Disclosure of Invention
The invention provides a method for recovering platinum from platinum-containing organic silicon wastewater, which is simple, low in recovery cost and high in platinum recovery rate.
The technical scheme of the invention is realized as follows:
a method for recovering platinum from platinum-containing organosilicon wastewater comprises the following steps:
1) adding platinum-containing organic silicon wastewater into water in a dropwise manner for hydrolysis, and filtering to obtain acid water and hydrolysis filter residues;
2) washing the hydrolysis filter residue obtained in the step 1) with water, adjusting the pH value to be neutral, and filtering and drying to obtain washing filter residue;
3) adding the dried water-washed filter residue obtained in the step 2) into a muffle furnace, introducing air, and carrying out temperature programming roasting to obtain incineration ash;
4) adding the incineration ash obtained in the step 3) into formic acid, boiling, reducing and filtering to obtain reduced filter residue;
5) adding the reduced filter residue into the acid water obtained in the step 1), heating to slightly reflux, and adding a strong oxidant to leach out the platinum.
2. The method for recovering platinum from the platinum-containing organosilicon wastewater as claimed in claim 1, wherein in the step 1), the mass ratio of the platinum-containing organosilicon wastewater to water is 1: 3.
further, in step 3), the procedure of temperature programming is to maintain at 200 ℃ for 1h, to maintain at 250 ℃ for 1h, to maintain at 300 ℃ for 1h, to maintain at 350 ℃ for 2h, to maintain at 400 ℃ for 2h, and to maintain at 600 ℃ for 2 h.
Further, in the step 3), the temperature for burning by introducing air is 600 ℃ and the time is 2 hours.
Further, in the step 4), the addition amount of formic acid is 1.6 times of the mass of the incineration ash, and the reduction time of formic acid digestion is 2 hours.
Further, in the step 5), the strong oxidant is chlorine, and the mass ratio of the added chlorine to the reduced filter residue is 1: 3.
The invention provides a method for recovering platinum from platinum-containing organic silicon wastewater, which has the following advantages:
1) acid water generated by the hydrolysis of the platinum-containing waste is recycled to the oxidation leaching step, so that waste acid generated by hydrolysis is effectively utilized, and new acid is not used in the oxidation leaching step, and the generation of waste acid is reduced;
2) the washing filter residue is roasted by adopting programmed heating, so that the platinum loss caused by a large amount of smoke generated in the rapid heating process can be avoided, and the recovery rate of platinum can be improved;
3) the method is simple, the recovery cost is low, and the recovery rate of the platinum is high.
Detailed Description
The invention provides a method for recovering platinum from platinum-containing organic silicon wastewater, which comprises the following steps:
1) adding platinum-containing organic silicon wastewater into water in a dropwise manner for hydrolysis, and filtering to obtain acid water and hydrolysis filter residues;
2) washing the hydrolysis filter residue obtained in the step 1) with water, adjusting the pH value to be neutral, and filtering and drying to obtain washing filter residue;
3) adding the dried water-washed filter residue obtained in the step 2) into a muffle furnace, introducing air, and carrying out temperature programming roasting to obtain incineration ash;
4) adding the incineration ash obtained in the step 3) into formic acid, boiling, reducing and filtering to obtain reduced filter residue;
5) adding the reduced filter residue into the acid water obtained in the step 1), heating to slightly reflux, and adding a strong oxidant to leach out the platinum.
Dropwise adding the platinum-containing organic silicon wastewater into water for hydrolysis, and filtering to obtain acid water and hydrolysis filter residues; wherein the mass ratio of the platinum-containing organic silicon wastewater to water is 1: 3.
and washing the obtained hydrolysis filter residue with water, adjusting the pH value to be neutral, filtering and drying to obtain the washing filter residue. It should be noted that the hydrolysis filter residue is acidic, and an alkaline substance is needed when adjusting the pH value, and the alkaline substance may be sodium hydroxide, sodium bicarbonate, sodium carbonate, or the like.
And drying the water-washed filter residue, adding the dried filter residue into a muffle furnace, introducing air, and roasting at a programmed temperature to obtain incineration ash. The procedure of the temperature programming includes maintaining at 200 ℃ for 1 hour, raising to 250 ℃ for 1 hour, raising to 300 ℃ for 1 hour, raising to 350 ℃ for 2 hours, raising to 400 ℃ for 2 hours, and raising to 600 ℃ for 2 hours. The platinum loss caused by a large amount of smoke generated in the rapid heating process can be avoided by adopting the programmed heating, so that the yield of the platinum is reduced.
The temperature of the air-introduced incineration was 600 ℃ and the time was 2 hours.
Adding the incineration ash into formic acid, boiling, reducing and filtering to obtain reduced filter residue; the addition amount of the formic acid is 1.6 times of the mass of the incineration ash, and the reduction time of formic acid digestion is 2 hours.
And adding the reduced filter residue into acid water, heating to slightly reflux, and adding a strong oxidant to leach out the platinum. The strong oxidant is chlorine, and the mass ratio of the added chlorine to the reduced filter residue is 1: 3.
The acidic water obtained by hydrolyzing the platinum-containing organic silicon wastewater is used for oxidation leaching, so that the waste acid generated by hydrolysis is effectively utilized, and new acid is not used in the oxidation leaching step, so that the generation of waste acid is reduced.
According to the invention, acid water generated by platinum-containing waste hydrolysis is applied to the oxidation leaching step, so that waste acid generated by hydrolysis is effectively utilized, and new acid is not used in the oxidation leaching step, thereby reducing the generation of waste acid; the washing filter residue is roasted by adopting temperature programming, so that the platinum loss caused by a large amount of smoke generated in the rapid heating process can be avoided, and the recovery rate of platinum can be improved.
In order to further illustrate the present invention, the following will describe the method for recovering platinum from platinum-containing organosilicon wastewater in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
The platinum content in the platinum-containing silicone wastewater used in examples 1 to 3 and comparative examples 1 to 3 was 0.02% by mass.
Example 1
1) Dripping 200.00g of platinum-containing organic silicon wastewater into 600.00g of water for hydrolysis, and filtering to obtain 504.55g of acid water and 295.45g of hydrolysis filter residue;
2) 295.45g of hydrolysis filter residue obtained in the step 1) is added into 300.00g of water for washing, alkali liquor is added to adjust the pH value to be neutral, and the filter residue is filtered and dried to obtain washing filter residue;
3) adding the water-washed filter residue dried in the step 3) into a muffle furnace, introducing air, and roasting at a programmed temperature, wherein the programmed temperature flow is as follows: keeping the temperature at 200 ℃ for 1h, raising the temperature to 250 ℃ for 1h, raising the temperature to 300 ℃ for 1h, raising the temperature to 350 ℃ for 2h, raising the temperature to 400 ℃ for 2h, raising the temperature to 600 ℃ for 2h, and introducing air to the temperature of 600 ℃ for 2h to obtain 62.50g of incineration ash;
4) adding 62.50g of incineration ash obtained in the step 3) into 100g of formic acid, boiling and reducing for 2h, and filtering to obtain 100.30g of waste formic acid and 60.00g of reduced filter residue;
5) adding 60.00g of reduced filter residue obtained in the step 4) into 504.55g of acid water obtained in the step 1), heating to slightly reflux, introducing 20.00g of chlorine, cooling and filtering to obtain 501.23g of platinum-containing filtrate.
The platinum content was determined to be 76.08ppm, and the platinum yield was 95.34%.
Comparative example 1
1) Dripping 200.00g platinum-containing organic silicon wastewater into 600.00g water for hydrolysis, and filtering to obtain 501.75g acid water and 298.68g hydrolysis filter residue;
2) adding 298.68g of hydrolysis filter residue obtained in the step 2) into 300.00g of water for washing, adding alkali liquor to adjust the pH value to be neutral, filtering and drying to obtain washing filter residue;
3) adding the water-washed filter residue dried in the step 3) into a muffle furnace, heating to 600 ℃, keeping for 2h, introducing air, keeping for 2h at 600 ℃, and obtaining 60.30g of incineration ash;
4) adding 100g of formic acid into the incineration ash obtained in the step 3), boiling and reducing for 2 hours, and filtering to obtain 101.30g of waste formic acid and 58.45g of reduced filter residue;
5) 58.45g of reduced filter residue obtained in the step 4) is added into 501.75g of acid water obtained in the step 1) and heated to be slightly refluxed, 20.00g of chlorine is introduced, and the temperature is reduced and the filtration is carried out, so that 500.80g of platinum-containing filtrate is obtained.
The platinum content was found to be 72.08ppm, and the platinum yield was 90.25%.
Example 2
1) Dripping 200.00g platinum-containing organic silicon wastewater into 600.00g water for hydrolysis, and filtering to obtain 503.90g acid water and 297.65g hydrolysis filter residue;
2) adding 297.65g of hydrolysis filter residue obtained in the step 1) into 300.00g of water for washing, adding alkali liquor to adjust the pH value to be neutral, filtering and drying to obtain washing filter residue;
3) adding the water-washed filter residue dried in the step 2) into a muffle furnace, introducing air, and roasting by programmed heating, wherein the programmed heating process is as follows: keeping the temperature at 200 ℃ for 1h, raising the temperature to 250 ℃ for 1h, raising the temperature to 300 ℃ for 1h, raising the temperature to 350 ℃ for 2h, raising the temperature to 400 ℃ for 2h, raising the temperature to 600 ℃ for 2h, and introducing air to the temperature of 600 ℃ for 2h to obtain 61.50g of incineration ash;
4) adding 61.50g of incineration ash obtained in the step 3) into 100g of formic acid, boiling and reducing for 2h, and filtering to obtain 100.87g of waste formic acid and 61.56g of reduced filter residue;
5) 61.56g of reduced filter residue obtained in the step 4) is added into 503.90g of acid water obtained in the step 1) and heated to be slightly refluxed, 20.00g of chlorine is introduced, and the temperature is reduced and the filtration is carried out, so that 499.00g of platinum-containing filtrate is obtained.
The platinum content was found to be 76.27ppm, and the platinum yield was 95.15%.
Comparative example 2
1) Dripping 200.00g platinum-containing organic silicon wastewater into 600.00g water for hydrolysis, and filtering to obtain 502.90g acid water and 296.75g hydrolysis filter residue;
2) adding 296.75g of hydrolysis filter residue obtained in the step 1) into 300.00g of water for washing, adding alkali liquor to adjust the pH value to be neutral, filtering and drying to obtain washing filter residue;
3) adding the dried water-washed filter residue obtained in the step 2) into a muffle furnace, introducing air, and roasting at a programmed temperature, wherein the programmed temperature flow is as follows: keeping the temperature at 200 ℃ for 1h, raising the temperature to 250 ℃ for 1h, raising the temperature to 300 ℃ for 1h, raising the temperature to 350 ℃ for 2h, raising the temperature to 400 ℃ for 2h, raising the temperature to 600 ℃ for 2h, and introducing air to the temperature of 600 ℃ for 2h to obtain 61.98g of incineration ash;
4) adding 61.98g of incineration ash obtained in the step 3) into 100g of formic acid, boiling and reducing for 2h, and filtering to obtain 100.12g of waste formic acid and 61.10g of reduced filter residue;
5) 61.10g of reduced filter residue obtained in the step 4) is added into 502.90g of concentrated hydrochloric acid, the temperature is raised to micro reflux, 20.00g of chlorine gas is introduced, the temperature is reduced, and filtration is carried out, so that 498.80g of platinum-containing filtrate is obtained.
The platinum content was found to be 76.38ppm, and the platinum yield was found to be 95.25%.
Example 3
1) Dripping 200.00g platinum-containing organic silicon wastewater into 600.00g water for hydrolysis, and filtering to obtain 502.78g acid water and 296.21g hydrolysis filter residue;
2) adding 296.21g of hydrolysis filter residue obtained in the step 1) into 300.00g of water for washing, adding alkali liquor to adjust the pH value to be neutral, filtering and drying to obtain washing filter residue;
3) adding the dried water-washed filter residue obtained in the step 2) into a muffle furnace, introducing air, and roasting at a programmed temperature, wherein the programmed temperature flow is as follows: keeping the temperature at 200 ℃ for 1h, raising the temperature to 250 ℃ for 1h, raising the temperature to 300 ℃ for 1h, raising the temperature to 350 ℃ for 2h, raising the temperature to 400 ℃ for 2h, raising the temperature to 600 ℃ for 2h, and introducing air to the temperature of 600 ℃ for 2h to obtain 62.09g of incineration ash;
4) adding 62.09g of incineration ash obtained in the step 3) into 100g of formic acid, boiling and reducing for 2h, and filtering to obtain 101.50g of waste formic acid and 61.09g of reduced filter residue;
5) adding 61.09g of reduced filter residue obtained in the step 4) into 502.78g of acid water obtained in the step 1), heating to slightly reflux, introducing 20.00g of chlorine, cooling and filtering to obtain 502.66g of platinum-containing filtrate.
The platinum content is detected to be 76.03ppm, and the platinum yield is 95.54%.
Comparative example 3
1) Dripping 200.00g platinum-containing organic silicon wastewater into 600.00g water for hydrolysis, and filtering to obtain 505.68g acid water and 293.28g hydrolysis filter residue;
2) adding 293.28g of hydrolysis filter residue obtained in the step 1) into 300.00g of water for washing, adding alkali liquor to adjust the pH value to be neutral, filtering and drying to obtain washing filter residue;
3) adding the dried water-washed filter residue obtained in the step 2) into a muffle furnace, introducing air, and carrying out temperature programming roasting, wherein the temperature programming flow is as follows: keeping the temperature at 200 ℃ for 1h, raising the temperature to 250 ℃ for 1h, raising the temperature to 300 ℃ for 1h, raising the temperature to 350 ℃ for 2h, raising the temperature to 400 ℃ for 2h, and introducing air to the mixture for 2h at 400 ℃ to obtain 95.88g of incineration ash;
4) adding 95.88g of incineration ash obtained in the step 2) into 100g of formic acid, boiling and reducing for 2h, and filtering to obtain 102.67g of waste formic acid and 94.32g of reduced filter residue;
5) adding 94.32g of reduced filter residue obtained in the step 4) into acid water, heating to slightly reflux, introducing 20.00g of chlorine, cooling and filtering to obtain 504.77g of platinum-containing filtrate.
The platinum content is 67.79ppm and the platinum yield is 85.55%.
In conclusion, the above embodiments are merely intended to illustrate the technical solution of the present invention and not to limit, although the present invention has been described by referring to certain preferred embodiments thereof, it should be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims.