method that micro passage reaction continuously synthesizes 2,3 pairs of diketone of ((4 fluorophenyl) sulfenyl) naphthalene 1,4 | |
| CN114105905A (en) | Preparation method and synthesis system of N-tertiary butyl-2-benzothiazole sulfonamide | |
| CN203440262U (en) | Device for producing trans-1, 2-dichloroethylene with acetylene by adopting catalytic chlorination method | |
| CN109675508B (en) | Preparation method and application of perfluorosulfonic acid resin/solid acid microfibrillated microchannel reactor | |
| CN103864575A (en) | Method for preparing 1,2-pentanediol | |
| CN105819564A (en) | Treatment method for paraformaldehyde wastewater | |
| CN112174857A (en) | Preparation method of 3-hydroxypropanesulfonic acid | |
| CN110038636A (en) | A kind of AgI/Ag-Ce-2MI composite photo-catalyst and its preparation and application | |
| CN112479459B (en) | Preparation method of preferential water permeable membrane, morpholine wastewater treatment method and morpholine substance recovery method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |