CN1775749A - Benzyl iso-octyl sulfoxide, and its preparing method, and method for extracting and separating palladium-platinum using same - Google Patents
Benzyl iso-octyl sulfoxide, and its preparing method, and method for extracting and separating palladium-platinum using same Download PDFInfo
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Abstract
The invention discloses a benzyl isooctyl sulfoxide, called BSO for short, molecular formula C15H24OS, and relative molecular weight 252.4. The preparing method is as follows: placing isooctyl thioalcohol in a flask, dissolving with alcohol, then adding in equimolar NaOH, heating, blending and returning, adding in equimolar benzyl chloride, continuing heating, blending and returning, filtering and evaporating solvent from filtrate and obtaining benzyl isooctyl thioether; dissolving the benzyl isooctyl thioether in acetic acid, blending and gradually adding in equimolar oxydol, then adding in water to make phase separation, extracting residual sulfoxide from the water phase with ethyl ether, merging organic phases, evaporating the ethyl ester and obtaining the product BSO. The invention also uses the BSO to extractively separate by the difference in the BSO extraction ratios of Pd and Pt in low basicity medium, and where the higher the Pd concentration is, the higher the separation coefficient is; and the invention uses the BSO to be able to perfectly coextract the Pd and Pt in high basicity medium, and then separate the Pt from the Pd by the difference in the water extraction ratios of Pd and Pt, the separation coefficient high.
Description
Technical field
The invention belongs to the sulfoxide compound field, relate in particular to a kind of benzyl iso-octyl sulfoxide (BSO) and preparation method thereof and with its method as the extraction agent extracting and separating palladium-platinum.
Background technology
Platinum and palladium belong to the platinum metals, owing to have the fusing point height, the characteristics that electroconductibility, solidity to corrosion and high-temperature stability are good, the while hot strength is big and the high temperature creep ability is strong, make them become the important materials of modern industry and national defense construction, be widely used in navigating in worker, space flight, guided missile, rocket, nuclear power, little power technology, chemical industry, glass industry, gas sweetening and the metallurgical industry, effect in new high-tech industry strengthens day by day, so be described as " VITAMIN " and " modern new metal " of modern industry.
Concerning China, the platinum metals resource-constrained, and do not have the platinum metals resource of exploitation separately.Platinum metals secondary resource yield is the important component part in China's platinum metals aggregate supply, year yield 3.5～4t.Under the situation of resource shortage, make full use of the recovery of domestic platinum metals mineral products resource and secondary resource and just seem more and more important.
Because physics, the chemical property of platinum metals are very similar, and valence state is changeable, nature difference is very big between the different valence state; Therefore, the platinum metals separation is the difficult problem in the metallurgy always.It is traditional that main platinum metals separating technology process is tediously long, yield is low, cost is high, troublesome poeration to be precipitated as, after solvent extraction and separation technology manifests its superiority, use this method extraction separation and purifying platinum metals and caused people's very big attention, and this method is acknowledged as the novel process of extraction separation platinum metals at present, and the precious metal smelting factory that has part has adopted the extracting and separating flow process.Along with the research and development of new extractant and extraction new system, abstraction technique research in platinum metals constantly obtains new progress.
Sulfoxide is as a kind of neutral extraction agent, and the electronation of its Sauerstoffatom can force rate neutral phosphate (RO)
3PO phosphinylidyne Sauerstoffatom is also strong, also has stable chemical performance simultaneously, the effect of ability strong acid, highly basic and oxygenant, and the flash-point height, operational safety, the extraction mechanical property is good.
Sulfoxide generally is divided into synthetic sulfoxide and petrolenum sulfoxide.Petrolenum sulfoxide is the new neutral extraction agent of a class that grows up in the sixties in twentyth century, becomes the extraction agent of industrial application gradually at the seventies.Have originate wide, little, the steady performance of toxicity.
In relevant numerous sulfoxides, comprise with dioctylsulfoxide(DOSO) extraction palladium platinum the platinum metals technical study the most extensively and profoundly, since the sixties in twentyth century a large amount of reports has been arranged at home and abroad, but because its solubility property in aliphatic hydrocarbon is poor, with consider from environmental angle, be difficult to large-scale industrial application always.
In China, and comprehensively with the research comparison system of petrolenum sulfoxide (PSO) extraction of palladium platinum.Petrolenum sulfoxide (PSO) be a kind of natural oil thioether mixture through oxidation or from high sulphur-bearing diesel through oxidation and the sulfoxide extraction agent, reclaiming precious metal with the PSO extraction has potential application foreground preferably.But because present high sulfur-bearing oil resource shortage, market competition is violent, and high sulphur-bearing diesel raw material supply existing problems have not had the PSO product on the market.
Summary of the invention
The object of the present invention is to provide a kind of benzyl iso-octyl sulfoxide (BSO) that is used for extracting and separating palladium-platinum and preparation method thereof.This BSO has good solubility in odorless kerosene(OK), palladium is had excellent extraction ability, equally platinum is had excellent extraction ability in high acidity medium, can well be used for extracting and separating palladium-platinum.
Another object of the present invention is to provide method with the benzyl iso-octyl sulfoxide extracting and separating palladium-platinum.
BSO of the present invention is a kind of asymmetric sulfoxide that contains benzyl, can be used for extracting and separating palladium-platinum, has good effect of extracting.The present invention is that molecular designing is carried out on the basis with the quantum chemistry calculation, synthesizes to have obtained BSO, and molecular formula is C
15H
24OS, relative molecular mass are 252.4, and structural formula is:
Its preparation process is as follows:
Get 1mol iso-octyl mercaptan and put into reaction flask, after adding 9～17mol dissolve with ethanol, add and the equimolar NaOH of iso-octyl mercaptan again, refluxed 20～60 minutes 80 ℃ of following heated and stirred, add and the equimolar benzyl chloride of iso-octyl mercaptan, continue heated and stirred and refluxed 1～3 hour, adularescent precipitation NaCl separates out, filter, filtrate boils off solvent with rotatory evaporator and obtains lurid benzyl iso-octyl thioether; The benzyl iso-octyl thioether is dissolved in the acetate, add and the equimolar hydrogen peroxide of iso-octyl mercaptan, stir after 1～3 hour, add water and continue to stir again, standing demix is told upper organic phase and lower floor's water, the sulfoxide of aqueous phase remnants is with ether extraction, merge upper organic phase, in rotatory evaporator, boil off ether, obtain BSO.
The concentration of described hydrogen peroxide is 30%.
Reaction equation:
The chemical property parameter of the above-mentioned BSO that obtains is:
Mass spectrum Fab-MS:m/z:253.0 (100%), 91.0 (32%); Infrared IR (KBr): v
S=O=1029.5cm
-1UV, visible light UV-Vis (λ max, nm, in CH
2Cl
2): 239.0,294.5, λ=407.5;
13C-NMR (400MHz, CDCl
3, ppm): 130.282,130.172,129.057,128.436,59.242,56.836,34.486,32.679,28.648,26.481,25.538,23.149,, 14.373,10.695.Molecular formula is C
15H
24OS, relative molecular mass are 252.4.
Make extraction experiments with BSO of the present invention: palladium feed liquid and platinum feed liquid contain palladium or platinum 1.000g/L respectively, and BSO is thinner with the odorless kerosene(OK), and as the used organic phase of extraction.By comparing (O/A) 1: 1 organic phase and feed liquid (water) are placed in the 10mL colorimetric cylinder, mixed phase left standstill after 5 minutes, and with the concentration of atomic absorption spectroscopy determination aqueous phase Pd or Pt, the concentration of Pd or Pt is obtained with minusing in the organic phase after the centrifugal phase-splitting.
The collection palladium effect:
Experimental results show that: fixedly feed liquid is 1.000g/L at the Pd initial concentration, and under different concentration of hydrochloric acid, the BSO of 0.3mol/L the results are shown in Table 1.1 to the percentage extraction influence of Pd.
