CN104774187B - 2-(hexylsulfinyl) benzoxazoles and preparation and the method with its extract and separate iridium, rhodium - Google Patents

2-(hexylsulfinyl) benzoxazoles and preparation and the method with its extract and separate iridium, rhodium Download PDF

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CN104774187B
CN104774187B CN201510214709.6A CN201510214709A CN104774187B CN 104774187 B CN104774187 B CN 104774187B CN 201510214709 A CN201510214709 A CN 201510214709A CN 104774187 B CN104774187 B CN 104774187B
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黄章杰
陈慕涵
张金燕
李�荣
吴胜杰
刘婉秋
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Yunnan University YNU
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D263/00—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings
    • C07D263/52—Heterocyclic compounds containing 1,3-oxazole or hydrogenated 1,3-oxazole rings condensed with carbocyclic rings or ring systems
    • C07D263/54—Benzoxazoles; Hydrogenated benzoxazoles
    • C07D263/58—Benzoxazoles; Hydrogenated benzoxazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
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    • C22B3/34—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing sulfur, e.g. sulfonium
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Abstract

2-(hexylsulfinyl) benzoxazoles and preparation and the method with its extract and separate iridium, rhodium, belong to the preparation of oxazole heterocyclic compounds and use.The compounds of this invention is called for short HSBO, molecular formula C13H17NO2S, Mr 251.10.It is prepared by dissolving 2-(hexyl sulfo-with alcoholic solution) benzoxazoles, drip K under temperature control 40～45 DEG C stirring2S2O8Solution, stratification, collected organic layer.Extraction includes regulating containing Ir, Rh aqueous phase H+Ir in aqueous phase (III), at 1.0～6.0 mol/L, is oxidized to Ir (IV) by concentration；Preparation organic facies, makes Ir transfer to organic facies from aqueous phase, with NaOH solution back extraction Ir.The present invention utilizes HSBO to Ir (IV), Rh(III) difference of extraction yield comes extract and separate Ir, Rh, and Ir (IV) has the extraction ability of excellence, Ir (IV), Rh(III) separation is high.

Description

2-(hexylsulfinyl) benzoxazoles and preparation and the method with its extract and separate iridium, rhodium
Technical field
The invention belongs to oxazole heterocyclic compounds and preparation the method relating to extract and separate iridium, rhodium.
Background technology
Iridium, rhodium chemical property are quite similar, existence in hydrochloric acid medium is sufficiently complex again, therefore, rhodium, iridium separate and are always up a difficult problem generally acknowledged in the metallurgy of platinum group metal, and current rhodium, iridium separation process technique mainly have: the sedimentation method, ion exchange and solvent extraction.These methods are respectively arranged with its feature:
The sedimentation method mainly include NH4CI, KCl sedimentation method and the large volume organic cation sedimentation method, the former direct yield is low, the latter is only suitable in a large amount of rhodium to separate a small amount of iridium, in addition, adopt the precipitant such as hydrogen sulfide, sodium sulfide, dioxy thiourea also can realize iridium, rhodium precipitate and separate, but the common shortcoming of the sedimentation method is that separating step is many, cycle length and inferior separating effect.Ion exchange mainly by anion exchange resin to IrCl6 2-Absorption comparison RhCl6 3-Higher characteristic carries out the separation between iridium, rhodium, and Ir (IV) is had reproducibility due to resin by this kind of method, so iridium, rhodium separate not thorough, it addition, limit its treatment scale because of resin absorption finite capacity.
Separation process is continuous, Process configuration is flexible, direct yield is high and operates the features such as safety owing to having for solvent extraction, is always up the prevailing technology of iridium, rhodium separation.Iridium, rhodium solvent extraction and separation are generally adopted phosphorus extractant and amine extractant, and phosphorus extractant mainly has tributyl phosphate (TBP), trioctyl phosphine oxide (TOPO) and trialkyl phosphine (TRPO) etc..TBP extraction is suitable in a small amount of iridium extracted a large amount of rhodiums, and separation when cannot be used for rhodium iridium concentration comparable or iridium concentration more than rhodium.In addition, TBP is unstable under highly acidity easily to be decomposed, the common material such as lucite and polrvinyl chloride there is corrosion swelling action, equipment selection difficulty during practice, the shortcoming adopting TOPO and TRPO is that the corrosion to lucite is also more serious than TBP, and TOPO and TRPO synthesizes cost height, practical application is very limited.The primary amine of amine extractant, secondary amine, tertiary amine, quaternary ammonium salt can extract iridium, extracting power quaternary ammonium salt from chloride media > tertiary amine > secondary amine > primary amine.Amine extractant mainly has: secondary carbon platinum amine (N1923), tri-n-octyl amine (TOA), N235(Alamine336), N263, N-hexyl valnoctamide (MNA) etc., though amine extractant extracting power is strong, but selectivity is relatively low, back extraction is also more difficult, commercial application that so far there are no.The efficiently new extraction system of development of new extractant and foundation, to increase the adaptability to material, improves separation efficiency, reduction cost, improves the industrial usability of method, be current iridium, rhodium solvent extraction and separation institute urgent problem.
Summary of the invention
First the purpose of the present invention is to provide a kind of new oxazole heterocyclic compounds: 2-(hexylsulfinyl) benzoxazoles (being called for short HSBO), and the method preparing this compound.
Meanwhile, it is desirable to provide one utilizes this compound (being called for short HSBO) to separate iridium, rhodium and the method with excellent extract and separate performance.
The object of the invention is accomplished by:
(1) the compounds of this invention 2-(hexylsulfinyl) benzoxazoles
This compound molecule formula is C13H17NO2S, relative molecular mass is 251.10, and structural formula is:
Above compound is referred to as HSBO.
The HSBO of the present invention is a kind of oxazole heterocyclic compounds, can be used for extract and separate iridium, rhodium.
Described 2-(hexylsulfinyl) the chemical characteristic parameter of benzoxazoles (be called for short HSBO) is:
Infrared IR(KBr): ν 2928,2859,1603,1499,1453,1236,1132,1090,744cm-1;
1HNMR (300MHz, CDCl3) δ 7.54(1H, d, J=6.5Hz), 7.38(1H, d, J=6.5Hz), 7.04(1H, m), 6.90(1H, m), and 2.99(2H, t, J=6.0Hz), 1.71-1.61 (2H, m), 1.44-1.27(6H, m), 0.89 (3H, t, J=6.5) ppm;
13CNMR(75MHz,CDCl3) δ 168.4,147.1,126.1,121.8,120.9,117.9,31.3,30.7,30.1,28.4,22.5,14.0ppm;
HRMS (ESI) m/z:found:274.0871 (M+Na)+；calc:274.0872(M+Na)+。
(2) preparation of the compounds of this invention HSBO
One prepares 2-(hexylsulfinyl) method of benzoxazoles (be called for short HSBO):
Weighing 2-(hexyl sulfo-) benzoxazoles 23.5g is in there-necked flask, and addition, by 20mL95% alcoholic solution, drips 20mL0.1mol/LK2S2O8Solution, controls reaction temperature to stir 40min at 40～45 DEG C, then places 12h, precipitate out light yellow oil, separate organic facies, obtain 2-(hexylsulfinyl) benzoxazoles, its reaction equation is:
(3) by the method for HSBO extract and separate iridium, rhodium
Comprise the following steps:
(1) preparation aqueous phase: regulate the H of Rh and Ir mixed liquor with HCI+Concentration, makes the H of mixed liquor+Concentration is 1.0～6.0mol/L, and adds the appropriate sodium chlorate solution of people, and making Ir oxidation number in mixed liquor is+4;
(2) preparation organic facies: HSBO is with sulfonated kerosene for diluent, and concentration is 0.1～0.4mol/L, as extracting organic facies used；
(3) organic facies is put in separatory funnel with aqueous phase by comparing (O/A) 1:1, stand after mixed phase 6～10min, divide and afterwards Ir is transferred to organic facies from aqueous phase mutually；
(4) take the organic facies being loaded with Ir, be placed in separatory funnel, add 0.1～0.3mol/LNaOH solution back extraction, by comparing (O/A) 1:1, stand after mixed phase 5～8min, treat point to collect Ir mutually；
Described extract and separate Ir, the method for Rh, step (3) is further for point measuring the concentration of Ir and Rh in aqueous phase and organic facies mutually afterwards, and calculates extraction yield and separation.
Described extract and separate Ir, the method for Rh, step (4) is further for point measuring a concentration of Ir in back extraction mutually mutually afterwards, and calculates the back extraction ratio of NaOH solution back extraction Ir
The present invention has such good effect:
The HSBO of the present invention, adapts to Acidity Range width, and Ir (IV) has the extraction ability of excellence in 1.0～6.0mol/L hydrochloric acid medium；Ir, Rh separation is high, β (DIr/Rh) > 103, separate it is thus possible to realize Ir, Rh very well；HSBO synthetic method is simple, and cost is low, and the common material such as lucite and polrvinyl chloride is not corroded, and industrial sector equipment requirements is low；Back extraction condition is easily to control, and back extraction ratio is higher；Expand material subject range, be applicable not only to a small amount of iridium extracting in a large amount of rhodium, and separation when can be used for Ir, Rh concentration comparable or Ir concentration more than Rh, enhance the industrial usability of solvent extraction and separation iridium, rhodium.
Above-mentioned advantage can be found out from experiment, and extraction experiments result is as follows:
1. extract the effect of iridium
With sodium chlorate solution, Ir in aqueous phase (III) is oxidized to Ir (IV), containing iridium 1.027g/L feed liquid as extracting aqueous phase used after oxidation, HSBO is with sulfonated kerosene for diluent, concentration is 0.3mol/L, as extracting organic facies used, by comparing (O/A) 1:1,20mL organic facies and 20mL feed liquid (aqueous phase) are put in 125mL separatory funnel, stand after 10 points of kinds of mixed phase, divide and measure the concentration of iridium in aqueous phase mutually afterwards, in organic facies, the concentration minusing of iridium is obtained, and under different concentration of hydrochloric acid, extraction experiments result is in Table 1.
The HSBO of table 1.0.3mol/L extracts Ir performance under different HCl concentration
HCl concentration (mol/L) 1.0 2.0 3.0 4.0 5.0 6.0
Extraction yield E (%) 99.2 99.2 99.0 99.4 99.1 99.0
In 1.0～6.0mol/L hydrochloric acid medium, Ir (IV) is had the extraction ability of excellence by HSBO.
2. extract the effect of rhodium
Rhodium feed liquid rhodium-containing 1.103g/L, HSBO is with sulfonated kerosene for diluent, concentration is 0.3mol/L, as extracting organic facies used, by comparing (O/A) 1:1,20mL organic facies and 20mL feed liquid (aqueous phase) are put in 125mL separatory funnel, stand after 10 points of kinds of mixed phase, divide and measure the concentration of rhodium in aqueous phase mutually afterwards, in organic facies, the concentration minusing of rhodium is obtained, and under different concentration of hydrochloric acid, extraction experiments result is in Table 2.
The HSBO of table 2.0.3mol/L extracts Rh performance under different HCl concentration
HCl concentration (mol/L) 1.0 2.0 3.0 4.0 5.0 6.0
Extraction yield E (%) 1.8 2.3 2.2 1.9 2.0 1.6
The HSBO extraction yield equal < 2.5% to Rh in 1.0～6.0mol/L hydrochloric acid medium.
In order to be more fully understood that the present invention, below by detailed description of the invention, the present invention is further described through, but cited embodiment is not limiting as the scope of protection of the invention.
Detailed description of the invention
(1) 2-(hexylsulfinyl) benzoxazoles (being called for short HSBO)
Weigh 2-hexyl sulfo-benzoxazoles 23.5g in there-necked flask, add by 20mL95% alcoholic solution, drip 20mL0.1mol/LK2S2O8Solution, controls reaction temperature to stir 40min at 40～45 DEG C, then places 12h, precipitate out light yellow oil, separate organic facies, obtain 2-(hexylsulfinyl) benzoxazoles.
Test chemical characteristic parameter is:
Infrared IR(KBr): ν 2928,2859,1603,1499,1453,1236,1132,1090,744cm-1;
1HNMR (300MHz, CDCl3) δ 7.54(1H, d, J=6.5Hz), 7.38(1H, d, J=6.5Hz), 7.04(1H, m), 6.90(1H, m), and 2.99(2H, t, J=6.0Hz), 1.71-1.61 (2H, m), 1.44-1.27(6H, m), 0.89 (3H, t, J=6.5) ppm;
13CNMR(75MHz,CDCl3) δ 168.4,147.1,126.1,121.8,120.9,117.9,31.3,30.7,30.1,28.4,22.5,14.0ppm;
HRMS (ESI) m/z:found:274.0871 (M+Na)+；calc:274.0872(M+Na)+。
(2) HSBO extract and separate iridium of the present invention, rhodium and effect
Embodiment 1
A, to take C (HCl) be 1.0mol/L, and mixed liquor 20mL containing Ir and Rh after sodium chlorate solution aoxidizes, making Ir oxidation number is+4, the content of Ir and Rh respectively 165mg/L and 158mg/L in this mixed liquor, is placed in 125mL separatory funnel.With sulfonated kerosene for diluent, the organic facies 20mL of preparation C (HSBO)=0.1mol/L.By comparing (O/A) 1:1, stratification after 6 points of kinds of mixed phase, divide and measure the concentration of Ir and Rh in aqueous phase mutually afterwards, Ir and the Rh concentration minusing in organic facies is obtained, and obtaining Ir and Rh separation is 4.5 × 103(concrete data are in Table 3).
B, take the organic facies being loaded with Ir, it is placed in separatory funnel, by comparing (O/A) 1:1, add 0.1mol/LNaOH solution back extraction, stratification after 6 points of kinds of mixed phase, divide and measure the concentration of Ir in back extraction mutually mutually afterwards, and calculate the back extraction ratio (concrete data are in Table 3) with NaOH solution back extraction Ir.
Embodiment 2
A, to take C (HCl) be 2.0mol/L, and mixed liquor 20mL containing Ir and Rh after sodium chlorate solution aoxidizes, making Ir oxidation number is+4, the content of Ir and Rh respectively 86mg/L and 874mg/L in this mixed liquor, is placed in 125mL separatory funnel.With sulfonated kerosene for diluent, the organic facies 20mL of preparation C (HSBO)=0.2mol/L.By comparing (O/A) 1:1, stratification after 7 points of kinds of mixed phase, divide and measure the concentration of Ir and Rh in aqueous phase mutually afterwards, Ir and the Rh concentration minusing in organic facies is obtained, and obtaining Ir and Rh separation is 6.1 × 103(concrete data are in Table 3).
B, take the organic facies being loaded with Ir, it is placed in separatory funnel, by comparing (O/A) 1:1, add 0.1mol/LNaOH solution back extraction, after 5 points of kinds of mixed phase, stratification, divides and measures the concentration of Ir in back extraction mutually mutually afterwards, and calculate the back extraction ratio (concrete data are in Table 3) with NaOH solution back extraction Ir.
Embodiment 3
A, to take C (HCl) be 3.0mol/L, and mixed liquor 20mL containing Ir and Rh after sodium chlorate solution aoxidizes, making Ir oxidation number is+4, the content of Ir and Rh respectively 526mg/L and 518mg/L in this mixed liquor, is placed in 125mL separatory funnel.With sulfonated kerosene for diluent, the organic facies 20mL of preparation C (HSBO)=0.3mol/L.By comparing (O/A) 1:1, stratification after 8 points of kinds of mixed phase, divide and measure the concentration of Ir and Rh in aqueous phase mutually afterwards, Ir and the Rh concentration minusing in organic facies is obtained, and obtaining Ir and Rh separation is 4.0 × 103(concrete data are in Table 3).
B, take the organic facies being loaded with Ir, it is placed in separatory funnel, by comparing (O/A) 1:1, add 0.2mol/LNaOH solution back extraction, after 7 points of kinds of mixed phase, stratification, divides and measures the concentration of Ir in back extraction mutually mutually afterwards, and calculate the back extraction ratio (concrete data are in Table 3) with NaOH solution back extraction Ir.
Embodiment 4
A, to take C (HCl) be 4.0mol/L, and mixed liquor 20mL containing Ir and Rh after sodium chlorate solution aoxidizes, making Ir oxidation number is+4, the content of Ir and Rh respectively 1214mg/L and 78mg/L in this mixed liquor, is placed in 125mL separatory funnel.With sulfonated kerosene for diluent, the organic facies 20mL of preparation C (HSBO)=0.4mol/L.By comparing (O/A) 1:1, stratification after 10 points of kinds of mixed phase, divide and measure the concentration of Ir and Rh in aqueous phase mutually afterwards, Ir and the Rh concentration minusing in organic facies is obtained, and obtaining Ir and Rh separation is 5.9 × 103(concrete data are in Table 3).
B, take the organic facies being loaded with Ir, it is placed in separatory funnel, by comparing (O/A) 1:1, add 0.3mol/LNaOH solution back extraction, after 8 points of kinds of mixed phase, stratification, divides and measures the concentration of Ir in back extraction mutually mutually afterwards, and calculate the back extraction ratio (concrete data are in Table 3) with NaOH solution back extraction Ir.
Embodiment 5
A, to take C (HCl) be 5.0mol/L, and mixed liquor 20mL containing Ir and Rh after sodium chlorate solution aoxidizes, making Ir oxidation number is+4, the content of Ir and Rh respectively 428mg/L and 376mg/L in this mixed liquor, is placed in 125mL separatory funnel.With sulfonated kerosene for diluent, the organic facies 20mL of preparation C (HSBO)=0.3mol/L.By comparing (O/A) 1:1, stratification after 8 points of kinds of mixed phase, divide and measure the concentration of Ir and Rh in aqueous phase mutually afterwards, Ir and the Rh concentration minusing in organic facies is obtained, and obtaining Ir and Rh separation is 7.7 × 103(concrete data are in Table 3).
B, take the organic facies being loaded with Ir, it is placed in separatory funnel, by comparing (O/A) 1:1, add 0.2mol/LNaOH solution back extraction, after 7 points of kinds of mixed phase, stratification, divides and measures the concentration of Ir in back extraction mutually mutually afterwards, and calculate the back extraction ratio (concrete data are in Table 3) with NaOH solution back extraction Ir.
Embodiment 6
A, to take C (HCl) be 6.0mol/L, and mixed liquor 20mL containing Ir and Rh after sodium chlorate solution aoxidizes, making Ir oxidation number is+4, the content of Ir and Rh respectively 682mg/L and 654mg/L in this mixed liquor, is placed in 125mL separatory funnel.With sulfonated kerosene for diluent, the organic facies 20mL of preparation C (HSBO)=0.4mol/L.By comparing (O/A) 1:1, stratification after 9 points of kinds of mixed phase, divide and measure the concentration of Ir and Rh in aqueous phase mutually afterwards, Ir and the Rh concentration minusing in organic facies is obtained, and obtaining Ir and Rh separation is 6.8 × 103(concrete data are in Table 3).
B, take the organic facies being loaded with Ir, it is placed in separatory funnel, by comparing (O/A) 1:1, add 0.2mol/LNaOH solution back extraction, after 7 points of kinds of mixed phase, stratification, divides and measures the concentration of Ir in back extraction mutually mutually afterwards, and calculate the back extraction ratio (concrete data are in Table 3) with NaOH solution back extraction Ir.
Above C (HCl) is the HCl mixed liquor containing Ir and Rh, and above C (HSBO) is sulfonated kerosene and the HSBO organic facies being mixed with, and wherein, sulfonated kerosene is diluent, and HSBO is extractant.
Ir and Rh separation case in table 3.1.0～6.0mol/L hydrochloric acid medium
Ir (IV) is had the extraction ability of excellence by the HSBO of the present invention in 1.0～6.0mol/L hydrochloric acid medium as can be seen from Table 3, it is applicable not only to a small amount of iridium extracting in a large amount of rhodium, and separation when can be used for Ir, Rh concentration comparable or Ir concentration more than Rh concentration.The equal > 10 of Ir, Rh separation3, efficiently separating of Ir, Rh can be realized, 0.1～0.3mol/LNaOH solution can good back extraction Ir.

Claims (5)

1.2-(hexylsulfinyl) benzoxazoles, this compound molecule formula is C13H17NO2S, Mr251.10, structural formula is:
Above compound is referred to as HSBO.
2. the method preparing compound as claimed in claim 1, comprises the following steps:
Weigh 2-(hexyl sulfo-) benzoxazoles 23.5g in round-bottomed flask, add 20mL95% alcoholic solution, drip 20mL0.1mol/LK2S2O8Solution, controls reaction temperature to stir 40min at 40～45 DEG C, then places 12h, precipitate out light yellow oil, separate organic facies, obtain product HSBO, and its reaction equation is:
。
3. the method utilizing the Compound extraction separation iridium described in claim 1, rhodium, comprises the following steps:
(1) preparation aqueous phase: regulate the H of Ir and Rh mixed liquor with HCl+Concentration, makes the H of mixed liquor+Concentration is 1.0～6.0mol/L, and adds appropriate sodium chlorate solution, and making Ir oxidation number in mixed liquor is+4；
(2) preparation organic facies: HSBO is with sulfonated kerosene for diluent, and concentration is 0.1～0.4mol/L, as extracting organic facies used；
(3) putting in separatory funnel with aqueous phase by comparing (O/A) 1:1 by organic facies, stand after mixed phase 6～10min, a point rear mutually Ir transfers to organic facies from aqueous phase, and Rh is retained in aqueous phase；
(4) take the organic facies being loaded with Ir, be placed in separatory funnel, by comparing (O/A) 1:1, add 0.1～0.3mol/LNaOH solution back extraction, stand after mixed phase 5～8min, treat point to collect Ir mutually.
4. method according to claim 3, further characterized in that: the concentration of Ir and Rh in determination step (3) point rear aqueous phase mutually, in organic facies, the concentration minusing of Ir and Rh is obtained, and calculates extraction yield and separation.
5. the method according to claim 3 or 4, further characterized in that: the concentration of Ir in determination step (4) point rear back extraction mutually mutually, and calculate the back extraction ratio of NaOH solution back extraction Ir.
CN201510214709.6A 2015-04-30 2015-04-30 2-(hexylsulfinyl) benzoxazoles and preparation and the method with its extract and separate iridium, rhodium Expired - Fee Related CN104774187B (en)

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