CN104313324B - By dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium method of extraction of palladium from alkaline cyanide liquid - Google Patents
By dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium method of extraction of palladium from alkaline cyanide liquid Download PDFInfo
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Abstract
By dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium method of extraction of palladium from alkaline cyanide liquid, belong to precious metal hydrometallurgy. Including regulating [Pd (CN)4]2-Material liquid pH 9.5-11.5 is as the aqueous phase of extraction system; With dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium (being called for short DDPB) for extractant, for synergic reagent one of in n-amyl alcohol or hexanol or n-heptanol or n-octyl alcohol or Decanol, for diluent one of in benzene or dimethylbenzene or normal heptane or sulfonated kerosene, does is DDPB concentration in organic facies 0.01 ~ 0.03? mol/L and mixed phase, stratification, by [Pd (CN)4]2-Organic facies is transferred to, with 0.1 ~ 0.3 from aqueous phase? mol/L? NH4SCN solution back extraction palladium etc. The saturated loading capacity of solvent-extraction system of the present invention is high, and back extraction is easy, and extraction cycle is short, and cost is low, has popularizing application prospect.
Description
Technical field
The invention belongs to precious metal hydrometallurgy, the technique particularly relating to extract palladium from alkaline cyanide liquid.
Background technology
For extracting the metallurgical technology of platinum group metal from flotation concentrate, all adopt the firing method process of matte smelting trapping noble metal both at home and abroad, this flow process precious metal refinery complex process, noble metal recovery index is low, calendar year 2001, Chen Jing academician as one of the present inventor proposes the New whole-wet technology that treasure mountain flotation concentrate is made directly oxygen pressure acidleach, the technology path of New whole-wet technology is: first flotation concentrate carries out oxygen pressure acidleach, make the Cu of > 99% in mineral aggregate, Ni, Co proceeds to solution with sulfate form, the Fe overwhelming majority in the process is hydrolyzed to bloodstone Fe2O3And goethitum FeO (OH) enters in slag; Slag rate be 50% oxygen pressure acid leaching residue carry out two-stage pressure cyanide, make platinum group metal proceed to cyanating solution with cyanogen complex anion form, can adopt zinc dust precipitation or active carbon adsorption that liquid after cyaniding is processed respectively, continue after carry out Refining of Platinum Metals. Unfortunately, zinc replacement need to first destroy the cyanogen root in solution to this technique, operates more complicated, and after displacement, the zinc in solution is difficult in return to utilize; And active carbon adsorption selectivity is not high, long flow path, direct yield is low. Adopt solvent extraction to extract palladium to have started to the eighties in last century abroad to apply to produce, domestic also achieved industrialization in recent years, but the extraction of palladium system set up is limited only to acid medium. In research alkaline cyanide liquid medium, the Extraction behavior of platinum group metal, sets up efficient extraction system, it is achieved platinum group metal is extracting directly from alkaline cyanide liquid, is an important problem of current platinum group metal metallurgy urgent need solution.
Summary of the invention
Present invention aim at setting up suitable solvent-extraction system, adopt solvent extraction method, the method can overcome the deficiency of zinc dust precipitation or active carbon adsorption, liquid after cyaniding is processed without destroying cyanogen root or enrichment, can from alkaline cyanide liquid direct extraction of palladium, effectively shorten the extracting cycle of palladium, reduce production cost.
It is an object of the invention to be achieved through the following technical solutions:
By dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium method of extraction of palladium from alkaline cyanide liquid, comprise the following steps:
(1) will containing [Pd (CN)4]2-The pH value of feed liquid regulates within the scope of 9.5-11.5, as the aqueous phase of extraction system;
(2) organic facies being made up of extractant, diluent, synergic reagent is prepared, wherein,
With dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium for extractant, this extractant concentration in organic facies is 0.01 ~ 0.03mol/L;
Choosing any one kind of them as synergic reagent in n-amyl alcohol or hexanol or n-heptanol or n-octyl alcohol or Decanol, synergic reagent volume occupies the 20-40% (V/V) of machine phase volume;
Choosing any one kind of them as diluent in benzene or dimethylbenzene or normal heptane or sulfonated kerosene, diluent volume is the surplus of extractant, synergic reagent;
(3) comparing (O/A) 11 ~ 13 with aqueous phase by organic facies and aqueous phase and organic facies are put into mixed phase in separatory funnel, stratification, by [Pd (CN)4]2-Transfer to organic facies from aqueous phase;
(4) taking above step (3) and extract the organic facies of back loading palladium, put in another separatory funnel, comparing (A/O) 11 ~ 12 addition concentration with organic facies by aqueous phase is the NH of 0.1 ~ 0.3mol/L4SCN solution, [Pd (CN) in back extraction organic facies4]2-��
Described method is furthermore that step (3) is to put into organic facies in separatory funnel and aqueous phase vibration 4-8 point of kind of mixed phase, stratification.
Described method is furthermore that step (4) is NH4[Pd (CN) in SCN solution back extraction organic facies4]2-The mixed phase time be 5-8 point of kind, stratification.
Described method is furthermore that step (3) and (4) are measuring point mutually the concentration of Pd in aqueous phase afterwards respectively, calculates extraction yield and the NH of dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium extraction Pd respectively with minusing4The back extraction ratio of SCN back extraction Pd.
The molecular formula of the dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium (being called for short DDPB) alleged by technique scheme is C22H40BrNO, relative molecular mass is 414.48, and structural formula is:
��
In above-mentioned steps (4), [Pd (CN) in organic facies4]2-Concentration is more high, added NH4SCN stripping workshop concentration is more high, added NH4SCN liquor capacity is more big, and A/O ratio is more big.
Above-mentioned substantive distinguishing features and progressive based on extraction experiments and result, including:
1, DDPB is extracted Pd (CN) by pH value4 2-The impact of performance
Under room temperature, fixing waiting extracts Pd (CN) in liquid4 2-Initial concentration be 99.3mg/L, in organic facies, the concentration of DDPB is 0.01mol/L, organic facies compares (O/A) 11 with aqueous phase, mechanical oscillation five minutes is extraction time t=5min, select benzene as the diluent of extraction system, n-octyl alcohol makes synergic reagent, containing 40% n-octyl alcohol (V in organic faciesN-octyl alcohol/VOrganic facies), organic facies cumulative volume is 10mL, and DDPB is extracted Pd (CN) by different pH value4 2-The impact of performance is as shown in table 1.
DDPB is extracted Pd (CN) by table 1.pH value4 2-The impact of performance
| PH value | 8.5 | 9.0 | 9.5 | 10.5 | 11.5 | 12.0 | 14.0 |
| Extraction yield E (%) | 87.4 | 91.6 | 96.5 | 97.2 | 96.4 | 92.2 | 86.8 |
2, the saturated loading capacity of DDPB measures:
Under room temperature, controlling solution ph is 11, and organic facies compares (O/A) 11, extraction time 5 minutes with aqueous phase, and fixing waiting extracts Pd (CN) in liquid4 2-Initial concentration be 99.3mg/L, select benzene as the diluent of extraction system, n-octyl alcohol makes synergic reagent, containing 40% n-octyl alcohol (V in organic faciesN-octyl alcohol/VOrganic facies), organic facies cumulative volume is 30mL, adopts sequential extractions to measure variable concentrations DDPB solution extraction Pd (CN)4 2-Saturated loading capacity.Variable concentrations DDPB solution extraction Pd (CN)4 2-Saturated loading capacity is as shown in table 2:
Table 2. variable concentrations DDPB solution extraction Pd (CN)4 2-Saturated loading capacity
| CDDPB(mol/L) | 0.01 | 0.02 | 0.03 | 0.04 | 0.05 | 0.06 |
| Saturated loading capacity (g/L) | 0.32 | 0.54 | 0.87 | 1.18 | 1.42 | 1.64 |
Test result indicate that: DDPB can from alkaline cyanide liquid quantified extract palladium, extract pH scope wide, saturated loading capacity is high, and pH value is in 9.5-11.5 scope, and effect of extracting is best.
The present invention has following substantive distinguishing features and progress:
1, can from alkaline cyanide liquid directly quantified extract palladium, overcome the deficiency of zinc dust precipitation or active carbon adsorption, it is not necessary to liquid after cyaniding is carried out enrichment process or cyanogen root destroys;
2, extracting required aqueous phase pH span wide, in suitable scope, directly the extraction yield of quantified extract palladium is more than 97%, and back extraction ratio is more than 96%;
3, extracting and back extraction kinetics speed is fast, namely several minutes reaches balance, with short production cycle;
4, except These characteristics, the adopted extractant DDPB of the present invention is or/and NH4SCN commodity price is cheap, and construction investment is little, and production cost is low, recoups the investment fast, and benefit space is big, is appropriate to the scale of chemical production, has popularizing application prospect.
