阅读说明：本技术 一种从废料回收铂金的方法 (Method for recovering platinum from waste ) 是由 陈平华 于 2021-08-20 设计创作，主要内容包括：本发明提供了一种从废料回收铂金的方法,包括以下步骤：步骤一：废料的溶解：步骤二：铂的降沉：步骤三：激活化处理：步骤四：二次降沉处理：步骤五：养护处理。本发明铂金回收中,先采用废料的溶解处理,然后再进行铂的降沉,通过氯化铵溶液的降沉处理,可首先提取出铂金,从而提高铂金的提取率；而在铂金通过改性黏土进行改进处理,改性粘土首先采用氯化铁处理,提高其表面孔隙度,然后再进行煅烧炉变温处理,粘土的活性增强,通过粘土与铂金复合,从而起到承载的效果,目的在质子辐照箱内辐照处理、等离子处理中,提高铂金的活化效率,最后再进行二次的降沉中,可极大程度的提高铂金的提纯效果。(The invention provides a method for recovering platinum from waste materials, which comprises the following steps: the method comprises the following steps: dissolution of waste materials: step two: precipitation of platinum: step three: activation treatment: step four: secondary sedimentation treatment: step five: and (5) maintaining. In the platinum recovery, the waste is dissolved firstly, then the platinum is precipitated, and the platinum can be extracted firstly through the precipitation treatment of the ammonium chloride solution, so that the extraction rate of the platinum is improved; the platinum is improved by modified clay, the modified clay is firstly treated by ferric chloride to improve the surface porosity of the modified clay, then the temperature change treatment of a calcining furnace is carried out, the activity of the clay is enhanced, and the clay and the platinum are compounded to play a bearing effect, so that the activation efficiency of the platinum is improved in the irradiation treatment and the plasma treatment in a proton irradiation box, and finally the purification effect of the platinum can be greatly improved in the secondary sedimentation.)

1. A method of recovering platinum from waste material, comprising the steps of:

the method comprises the following steps: dissolution of waste materials:

mixing the noble metal waste with aqua regia according to the weight ratio of 8:1, then stirring and dissolving in a reaction kettle at the temperature of 80-120 ℃, the dissolving time of 30-40min and the stirring speed of 600r/min, and completely dissolving the waste after stirring;

step two: precipitation of platinum:

adding 30-40% by mass of ammonium chloride solution into the dissolved material obtained in the first step, stirring at a rotating speed of 100-300r/min for 10-20min, standing for precipitation to obtain ammonium chloroplatinate, and finally washing with solution to obtain precipitated platinum material;

step three: activation treatment:

s1: sending the precipitated platinum material and the modified clay into deionized water for ultrasonic dispersion for 20-30min, wherein the ultrasonic power is 100-200W, and obtaining the material to be activated after the ultrasonic treatment;

s2: sending the material to be activated into a proton irradiation box for irradiation treatment, and finally performing plasma treatment to obtain an activated material;

s3: the activation material is sent into a centrifuge for centrifugation, and then is washed, filtered and dried to obtain pure platinum activation material;

step four: secondary sedimentation treatment:

sending the pure platinum activating material into aqua regia for secondary dissolution, then adding an oxidant solution, then adding an ammonium chloride solution for precipitation treatment, and finally washing with the ammonium chloride solution;

step five: and (3) maintenance treatment:

and feeding the platinum material subjected to the secondary sedimentation treatment into a drying box for curing for 10-30min to obtain the platinum of the invention.

2. The method for recovering platinum from waste materials according to claim 1, wherein the modified clay in the third step is prepared by the following steps: and (2) feeding the clay into ferric chloride with the mass fraction of 10-30%, stirring for 20-30min at the stirring speed of 400-800W, finishing stirring, then feeding into a calcining furnace for continuous temperature change treatment, finally feeding into deionized water with the temperature of-5 ℃ for high-speed stirring treatment, finishing stirring, washing with water, and drying to obtain the modified clay.

3. The method for recovering platinum from waste materials as claimed in claim 2, wherein the continuous temperature-changing treatment is carried out by the following specific operation method: the reaction temperature is increased to 300 ℃ at the speed of 1-3 ℃/min, then the temperature is preserved for 10-20min, then the temperature is directly increased to 600 ℃ at the speed of 5 ℃/min, and then the temperature is immediately decreased to 150 ℃ and 200 ℃ at the speed of 3 ℃/min for standby.

4. The method for recovering platinum from waste material as claimed in claim 2, wherein the stirring speed of the high speed stirring process is 1000-1500r/min, and the stirring time is 20-30 min.

5. The method for recovering platinum from waste materials as claimed in claim 1, wherein the irradiation power in the proton irradiation box is 100-.

6. The method for recovering platinum from waste materials according to claim 5, wherein the secondary activation treatment is performed by placing the waste materials in 10-20% sodium dodecyl sulfate solution for standing for 20-30min at 65-75 ℃, and after standing, washing and drying the waste materials.

7. The method as claimed in claim 1, wherein the plasma power of the plasma treatment is 100-600W, and the plasma treatment time is 10-30 min.

8. The method for recovering platinum from waste material according to claim 7, wherein the plasma power is 350W, and the plasma treatment time is 20 min.

9. The method for recycling platinum from waste materials according to claim 1, wherein the oxidant solution is formed by mixing hydrogen peroxide and sodium sulfate according to a weight ratio of 3: 1.

10. The method for recovering platinum from waste material according to claim 1, wherein the curing temperature is 45-55 ℃ and the curing time is 10-30 min.

Technical Field

The invention relates to the technical field of platinum recovery, in particular to a method for recovering platinum from waste materials.

Background

The noble metal mainly refers to 8 metal elements such as gold, silver and platinum group metals (ruthenium, rhodium, palladium, osmium, iridium, platinum). Most of these metals have beautiful colors, are considerably resistant to chemicals, and are not easily chemically reacted under general conditions. The rare earth is not a single metal but an alloy of some rare metals. Since dilute gold has some characteristics comparable to gold, such as color like gold, chemical stability like gold and similar mechanical properties. The jewelry made of the rare gold can almost reach the level of being in a spurious way with gold jewelry; platinum is platinum. Is a precious metal, and compared with gold and silver, the time for manufacturing the jewelry is later. Platinum has bright white color, excellent ductility and wear and acid resistance.

The existing platinum recovery process for waste materials is relatively conventional, the recovery rate of platinum is difficult to improve, the recovery efficiency is influenced, and further improvement treatment is needed on the basis.

Disclosure of Invention

In view of the drawbacks of the prior art, it is an object of the present invention to provide a method for recovering platinum from scrap.

The technical scheme adopted by the invention for solving the technical problems is as follows:

the invention provides a method for recovering platinum from waste materials, which comprises the following steps:

the method comprises the following steps: dissolution of waste materials:

mixing the noble metal waste with aqua regia according to the weight ratio of 8:1, then stirring and dissolving in a reaction kettle at the temperature of 80-120 ℃, the dissolving time of 30-40min and the stirring speed of 600r/min, and completely dissolving the waste after stirring;

step two: precipitation of platinum:

adding 30-40% by mass of ammonium chloride solution into the dissolved material obtained in the first step, stirring at a rotating speed of 100-300r/min for 10-20min, standing for precipitation to obtain ammonium chloroplatinate, and finally washing with solution to obtain precipitated platinum material;

step three: activation treatment:

s1: sending the precipitated platinum material and the modified clay into deionized water for ultrasonic dispersion for 20-30min, wherein the ultrasonic power is 100-200W, and obtaining the material to be activated after the ultrasonic treatment;

s2: sending the material to be activated into a proton irradiation box for irradiation treatment, and finally performing plasma treatment to obtain an activated material;

s3: the activation material is sent into a centrifuge for centrifugation, and then is washed, filtered and dried to obtain pure platinum activation material;

step four: secondary sedimentation treatment:

sending the pure platinum activating material into aqua regia for secondary dissolution, then adding an oxidant solution, then adding an ammonium chloride solution for precipitation treatment, and finally washing with the ammonium chloride solution;

step five: and (3) maintenance treatment:

and feeding the platinum material subjected to the secondary sedimentation treatment into a drying box for curing for 10-30min to obtain the platinum of the invention.

Preferably, the preparation method of the modified clay in the third step is as follows: and (2) feeding the clay into ferric chloride with the mass fraction of 10-30%, stirring for 20-30min at the stirring speed of 400-800W, finishing stirring, then feeding into a calcining furnace for continuous temperature change treatment, finally feeding into deionized water with the temperature of-5 ℃ for high-speed stirring treatment, finishing stirring, washing with water, and drying to obtain the modified clay.

Preferably, the specific operation method of the continuous variable temperature treatment is as follows: the reaction temperature is increased to 300 ℃ at the speed of 1-3 ℃/min, then the temperature is preserved for 10-20min, then the temperature is directly increased to 600 ℃ at the speed of 5 ℃/min, and then the temperature is immediately decreased to 150 ℃ and 200 ℃ at the speed of 3 ℃/min for standby.

Preferably, the stirring speed of the high-speed stirring treatment is 1000-1500r/min, and the stirring time is 20-30 min.

Preferably, the irradiation power in the irradiation treatment in the proton irradiation box is 100-.

Preferably, the secondary activation treatment is carried out by placing the mixture into 10-20% sodium dodecyl sulfate solution for standing for 20-30min at 65-75 ℃, washing with water and drying.

Preferably, the plasma power of the plasma treatment is 100-600W, and the plasma treatment time is 10-30 min.

Preferably, the plasma power is 350W, and the plasma treatment time is 20 min.

Preferably, the oxidant solution is prepared by mixing hydrogen peroxide and sodium sulfate according to the weight ratio of 3: 1.

Preferably, the curing temperature is 45-55 ℃, and the curing time is 10-30 min.

Compared with the prior art, the invention has the following beneficial effects:

(1) in the platinum recovery, the waste is dissolved firstly, then the platinum is precipitated, and the platinum can be extracted firstly through the precipitation treatment of the ammonium chloride solution, so that the extraction rate of the platinum is improved.

(2) The platinum is improved by modified clay, the modified clay is firstly treated by ferric chloride to improve the surface porosity of the modified clay, then the temperature change treatment of a calcining furnace is carried out, the activity of the clay is enhanced, and the clay and the platinum are compounded to play a bearing effect, so that the activation efficiency of the platinum is improved in the irradiation treatment and the plasma treatment in a proton irradiation box, and finally the purification effect of the platinum can be greatly improved in the secondary sedimentation.

Drawings

FIG. 1 is a schematic flow diagram of the present invention;

fig. 2 is a schematic view of a process for preparing modified clay according to the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, 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.

Example 1.

The method for recovering platinum from the waste comprises the following steps:

the method comprises the following steps: dissolution of waste materials:

mixing the noble metal waste with aqua regia according to the weight ratio of 8:1, then stirring and dissolving in a reaction kettle at the stirring and dissolving temperature of 80 ℃, the dissolving time of 30min and the stirring speed of 100r/min, and completely dissolving the waste after stirring;

step two: precipitation of platinum:

adding an ammonium chloride solution with the mass fraction of 30% into the dissolved material obtained in the first step, stirring at the rotating speed of 100r/min for 10min, standing for precipitation to obtain ammonium chloroplatinate, and finally washing with the solution to obtain a precipitation platinum material;

step three: activation treatment:

s1: sending the precipitated platinum material and the modified clay into deionized water for ultrasonic dispersion for 20min, wherein the ultrasonic power is 100W, and obtaining a material to be activated after ultrasonic treatment;

s2: sending the material to be activated into a proton irradiation box for irradiation treatment, and finally performing plasma treatment to obtain an activated material;

s3: the activation material is sent into a centrifuge for centrifugation, and then is washed, filtered and dried to obtain pure platinum activation material;

step four: secondary sedimentation treatment:

sending the pure platinum activating material into aqua regia for secondary dissolution, then adding an oxidant solution, then adding an ammonium chloride solution for precipitation treatment, and finally washing with the ammonium chloride solution;

step five: and (3) maintenance treatment:

and feeding the platinum material subjected to the secondary sedimentation treatment into a drying box for curing for 10min to obtain the platinum of the invention.

The preparation method of the modified clay in step three of this example is as follows: and (2) feeding the clay into ferric chloride with the mass fraction of 10%, stirring for 20min at the stirring speed of 400W, finishing stirring, then feeding into a calcining furnace for continuous temperature change treatment, finally feeding into deionized water with the temperature of-5 ℃ for high-speed stirring treatment, finishing stirring, washing with water, and drying to obtain the modified clay.

The specific operation method of the continuous variable temperature treatment in this embodiment is as follows: the reaction temperature is increased to 300 ℃ at the speed of 1 ℃/min, then the temperature is preserved for 10min, then the temperature is directly increased to 600 ℃ at the speed of 5 ℃/min, and then the temperature is immediately reduced to 150 ℃ at the speed of 3 ℃/min for standby.

The stirring speed of the high-speed stirring treatment in this embodiment is 1000-1500r/min, and the stirring time is 20-30 min.

In the irradiation treatment in the proton irradiation box of this embodiment, the irradiation power is 100W, the irradiation time is 10min, the irradiation is completed, and then the secondary activation treatment is performed.

In the second activation treatment of this example, the mixture was first placed in a 10% sodium dodecyl sulfate solution and allowed to stand for 20 inches at a temperature of 65 ℃, and the mixture was washed with water and dried.

The plasma power of the plasma treatment in this example was 100W, and the plasma treatment time was 10 min.

The oxidant solution of the embodiment is prepared by mixing hydrogen peroxide and sodium sulfate according to the weight ratio of 3: 1.

The curing temperature in this example was 45 ℃ and the curing time was 10 min.

Example 2.

The method for recovering platinum from the waste comprises the following steps:

the method comprises the following steps: dissolution of waste materials:

mixing the noble metal waste with aqua regia according to the weight ratio of 8:1, then stirring and dissolving in a reaction kettle at the stirring and dissolving temperature of 120 ℃, the dissolving time of 40min and the stirring speed of 600r/min, and completely dissolving the waste after stirring;

step two: precipitation of platinum:

adding an ammonium chloride solution with the mass fraction of 40% into the dissolved material obtained in the first step, stirring at the rotating speed of 300r/min for 20min, standing for precipitation to obtain ammonium chloroplatinate, and finally washing with the solution to obtain a precipitation platinum material;

step three: activation treatment:

s1: sending the precipitated platinum material and the modified clay into deionized water for ultrasonic dispersion for 30min, wherein the ultrasonic power is 200W, and obtaining a material to be activated after ultrasonic treatment;

s2: sending the material to be activated into a proton irradiation box for irradiation treatment, and finally performing plasma treatment to obtain an activated material;

s3: the activation material is sent into a centrifuge for centrifugation, and then is washed, filtered and dried to obtain pure platinum activation material;

step four: secondary sedimentation treatment:

sending the pure platinum activating material into aqua regia for secondary dissolution, then adding an oxidant solution, then adding an ammonium chloride solution for precipitation treatment, and finally washing with the ammonium chloride solution;

step five: and (3) maintenance treatment:

and (4) feeding the platinum material subjected to the secondary sedimentation treatment into a drying box for curing for 30min to obtain the platinum of the invention.

The preparation method of the modified clay in step three of this example is as follows: and (2) feeding the clay into ferric chloride with the mass fraction of 30%, stirring for 30min at the stirring speed of 800W, finishing stirring, then feeding into a calcining furnace for continuous temperature change treatment, finally feeding into deionized water with the temperature of-5 ℃ for high-speed stirring treatment, finishing stirring, washing with water, and drying to obtain the modified clay.

The specific operation method of the continuous variable temperature treatment in this embodiment is as follows: the reaction temperature is increased to 300 ℃ at the speed of 1-3 ℃/min, then the temperature is preserved for 20min, then the reaction temperature is directly increased to 600 ℃ at the speed of 5 ℃/min, and then the reaction temperature is immediately reduced to 200 ℃ at the speed of 3 ℃/min for standby.

In this example, the stirring speed of the high-speed stirring treatment was 1500r/min, and the stirring time was 30 min.

In the irradiation treatment in the proton irradiation box of the embodiment, the irradiation power is 200W, the irradiation time is 20min, the irradiation is finished, and then the secondary activation treatment is performed.

In the second activation treatment of the embodiment, the mixture is placed in a 10-20% sodium dodecyl sulfate solution and stands for 30min at a temperature of 75 ℃, and the mixture is washed and dried after the standing is finished.

The plasma power of the plasma treatment in this example was 600W, and the plasma treatment time was 30 min.

The oxidant solution of the embodiment is prepared by mixing hydrogen peroxide and sodium sulfate according to the weight ratio of 3: 1.

The curing temperature in this example was 55 ℃ and the curing time was 30 min.

Example 3.

The method for recovering platinum from the waste comprises the following steps:

the method comprises the following steps: dissolution of waste materials:

mixing the noble metal waste with aqua regia according to the weight ratio of 8:1, then stirring and dissolving in a reaction kettle at the stirring and dissolving temperature of 100 ℃, the dissolving time of 35min and the stirring speed of 300r/min, and completely dissolving the waste after stirring;

step two: precipitation of platinum:

adding an ammonium chloride solution with the mass fraction of 35% into the dissolved material obtained in the first step, stirring at the rotating speed of 200r/min for 15min, standing for precipitation to obtain ammonium chloroplatinate, and finally washing with the solution to obtain a precipitation platinum material;

step three: activation treatment:

s1: sending the precipitated platinum material and the modified clay into deionized water for ultrasonic dispersion for 25min, wherein the ultrasonic power is 150W, and obtaining a material to be activated after ultrasonic treatment;

s2: sending the material to be activated into a proton irradiation box for irradiation treatment, and finally performing plasma treatment to obtain an activated material;

s3: the activation material is sent into a centrifuge for centrifugation, and then is washed, filtered and dried to obtain pure platinum activation material;

step four: secondary sedimentation treatment:

sending the pure platinum activating material into aqua regia for secondary dissolution, then adding an oxidant solution, then adding an ammonium chloride solution for precipitation treatment, and finally washing with the ammonium chloride solution;

step five: and (3) maintenance treatment:

and feeding the platinum material subjected to the secondary sedimentation treatment into a drying box for curing for 20min to obtain the platinum of the invention.

The preparation method of the modified clay in step three of this example is as follows: and (2) feeding the clay into 20 mass percent ferric chloride, stirring for 25min at the stirring speed of 600W, then feeding the clay into a calcining furnace for continuous temperature change treatment, finally feeding the clay into deionized water at the temperature of-5 ℃ for high-speed stirring treatment, and after stirring, washing and drying to obtain the modified clay.

The specific operation method of the continuous variable temperature treatment in this embodiment is as follows: the reaction temperature is increased to 300 ℃ at the speed of 2 ℃/min, then the temperature is preserved for 15min, then the temperature is directly increased to 600 ℃ at the speed of 5 ℃/min, and then the temperature is immediately reduced to 175 ℃ at the speed of 3 ℃/min for standby.

In this example, the stirring speed of the high-speed stirring treatment was 1250r/min, and the stirring time was 25 min.

In the irradiation treatment in the proton irradiation box of the embodiment, the irradiation power is 150W, the irradiation time is 15min, the irradiation is finished, and then the secondary activation treatment is performed.

In the second activation treatment of this example, the mixture was first placed in a 15% sodium dodecyl sulfate solution and allowed to stand for 25min at a temperature of 70 ℃, and the mixture was washed with water and dried.

The plasma power of this example was 350W, and the plasma treatment time was 20 min.

The oxidant solution of the embodiment is prepared by mixing hydrogen peroxide and sodium sulfate according to the weight ratio of 3: 1.

The curing temperature in this example was 50 ℃ and the curing time was 20 min.

Comparative example 1.

The only difference from example 3 is that no activation treatment was used.

Comparative example 2.

The only difference from example 3 is that no modified clay treatment was used in the activation treatment.

The properties of examples 1-3 and comparative examples 1-2 were tested as follows:

group of	Extraction ratio of platinum (%)	Purification ratio of platinum (%)
			Example 1	98.7	88.9
Example 2	99.1	89.1
			Example 3	99.3	89.9
Comparative example 1	93.2	82.1
			Comparative example 2	94.3	84.3

As can be seen from examples 1-3 and comparative examples 1-2, the extraction rate of the platinum of the invention can reach 99.3% at most, the purification rate of the platinum reaches 89.9%, and the recovery rate of the platinum is obviously improved compared with the prior art.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.