Table 1.1 c (BSO) is that 0.3mol/L concentration is to extraction Pd performance under different HCL concentration
| HCl concentration (mol/L) | 0.1 | 1.0 | 2.0 | 3.0 | 4.0 |
| Percentage extraction E (%) | 100.0 | 100.0 | 99.4 | 99.6 | 99.9 |
Experimental results show that: fixedly feed liquid is 1.000g/L at the Pd initial concentration, with the fixing c (H of HCl
+)=0.1mol/L, NaCl regulates Cl
-Concentration, at different Cl
-Under the concentration, the BSO of 0.3mol/L the results are shown in Table 1.2 to the percentage extraction influence of Pd.
Table 1.2 c (BSO) is a 0.3mol/L concentration at different Cl
-Extraction Pd performance under the concentration
| Cl -Ionic concn (mol/L) | 0.1 | 1.0 | 2.0 | 3.0 | 4.0 |
| Percentage extraction E (%) | 100.0 | 91.4 | 62.9 | 43.3 | 39.7 |
Experimental results show that: fixedly feed liquid is 1.000g/L at the Pd initial concentration, with the fixing c (Cl of NaCl
-)=4mol/L is at different H
+Under the concentration, the BSO of 0.3mol/L the results are shown in Table 1.3 to the percentage extraction influence of Pd.
Table 1.3 c (BSO) is a 0.3mol/L concentration at different H
+Extraction Pd performance under the concentration
| H +Ionic concn (mol/L) | 0.1 | 1.0 | 2.0 | 3.0 | 4.0 |
| Percentage extraction E (%) | 37.9 | 44.8 | 95.5 | 99.4 | 99.9 |
The collection platinum effect:
Experimental results show that: fixedly feed liquid is 1.000g/L at the Pt initial concentration, and under different concentration of hydrochloric acid, the BSO of 0.6mol/L the results are shown in following table 2.1 to the percentage extraction influence of Pt.
Table 2.1 c (BSO) is that 0.6mol/L concentration is to extraction Pt performance under different HCl concentration
| HCl concentration (mol/L) | 0.1 | 1.0 | 2.0 | 3.0 | 4.0 |
| Percentage extraction E (%) | 3.0 | 3.3 | 18.5 | 91.8 | 99.5 |
Experimental results show that: fixedly feed liquid is 1.000g/L at the t initial concentration, respectively fixing c (H
+) be under 0.1mol/L and the 2.0mol/L concentration, NaCl regulates Cl
-Concentration, at different Cl
-Under the concentration, the BSO of 0.6mol/L the results are shown in Table 2.2 to the percentage extraction influence of Pt.
Table 2.2 c (BSO) is a 0.6mol/L concentration at different Cl
-Extraction Pt performance under the concentration
| Cl -Ionic concn (mol/L) | 0.1 | 1.0 | 2.0 | 3.0 | 4.0 | 5.0 |
| Percentage extraction E (%) (c (H +The percentage extraction of)=0.1mol/L) E (%) (c (H +)＝2.0mol/L) | 3.0 | 1.6 | 7.6 18.5 | 7.6 76.6 | 10.5 85.3 | 97.8 |
Experimental results show that: fixedly feed liquid is 1.000g/L at the Pt initial concentration, with the fixing c (Cl of NaCl
-)=4.0mol/L is at different H
+Under the concentration, the BSO of 0.6mol/L the results are shown in Table 2.3 to the percentage extraction influence of Pt.
Table 2.3 c (BSO) is a 0.6mol/L concentration at different H
+Extraction Pt performance under the concentration
| H +Ionic concn (mol/L) | 0.1 | 1.0 | 2.0 | 3.0 | 4.0 |
| Percentage extraction E (%) | 19.4 | 36.2 | 85.3 | 96.5 | 99.5 |
BSO of the present invention as can be seen has excellent extraction ability to palladium from experiment, equally platinum is had excellent extraction ability in high acidity medium.
Method with BSO extracting and separating palladium-platinum of the present invention has two kinds.
First kind: the H of the mixed liquor that contains palladium and platinum
+Concentration adjustment is in 0.1～1.0mol/L scope, as water; BSO is thinner with the odorless kerosene(OK), and concentration is 0.2～0.4mol/L, as the used organic phase of extraction; Comparing (O/A) 1: 1 with water by organic phase is placed on organic phase and water in the colorimetric cylinder, mixed phase left standstill after 2～5 minutes, use the concentration of atomic absorption spectroscopy determination aqueous phase Pd and Pt after the centrifugal phase-splitting, the concentration of Pd and Pt is obtained with minusing in the organic phase, calculates percentage extraction and separation factor.
Second kind: the H of the mixed liquor that contains palladium and platinum
+Concentration adjustment is in 3.0～5.0mol/L scope, as water; BSO is thinner with the odorless kerosene(OK), and concentration is 0.3～0.8mol/L, as the used organic phase of extraction; Comparing (O/A) 1: 1 with water by organic phase is placed on organic phase and water in the colorimetric cylinder, mixed phase left standstill after 2～5 minutes, use the concentration of atomic absorption spectroscopy determination aqueous phase Pd and Pt after the centrifugal phase-splitting, the concentration of Pd and Pt is obtained with minusing in the organic phase, get load the organic phase of Pd and Pt is arranged, be put in the colorimetric cylinder, add the entry back extraction again, behind the mixed phase 2～5 minutes, standing demix, with the concentration of Pd in the atomic absorption spectroscopy determination strip aqueous and Pt, and calculate Pt and the Pd back extraction ratio and the separation factor of water back extraction after the centrifugal phase-splitting.
The present invention has following advantage and beneficial effect:
(1) BSO of the present invention has excellent extraction ability to palladium, equally platinum is had excellent extraction ability in high acidity medium;
(2) the good extracting and separating palladium-platinum of BSO energy, the separation factor height;
(3) BSO has good solubility in the odorless kerosene(OK) product, and environmental pollution is little.
Embodiment
In order to understand the present invention better, the present invention is done to describe further below by embodiment.
Embodiment 1
Get 10g iso-octyl mercaptan and put into reaction flask, after adding the 40g dissolve with ethanol, add 2.74gNaOH again, after heated and stirred refluxed 30 minutes, add the 8.67g benzyl chloride, continue heated and stirred down at 80 ℃ and refluxed 2 hours, adularescent precipitation NaCl separates out, filter, filtrate boils off solvent with rotatory evaporator and obtains the lurid benzyl iso-octyl thioether of 16g; 16g benzyl iso-octyl thioether is dissolved in the acetate, 30% hydrogen peroxide that adds 6.72ml, stir after 2 hours, be dissolved in water and treat layering, tell upper organic phase and lower floor's water, the sulfoxide of aqueous phase remnants merges upper organic phase with ether extraction, boil off ether at rotatory evaporator, obtain 16.08g BSO.Test chemical property parameter is: mass spectrum Fab-MS:m/z:253.0 (100%), 91.0 (32%); Infrared IR (KBr): v
S=O=1029.5cm
-1UV, visible light UV-Vis (λ max, nm, in CH
2Cl
2): 239.0,294.5, λ=407.5;
13C-NMR (400MHz, CDCl
3, ppm): 130.282,130.172,129.057,128.436,59.242,56.836,34.486,32.679,28.648,26.481,25.538,23.149,, 14.373,10.695.Molecular formula is C
15H
24OS, relative molecular mass are 252.4.
Embodiment 2
Get 5g iso-octyl mercaptan and put into reaction flask, after adding the 15g dissolve with ethanol, add 1.37gNaOH again, after heated and stirred refluxed 20 minutes, add the 4.34g benzyl chloride, continue heated and stirred down at 80 ℃ and refluxed 1 hour, adularescent precipitation NaCl separates out, filter, filtrate boils off solvent with rotatory evaporator and obtains the lurid benzyl iso-octyl thioether of 8g; 8g benzyl iso-octyl thioether is dissolved in the acetate, 30% hydrogen peroxide that adds 3.36ml, stir after 1 hour, be dissolved in water and treat layering, tell upper organic phase and lower floor's water, the sulfoxide of aqueous phase remnants merges upper organic phase with ether extraction, boil off ether at rotatory evaporator, obtain 8.03g BSO.Test chemical property parameter such as embodiment 1.
Embodiment 3
Get 7.50g iso-octyl mercaptan and put into reaction flask, after adding the 37.5g dissolve with ethanol, add 2.06gNaOH again, after heated and stirred refluxed 60 minutes, add the 6.50g benzyl chloride, continue heated and stirred down at 80 ℃ and refluxed 3 hours, adularescent precipitation NaCl separates out, filter, filtrate boils off solvent with rotatory evaporator and obtains the lurid benzyl iso-octyl thioether of 12g; 12g benzyl iso-octyl thioether is dissolved in the acetate, 30% hydrogen peroxide that adds 5.04ml, stir after 3 hours, be dissolved in water and treat layering, tell upper organic phase and lower floor's water, the sulfoxide of aqueous phase remnants merges upper organic phase with ether extraction, boil off ether at rotatory evaporator, obtain 12.05g BSO.Test chemical property parameter is as embodiment 1.
Embodiment 4
Getting c (HCl) is 0.1mol/L, the mixed liquor 2ml (content of Pd and Pt is respectively 152.6mg/L and 745.0mg/L) that contains Pd and Pt, by comparing (O/A) 1: 1, add with the odorless kerosene(OK) is thinner again, the organic phase 2ml of c (BSO)=0.3mol/L, mixed phase is standing demix after 5 minutes, measure the concentration of aqueous phase palladium and platinum after the centrifugal phase-splitting respectively with atomic absorption spectrophotometry, palladium in the organic phase and platinum concentration are obtained with minusing, obtaining separation factor is 2.16E+03, and concrete data see Table 3.
Embodiment 5
Getting c (HCl) is 0.3mol/L, the mixed liquor 2ml (content of Pd and Pt is respectively 381.6mg/L and 465.6mg/L) that contains Pd and Pt, by comparing (O/A) 1: 1, add with the odorless kerosene(OK) is thinner again, the organic phase 2ml of c (BSO)=0.2mol/L, mixed phase is standing demix after 3 minutes, measure the concentration of aqueous phase palladium and platinum after the centrifugal phase-splitting respectively with atomic absorption spectrophotometry, palladium in the organic phase and platinum concentration are obtained with minusing, obtaining separation factor is 5.22E+03, and concrete data see Table 3.
Embodiment 6
Getting c (HCl) is 0.9mol/L, the mixed liquor 2ml (content of Pd and Pt is respectively 610.6mg/L and 186.2mg/L) that contains Pd and Pt, by comparing (O/A) 1: 1, add with the odorless kerosene(OK) is thinner again, the organic phase 2ml of c (BSO)=0.4mol/L, mixed phase is standing demix after 2 minutes, measure the concentration of aqueous phase palladium and platinum after the centrifugation respectively with atomic absorption spectrophotometry, palladium in the organic phase and platinum concentration are obtained with minusing, obtaining separation factor is 2.23E+05, and concrete data see Table 3.
Embodiment 7
Getting c (HCl) is 3.0mol/L, the mixed liquor 2ml (content of Pd and Pt is respectively 156.0mg/L and 939.8mg/L) that contains Pd and Pt, by comparing (O/A) 1: 1, add with the odorless kerosene(OK) is thinner again, the organic phase 2ml of c (BSO)=0.3mol/L, mixed phase is standing demix after 5 minutes, measure the concentration of aqueous phase palladium and platinum after the centrifugal phase-splitting respectively with atomic absorption spectrometry, palladium in the organic phase and platinum concentration are obtained with minusing, get load the organic phase of Pd and Pt is arranged, be put in the colorimetric cylinder, add the entry back extraction again, mixed phase 2 minutes, standing demix, measure the concentration of palladium and platinum in the strip aqueous after the centrifugal phase-splitting with atomic absorption spectrophotometry respectively, calculate back extraction ratio, obtain separation factor β (D
Pt/ D
Pd) be 1.41E+02, concrete data see Table 4.
Embodiment 8
Getting c (HCl) is 5.0mol/L, the mixed liquor 2ml (content of Pd and Pt is respectively 389.9mg/L and 587.4mg/L) that contains Pd and Pt, by comparing (O/A) 1: 1, add with the odorless kerosene(OK) is thinner again, the organic phase 2ml of c (BSO)=0.8mol/L, mixed phase is standing demix after 3 minutes, measure the concentration of aqueous phase palladium and platinum after the centrifugation respectively with atomic absorption spectrometry, palladium in the organic phase and platinum concentration are obtained with minusing, off-loading has the organic phase of Pd and Pt, be put in the colorimetric cylinder, add the entry back extraction again, mixed phase 3 minutes, standing demix, measure the concentration of palladium and platinum in the strip aqueous after the centrifugal phase-splitting with atomic absorption spectrophotometry respectively, calculate back extraction ratio, obtain separation factor β (D
Pt/ D
Pd) be 2.28E+02, concrete data see Table 4.
Embodiment 9
Getting c (HCl) is 4.0mol/L, the mixed liquor 2ml (content of Pd and Pt is respectively 623.9mg/L and 235.0mg/L) that contains Pd and Pt, by comparing (O/A) 1: 1, add with the odorless kerosene(OK) is thinner again, the organic phase 2ml of c (BSO)=0.5mol/L, mixed phase is standing demix after 2 minutes, measure the concentration of aqueous phase palladium and platinum after the centrifugation respectively with atomic absorption spectrometry, palladium in the organic phase and platinum concentration are obtained with minusing, off-loading has the organic phase of Pd and Pt, be put in the colorimetric cylinder, add the entry back extraction again, mixed phase 5 minutes, standing demix, measure the concentration of palladium and platinum in the strip aqueous after the centrifugal phase-splitting with atomic absorption spectrophotometry respectively, calculate back extraction ratio, obtain separation factor β (D
Pt/ D
Pd) be 5.04E+03, concrete data see Table 4.
Extraction Pd and the isolating separation factor of Pt under table 3.0.1～1.0mol/l HCl acidity
| Pd | Pt | Separation factor β (D Pd/D Pt) | ||||||
| Pd concentration (mg/L) | Pd percentage extraction E (%) | Pd partition ratio D | Pt concentration (mg/L) | Pt percentage extraction E (%) | Pt partition ratio D | |||
| Embodiment 4 embodiment 5 | Feed liquid raffinate feed liquid raffinate | 152.6 5.7 381.6 1.5 | 96.3 99.6 | 25.874 250.756 | 745.0 736.4 465.6 444.1 | 1.2 4.6 | 0.012 0.048 | 2.16E+03 5.22E+03 |
| Embodiment 6 | The feed liquid raffinate | 610.6 0.7 | 99.9 | 893.032 | 186.2 185.5 | 0.4 | 0.004 | 2.23E+05 |
Extraction Pd and the isolating separation factor of Pt under table 4.3.0～5.0mol/l HCl acidity
| Pd | Pt | Separation factor β (D Pd/D Pt) | ||||||
| Pd concentration (mg/L) | Pd percentage extraction E (%) | Pd partition ratio D | Pt concentration (mg/L) | Pt percentage extraction E (%) | Pt partition ratio D | |||
| Embodiment 7 embodiment 8 embodiment 9 | Feed liquid raffinate water strip liquor *Feed liquid raffinate water strip liquor *Feed liquid raffinate water strip liquor * | 156.0 4.8 12.7 389.9 0.7 15.2 623.9 0.7 15.2 | 96.9 8.4 99.8 3.9 99.9 2.4 | 31.179 0.092 569.965 0.041 912.544 0.025 | 939.8 225.2 663.331 587.4 186.2 395.437 235.0 47.0 186.5 | 76.0 92.8 68.3 98.6 80.0 99.2 | 3.173 12.938 2.154 69.369 4.000 126.0 | 9.83E+00 1.41E+02 2.65E+02 1.69E+03 2.28E+02 5.04E+03 |
* for water back extraction result, the E of Pd and Pt is back extraction ratio, and separation factor β is β (D
Pt/ D
Pd)
The good extracting and separating palladium-platinum of BSO of the present invention as can be seen from Table 3 energy in low acidity medium, it is high more to separate coefficient when Pd concentration is high more; The BSO of the present invention as can be seen from Table 4 palladium platinum that can well come together altogether in high acidity medium can the good back extraction Pt of water, the separation factor height.
Claims (5)
1. a benzyl iso-octyl sulfoxide is characterized in that molecular formula is C
15H
24OS, relative molecular mass are 252.4, and structural formula is:
2. benzyl iso-octyl sulfoxide according to claim 1 is characterized in that the preparation method is as follows:
Get 1mol iso-octyl mercaptan and put into reaction flask, after adding 9～17mol dissolve with ethanol, add and the equimolar NaOH of iso-octyl mercaptan again, refluxed 20～60 minutes 80 ℃ of following heated and stirred, add and the equimolar benzyl chloride of iso-octyl mercaptan, continue heated and stirred and refluxed 1～3 hour, adularescent precipitation NaCl separates out, filter, filtrate boils off solvent with rotatory evaporator and obtains lurid benzyl iso-octyl thioether; The benzyl iso-octyl thioether is dissolved in the acetate, add and the equimolar hydrogen peroxide of iso-octyl mercaptan, stir after 1～3 hour, add water and continue to stir again, standing demix is told upper organic phase and lower floor's water, the sulfoxide of aqueous phase remnants is with ether extraction, merge upper organic phase, in rotatory evaporator, boil off ether, obtain C
15H
24OS.
3. benzyl iso-octyl sulfoxide according to claim 2, the concentration that it is characterized in that described hydrogen peroxide is 30%.
4. with the method for the described benzyl iso-octyl sulfoxide extracting and separating palladium-platinum of claim 1, it is characterized in that process is as follows:
The H+ concentration adjustment of the mixed liquor that contains palladium and platinum in 0.1～1.0mol/L scope, as water; BSO is thinner with the odorless kerosene(OK), and concentration is 0.2～0.4mol/L, as the used organic phase of extraction; Comparing 1: 1 by organic phase with water is placed on organic phase and water in the colorimetric cylinder, mixed phase left standstill after 2～5 minutes, with the concentration of atomic absorption spectroscopy determination aqueous phase Pd and Pt, the concentration of Pd and Pt is obtained with minusing in the organic phase, calculates percentage extraction and separation factor after the centrifugal phase-splitting.
5. with the method for the described benzyl iso-octyl sulfoxide extracting and separating palladium-platinum of claim 1, it is characterized in that process is as follows:
The H+ concentration adjustment of the mixed liquor that contains palladium and platinum in 3.0～5.0mol/L scope, as water; BSO is thinner with the odorless kerosene(OK), and concentration is 0.3～0.8mol/L, as the used organic phase of extraction; Comparing 1: 1 by organic phase with water is placed on organic phase and water in the colorimetric cylinder, mixed phase left standstill after 2～5 minutes, use the concentration of atomic absorption spectroscopy determination aqueous phase Pd and Pt after the centrifugal phase-splitting, the concentration of Pd and Pt is obtained with minusing in the organic phase, get load the organic phase of Pd and Pt is arranged, be put in the colorimetric cylinder, add the entry back extraction again, mixed phase is standing demix after 2～5 minutes, with the concentration of Pd in the atomic absorption spectroscopy determination strip aqueous and Pt, and calculate Pd and the Pt back extraction ratio and the separation factor of water back extraction after the centrifugal phase-splitting.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187932A (en) * | 2016-07-27 | 2016-12-07 | 红河学院 | 2 (2 methoxy ethyl sulfinyl) benzoxazoles method of extracting and separating palladium from many metallic ion mixed liquors |
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2005
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187932A (en) * | 2016-07-27 | 2016-12-07 | 红河学院 | 2 (2 methoxy ethyl sulfinyl) benzoxazoles method of extracting and separating palladium from many metallic ion mixed liquors |
| CN106316980A (en) * | 2016-07-27 | 2017-01-11 | 红河学院 | 2-(sulfo-2-methoxyethyl)benzothiazole and its preparation method and use |
| CN106187932B (en) * | 2016-07-27 | 2020-07-14 | 红河学院 | Method for extracting and separating palladium from multi-metal ion mixed solution by using 2- (2-methoxyethylsulfinyl) benzoxazole |
| CN106316980B (en) * | 2016-07-27 | 2021-02-05 | 红河学院 | 2- (sulfo-2-methoxyethyl) benzothiazole and preparation method and application thereof |
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