Method and device for recovering platinum in platinum liquid and sealing detection method

Abstract

The invention discloses a method and device for recycling platinum in platinum liquid and a sealing detection method, the platinum content in the platinum liquid is lower than 1.32 g / L, and the pH value is 10-10.5, the method for recycling platinum in the platinum liquid comprises the following steps: adding hydrochloric acid into the platinum liquid to adjust the pH value of the solution to a first preset value, the first preset value is 0.5-1, and a first solution is obtained; hydrogen peroxide is slowly added into the first solution, stirring is conducted for a first preset duration, a second solution is obtained, and the first preset duration ranges from 30 min to 40 min; after ammonium chloride is added into the second solution, platinum yellow is obtained through precipitation, and the adding amount of the ammonium chloride is 3.1-3.5 times of the platinum content; and calcining the precipitated platinum yellow to obtain the finished product platinum.

Description

Technical Field

[0001] The invention relates to the field of chemical technology, and in particular to a method and device for recovering platinum from platinum liquid, and a sealing detection method. Background Art

[0002] Platinum, commonly known as white gold, has an atomic number of 78 and is located in the sixth period of the periodic table, group VIII. It is one of the precious metals. Platinum belongs to the platinum series elements, with an atomic weight of 195.05 and a density of 21.45 g / cm 3 , melting point 1772℃, boiling point 3827℃.

[0003] The recovery rate of platinum in the platinum solution in the prior art is low, especially when the platinum content in the platinum solution is lower than 1.32 g / L and the pH value is 10-10.5.

[0004] The above contents are only used to assist in understanding the technical solution of the present invention and do not constitute an admission that the above contents are prior art. Summary of the invention

[0005] The main purpose of the present invention is to provide a method and device for recovering platinum from platinum liquid and a sealing detection method, aiming to solve the above-mentioned problems in the prior art.

[0006] To achieve the above object, the present invention provides a method for recovering platinum in a platinum solution, wherein the platinum content in the platinum solution is lower than 1.32 g / L and the pH value is 10-10.5. The method for recovering platinum in the platinum solution comprises:

[0007] Adding hydrochloric acid to the platinum solution to adjust the pH value of the solution to a first preset value, wherein the first preset value is 0.5-1, to obtain a first solution;

[0008] Slowly add hydrogen peroxide to the first solution and stir for a first preset time to obtain a second solution, wherein the first preset time is 30 min-40 min;

[0009] After adding ammonium chloride to the second solution, platinum yellow is precipitated, and the amount of ammonium chloride added is 3.1-3.5 times the platinum content;

[0010] The precipitated platinum yellow is calcined to obtain finished platinum.

[0011] Preferably, in the method for recovering platinum from platinum liquid, in the step of slowly adding hydrogen peroxide to the first solution and stirring for a first preset time to obtain the second solution,

[0012] Pt 2+ →Pt 4+ .

[0013] Preferably, in the method for recovering platinum from the platinum solution, in the step of adding ammonium chloride to the second solution to precipitate platinum yellow, Pt 4+ +NH4Cl→PtCl4.

[0014] Preferably, in the method for recovering platinum from platinum liquid, calcining the precipitated platinum yellow to obtain finished platinum comprises:

[0015] The precipitated platinum yellow is calcined at a first preset temperature to obtain finished platinum, wherein the first preset temperature is 600°C-650°C.

[0016] Preferably, in the method for recovering platinum from the platinum solution, after the step of adding ammonium chloride to the second solution to precipitate platinum yellow and before the step of calcining the precipitated platinum yellow to obtain finished platinum, the recovery method further comprises:

[0017] The precipitated platinum yellow was filtered and washed out.

[0018] Preferably, in the method for recovering platinum from the platinum solution, adding hydrochloric acid to the platinum solution to adjust the pH value of the solution to a first preset value comprises:

[0019] The platinum solution is placed in a reaction kettle, and industrial-grade hydrochloric acid is slowly added into the reaction kettle to adjust the pH value of the solution to 1.

[0020] In order to achieve the above object, the present invention also provides a recovery device for the above-mentioned method for recovering platinum in the platinum solution, the recovery device comprising:

[0021] A reaction kettle, used for reacting platinum in the platinum liquid to generate a mixed solution containing platinum yellow;

[0022] The filtering device is arranged downstream of the reaction kettle and is used for filtering the platinum yellow from the mixed solution.

[0023] Preferably, in the recovery device, the filtering device comprises:

[0024] The filter outer cylinder comprises an upper port and a lower port which are connected vertically and a cavity which is connected to the upper port and the lower port respectively;

[0025] An upper cover body, which covers the upper port and has an upper opening;

[0026] A lower cover body, which is arranged on the lower port, and the lower cover body is penetrated by a lower opening;

[0027] An upper sealing body and a lower sealing body are detachably disposed in the cavity, the upper sealing body is penetrated by a first through hole, the lower sealing body is penetrated by a second through hole, the second through hole is communicated with the lower opening, and the first through hole is communicated with the upper opening;

[0028] A filter membrane structure provided in a cylindrical body, wherein the upper end of the filter membrane structure is sealed on the upper sealing body, and the lower end is sealed on the lower sealing body, a first cavity is formed between the filter membrane structure and the filter outer cylinder, the first cavity is communicated with the first through hole, and the lower end of the filter membrane is communicated with the second through hole;

[0029] The mixed solution enters from the upper opening, enters the first cavity through the first through hole, and the liquid filtered by the filter membrane structure enters the filter membrane structure and flows out from the lower opening through the second through hole.

[0030] In order to achieve the above object, the present invention also provides a sealing detection method of the above recovery device, characterized in that it includes:

[0031] Applying a detection substance to the inner wall of the recovery device;

[0032] Immersing the recovery device in water, and when the detection substance changes color, it is determined that the recovery device is leaking;

[0033] Wherein, the test substances include, by mass:

[0034] Anhydrous ammonium chloride powder: 2-2.5 parts;

[0035] Phenolphthalein for acid-base indication: 1-3 parts;

[0036] Macroporous adsorption resin: 2-3 parts;

[0037] Solvent: 16-19 parts.

[0038] Preferably, in the sealing detection method, before the step of applying the detection substance to the inner wall of the recovery device, the method comprises:

[0039] First, the phenolphthalein and the anhydrous ammonium chloride powder are uniformly mixed to obtain a first mixture;

[0040] Then, the first mixture is mixed with a macroporous adsorption resin and a solvent to form a color-changing solution;

[0041] Correspondingly, the step of applying the detection substance to the inner wall of the recovery device comprises:

[0042] Brush the color-changing solution on the inner wall of the recovery device, and then carry out the sealing test after it dries.

[0043] The present invention has at least the following beneficial effects:

[0044] The present invention adds hydrochloric acid to the platinum liquid to adjust the pH value of the solution to a first preset value, wherein the first preset value is 0.5-1, to obtain a first solution; slowly adds hydrogen peroxide to the first solution and stirs for a first preset time to obtain a second solution, wherein the first preset time is 30 min-40 min; adds ammonium chloride to the second solution to precipitate platinum yellow, wherein the amount of ammonium chloride added is 3.1-3.5 times the content of platinum; calcines the precipitated platinum yellow to obtain finished platinum, thereby reducing the cost of recovering platinum, and directly precipitating and calcining the platinum salt to obtain platinum powder, and achieving a high recovery rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 A schematic diagram of an embodiment of a method for recovering platinum from platinum liquid provided by the present invention;

[0046] Figure 2 A schematic diagram of the filtration device.

[0047] Reference numerals of the present invention:

[0048]

[0049]

[0050] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings in conjunction with the embodiments. DETAILED DESCRIPTION

[0051] The technical solution of the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. The present invention will be described in detail below with reference to the accompanying drawings and in conjunction with the embodiments. It should be noted that the embodiments of the present invention and the features in the embodiments can be combined with each other without conflict.

[0052] In the embodiments of the present invention, the term "and / or" describes the association relationship of associated objects, indicating that three relationships may exist. For example, A and / or B may represent three situations: A exists alone, A and B exist at the same time, and B exists alone. The character " / " generally indicates that the associated objects before and after are in an "or" relationship.

[0053] It should be noted that the terms "first", "second", etc. in the specification and claims of the present invention and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence.

[0054] In the embodiments of the present invention, the term "plurality" refers to two or more than two, and other quantifiers are similar.

[0055] In the present invention, unless otherwise specified, the directional words used, such as "up, down, top, bottom", usually refer to the directions shown in the drawings, or to the components themselves in the vertical, perpendicular or gravity directions; similarly, for ease of understanding and description, "inside and outside" refer to the inside and outside relative to the outline of each component itself, but the above-mentioned directional words are not used to limit the present invention.

[0056] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings. However, it can be understood by those skilled in the art that in the embodiments of the present invention, many technical details are proposed in order to enable the reader to better understand the present invention. However, even without these technical details and various changes and modifications based on the following embodiments, the technical scheme claimed in the present invention can also be implemented. The division of the following embodiments is for the convenience of description and should not constitute any limitation on the specific implementation of the present invention. The various embodiments can be combined and referenced with each other under the premise of no contradiction.

[0057] The invention provides a method for recovering platinum in a platinum solution. The platinum content in the platinum solution is lower than 1.32 g / L, and the pH value is 10-10.5. Figure 1 The schematic diagram of the method for recovering platinum from platinum solution of the present invention is shown.

[0058] In step S100, hydrochloric acid is added to the platinum solution to adjust the pH value of the solution to a first preset value to obtain a first solution, wherein the first preset value is 0.5-1.

[0059] Specifically, the platinum solution is placed in a reaction kettle, and industrial-grade hydrochloric acid is slowly added into the reaction kettle to adjust the pH value of the solution to 1.

[0060] In other feasible implementations, the first preset value may also be 0.7, 0.8, or 0.9.

[0061] In step S200, hydrogen peroxide is slowly added to the first solution and stirred for a first preset time to obtain a second solution, wherein the first preset time is 30 min-40 min.

[0062] Specifically, Pt 2+ →Pt 4+ That is, divalent platinum is converted into tetravalent platinum by adding hydrogen peroxide.

[0063] The first preset duration may also be 35 minutes.

[0064] In step S300, ammonium chloride is added to the second solution to precipitate platinum yellow, and the amount of ammonium chloride added is 3.1-3.5 times the platinum content.

[0065] Specifically, Pt 4+ +NH4C l→PtC l4. That is, by adding ammonium chloride, tetravalent platinum is converted into platinum salt. The precipitated platinum yellow can be filtered and washed out.

[0066] In other embodiments, the amount of ammonium chloride added may be 3.2 times or 3.3 times the platinum content.

[0067] In step S400, the precipitated platinum yellow is calcined to obtain finished platinum. Specifically, the precipitated platinum yellow is calcined at a first preset temperature to obtain finished platinum, and the first preset temperature is 600°C-650°C.

[0068] The first preset temperature may also be 620°C or 630°C.

[0069] The present invention adds hydrochloric acid to the platinum liquid to adjust the pH value of the solution to a first preset value, wherein the first preset value is 0.5-1, to obtain a first solution; slowly adds hydrogen peroxide to the first solution and stirs for a first preset time to obtain a second solution, wherein the first preset time is 30 min-40 min; adds ammonium chloride to the second solution to precipitate platinum yellow, wherein the amount of ammonium chloride added is 3.1-3.5 times the content of platinum; calcines the precipitated platinum yellow to obtain finished platinum, thereby reducing the cost of recovering platinum, and directly precipitating and calcining the platinum salt to obtain platinum powder, and achieving a high recovery rate.

[0070] In order to verify the beneficial effects of the present invention, the following is a comparative example and a comparative example. 2L of platinum solution was taken respectively, the platinum content in the platinum solution was lower than 1.32g / L, and the pH value was 10-10.5 to conduct experiments.

[0071] Example 1

[0072] S1, adding hydrochloric acid to 2L of platinum solution to adjust the pH value of the solution to 1, thereby obtaining a first solution, wherein the platinum content is less than 1.32 g / L and the pH value of the platinum solution is 10-10.5;

[0073] S2, slowly adding 500 ml of hydrogen peroxide to the first solution and stirring for 30 minutes to obtain a second solution;

[0074] S3, adding ammonium chloride to the second solution, leaving it to stand for 1 hour, precipitating platinum yellow, and obtaining a tail liquid, wherein the amount of ammonium chloride added is 3.1 times the platinum content;

[0075] S4, calcining the precipitated platinum yellow to obtain finished platinum.

[0076] Comparative Example 1

[0077] Add 50 g of iron powder to 2 L of platinum solution, stir for 30 min, let stand for 1 h, and then test the tail liquid.

[0078] Comparative Example 2

[0079] After adding hydrochloric acid to 2L of platinum solution to adjust the pH value of the solution to 1, add 50g of iron powder, stir for 30min, let stand for 1h, and then test the tail liquid.

[0080] Table 1 Comparison of the effects of the embodiments and comparative examples

[0081] Platinum content in tail liquid / ppm Example 1 8.3 Comparative Example 1 185 Comparative Example 2 37

[0082] As can be seen from Table 1, the recovery method provided by the present invention has low cost for recovering platinum, and platinum powder can be obtained by directly precipitating the platinum salt and then calcining it, and the recovery rate is high; Comparative Examples 1 and 2 not only have high tail liquid content, but the replaced platinum also needs to be recovered through aqua regia, ammonium chloride precipitation, and calcination steps to obtain crude platinum powder, and the recovery cost is high.

[0083] Furthermore, the recovery rate of platinum in the present invention is greater than 95%.

[0084] The present invention also provides a recovery device for the above-mentioned method of recovering platinum in platinum liquid. The recovery device comprises a reactor and a filtering device 1, wherein the reactor is used to react platinum in the platinum liquid to generate a mixed solution containing platinum yellow; and the filtering device 1 is arranged downstream of the reactor and is used to filter out platinum yellow from the mixed solution.

[0085] Specifically, Figure 2As shown, the filter device 1 includes a filter outer cylinder 11, an upper cover body 12, a lower cover body 13, an upper sealing body 14 and a lower sealing body 15, and a filter membrane structure 16 arranged in a cylindrical shape. The filter outer cylinder 11 includes an upper port 111 and a lower port 112 that are connected from top to bottom, and a cavity that is connected to the upper opening 121 and the lower opening 131 respectively; the upper cover body 12 is covered on the upper port 111; the lower cover body 13 is covered on the lower port 112, the upper cover body 12 is provided with an upper opening 121; the lower cover body 13 is provided with a lower opening 131; the upper sealing body 14 and the lower sealing body 15 are detachably arranged in the cavity, the upper sealing body 14 is provided with a first through hole 141, the lower sealing body 15 is provided with a second through hole 151, the second through hole 151 is connected to the lower opening 131, and the first through hole 14 1 is communicated with the upper opening 121; the upper end of the filter membrane structure 16 is sealed on the upper sealing body 14, and the lower end is sealed on the lower sealing body 15, a first cavity is formed between the filter membrane structure 16 and the filter outer cylinder 11, the first cavity is communicated with the first through hole 141, and the lower end of the filter membrane is communicated with the second through hole 151; wherein the mixed solution enters from the upper opening 121, enters into the first cavity through the first through hole 141, and the liquid filtered by the filter membrane structure 16 enters the filter membrane structure 16, and flows out from the lower opening 131 through the second through hole 151.

[0086] In specific operation, the mixed solution is poured into the upper opening 121, and the mixed solution enters the first cavity through the first through hole 141 of the upper sealing body 14, and the liquid filtered by the filter membrane structure 16 enters the filter membrane structure 16, and flows out from the lower opening 131 through the second through hole 151. The platinum yellow is retained in the first cavity, and after the complete filtration is completed, the upper cover body 12, the lower cover body 13, the upper sealing body 14 and the lower sealing body 15 can be taken out to obtain the platinum yellow.

[0087] To facilitate rapid filtration, in some feasible implementations, an inert gas at a certain pressure may be delivered to the upper opening 121 to promote rapid filtration. Alternatively, a rotating drive device, such as a rotating motor, may be installed on the lower cover 13 so that the filter device 1 rotates as a whole, thereby accelerating filtration.

[0088] The present invention also provides a sealing detection method for the above-mentioned recovery device, comprising step S1000 and step S2000.

[0089] In step S1000, a detection substance is applied to the inner wall of the recovery device. The detection substance includes, by mass:

[0090] Anhydrous ammonium chloride powder: 2-2.5 parts;

[0091] Phenolphthalein for acid-base indication: 1-3 parts;

[0092] Macroporous adsorption resin: 2-3 parts;

[0093] Solvent: 16-19 parts.

[0094] Macroporous adsorption resin is a type of polymer adsorption resin that does not contain exchange groups and has a macroporous structure. It has a good macroporous network structure and a large specific surface area. It can selectively physically adsorb organic matter in aqueous solutions. It is a new type of organic polymer adsorbent developed in the 1960s and has been widely used in environmental protection, food, medicine and other fields.

[0095] The manufacturing method of the detection substance comprises the following steps: firstly, the phenolphthalein and the anhydrous ammonium chloride powder are uniformly mixed to obtain a first mixture; and then the first mixture is mixed with a macroporous adsorption resin and a solvent to form a color-changing solution.

[0096] When in use, the inner wall of the recovery device can be coated with the test substance; after drying, the sealing test can be performed. In this way, the test substance can be evenly spread to every corner to be tested, and the test is more precise and convenient. The test substance will not spread when it comes into contact with water, and the specific location where the leak occurs can be accurately determined.

[0097] After the charged phenolphthalein is mixed with the anhydrous ammonium chloride powder, the charged phenolphthalein first chelates with the anhydrous ammonium chloride to form a charged macromolecule; after mixing with the macroporous adsorption resin, the charged macromolecule is adsorbed by the macroporous adsorption resin, and the adsorption force at this time is the intermolecular force and the coordination bond force. Since this adsorption force is very strong and will not be separated by external moisture interference, even if it is not completely dried during use, it will not cause the phenolphthalein to develop color and become ineffective. When external moisture enters the color-changing substance, the macroporous adsorption resin fixes the phenolphthalein and absorbs moisture, so that it can develop color when it encounters water and will not diffuse.

[0098] In other embodiments, the anhydrous ammonium chloride powder may be replaced with anhydrous copper sulfate powder. In this way, the anhydrous copper sulfate powder can also show color when it comes into contact with water, which can further improve the color development effect.

[0099] In step S2000, the recovery device is immersed in water, and when the detection substance changes color, it is determined that the recovery device is leaking.

[0100] Specifically, the color-changing solution is brushed on the inner wall of the recovery device, and after drying, a sealing test can be performed.

[0101] In other feasible solutions, the recovery device can also be immersed in a container filled with water, and a certain pressure can be added to the container to promote detection efficiency.

[0102] Obviously, the embodiments described above are only some embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, ordinary technicians in this field can make other different forms of changes or modifications without creative work, which should fall within the scope of protection of the present invention.

Claims

1. A method for recovering platinum from a platinum solution, wherein the platinum content in the platinum solution is less than 1.32 g / L and the pH value is 10- 10.5, characterized in that it includes: Adding hydrochloric acid to the platinum solution to adjust the pH value of the solution to a first preset value, wherein the first preset value is 0.5-1, to obtain a first solution; Slowly add hydrogen peroxide to the first solution and stir for a first preset time to obtain a second solution, wherein the first preset time is 30 min-40 min; After adding ammonium chloride to the second solution, platinum yellow is precipitated, and the amount of ammonium chloride added is 3.1-3.5 times the platinum content; The precipitated platinum yellow is calcined to obtain finished platinum.

2. The method for recovering platinum from platinum liquid according to claim 1, characterized in that: In the step of slowly adding hydrogen peroxide to the first solution and stirring for a first preset time to obtain the second solution, Pt 2+ →Pt 4+ .

3. The method for recovering platinum from platinum liquid according to claim 1, characterized in that: In the step of adding ammonium chloride to the second solution to precipitate platinum yellow, Pt 4+ +NH4Cl→PtCl4.

4. The method for recovering platinum from platinum liquid according to claim 1, characterized in that: The step of calcining the precipitated platinum yellow to obtain finished platinum comprises: The precipitated platinum yellow is calcined at a first preset temperature to obtain finished platinum, wherein the first preset temperature is 600°C-650°C.

5. The method for recovering platinum from platinum liquid according to claim 1, characterized in that: After the step of adding ammonium chloride to the second solution to precipitate platinum yellow and before the step of calcining the precipitated platinum yellow to obtain finished platinum, the recovery method further comprises: The precipitated platinum yellow was filtered and washed out.

6. The method for recovering platinum from platinum liquid according to claim 1, characterized in that: The step of adding hydrochloric acid to the platinum solution to adjust the pH value of the solution to a first preset value comprises: The platinum solution is placed in a reaction kettle, and industrial-grade hydrochloric acid is slowly added into the reaction kettle to adjust the pH value of the solution to 1.

7. A recovery device for the method for recovering platinum in platinum liquid according to any one of claims 1 to 6, characterized in that: include: A reaction kettle, used for reacting platinum in the platinum liquid to generate a mixed solution containing platinum yellow; The filtering device is arranged downstream of the reaction kettle and is used for filtering the platinum yellow from the mixed solution.

8. The recovery device according to claim 7, characterized in that: The filtering device comprises: The filter outer cylinder comprises an upper port and a lower port which are connected vertically and a cavity which is connected to the upper port and the lower port respectively; An upper cover body, which covers the upper port and has an upper opening; A lower cover body, which is arranged on the lower port, and the lower cover body is penetrated by a lower opening; An upper sealing body and a lower sealing body are detachably disposed in the cavity, the upper sealing body is penetrated by a first through hole, the lower sealing body is penetrated by a second through hole, the second through hole is communicated with the lower opening, and the first through hole is communicated with the upper opening; A filter membrane structure provided in a cylindrical body, wherein the upper end of the filter membrane structure is sealed on the upper sealing body, and the lower end is sealed on the lower sealing body, a first cavity is formed between the filter membrane structure and the filter outer cylinder, the first cavity is communicated with the first through hole, and the lower end of the filter membrane is communicated with the second through hole; The mixed solution enters from the upper opening, enters the first cavity through the first through hole, and the liquid filtered by the filter membrane structure enters the filter membrane structure and flows out from the lower opening through the second through hole.

9. A sealing detection method for a recovery device as claimed in claim 7 or 8, characterized in that: include: Applying a detection substance to the inner wall of the recovery device; Immersing the recovery device in water, and when the detection substance changes color, it is determined that the recovery device is leaking; Wherein, the test substances include, by mass: Anhydrous ammonium chloride powder: 2-2.5 parts; Phenolphthalein for acid-base indication: 1-3 parts; Macroporous adsorption resin: 2-3 parts; Solvent: 16-19 parts.

10. The sealing detection method according to claim 9, characterized in that: Before the step of applying the detection substance to the inner wall of the recovery device, the method comprises: First, the phenolphthalein and the anhydrous ammonium chloride powder are uniformly mixed to obtain a first mixture; then the first mixture is mixed with a macroporous adsorption resin and a solvent to form a color-changing solution; Correspondingly, the step of applying the detection substance to the inner wall of the recovery device comprises: Brush the color-changing solution on the inner wall of the recovery device, and then carry out the sealing test after it dries.

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