In order to be more fully understood that the present invention, below by detailed description of the invention, the present invention is further described, but cited embodiment is not limiting as the scope of protection of the invention.
Detailed description of the invention
Embodiment 1
Take the Pd (CN) that Pd (II) concentration is 25.8mg/L4 2-Solution 60mL, in separatory funnel, regulates the solution ph 10.0 aqueous phase as extraction system. Preparation organic facies, wherein, organic facies cumulative volume is 20mL, and containing 4mL Decanol in organic facies, surplus is with dimethylbenzene for diluent, and in organic facies, the concentration of DDPB is 0.01mol/L. Organic facies adds aqueous phase (O/A=1 3), and mechanical oscillation is stratification after 5 minutes, divides and measures the concentration of palladium in aqueous phase mutually afterwards, and the concentration minusing of the palladium in organic facies is obtained. Taking the organic facies being loaded with palladium, put in another separatory funnel, comparing (A/O) 12 addition concentration with organic facies by aqueous phase is the NH of 0.1mol/L4SCN carries out back extraction, and mixed phase is stratification after 5 minutes, divides and measures the concentration of palladium in back extraction mutually mutually afterwards, and calculates NH4The back extraction ratio of SCN back extraction palladium, concrete data are in Table 3.
Embodiment 2
Take the Pd (CN) that Pd (II) concentration is 55.6mg/L4 2-Solution 40mL, in separatory funnel, regulates the solution ph 11.5 aqueous phase as extraction system. Preparation organic facies, wherein, organic facies cumulative volume is 20mL, and containing 5mL n-amyl alcohol in organic facies, surplus is with benzene for diluent, and in organic facies, the concentration of DDPB is 0.01mol/L. Organic facies adds aqueous phase (O/A=1 2), and mechanical oscillation is stratification after 4 minutes, divides and measures the concentration of palladium in aqueous phase mutually afterwards, and the concentration minusing of the palladium in organic facies is obtained. Taking the organic facies being loaded with palladium, put in another separatory funnel, comparing (A/O) 12 addition concentration with organic facies by aqueous phase is the NH of 0.1mol/L4SCN carries out back extraction, and mixed phase is stratification after 5 minutes, divides and measures the concentration of palladium in back extraction mutually mutually afterwards, and calculates NH4The back extraction ratio of SCN back extraction palladium, concrete data are in Table 3.
Embodiment 3
Take the Pd (CN) that Pd (II) concentration is 99.3mg/L4 2-Solution 20mL, in separatory funnel, regulates the solution ph 11.0 aqueous phase as extraction system. Preparation organic facies, wherein, organic facies cumulative volume is 20mL, and containing 6mL hexanol in organic facies, surplus is with normal heptane for diluent, and in organic facies, the concentration of DDPB is 0.01mol/L.Organic facies adds aqueous phase (O/A=1 1), and mechanical oscillation is stratification after 5 minutes, divides and measures the concentration of palladium in aqueous phase mutually afterwards, and the concentration minusing of the palladium in organic facies is obtained. Take the organic facies being loaded with palladium, put in another separatory funnel, compare (A/O) 11 with organic facies by aqueous phase and add 0.1mol/LNH4SCN carries out back extraction, and mixed phase is stratification after 5 minutes, divides and measures the concentration of palladium in back extraction mutually mutually afterwards, and calculates NH4The back extraction ratio of SCN back extraction palladium, concrete data are in Table 3.
Embodiment 4
Take the Pd (CN) that Pd (II) concentration is 199.8mg/L4 2-Solution 20mL, in separatory funnel, regulates the solution ph 10.5 aqueous phase as extraction system. Preparation organic facies, wherein, organic facies cumulative volume is 20mL, and containing 8mL n-heptanol in organic facies, surplus is with benzene for diluent, and in organic facies, the concentration of DDPB is 0.02mol/L. Organic facies adds aqueous phase (O/A=1 1), and mechanical oscillation is stratification after 6 minutes, divides and measures the concentration of palladium in aqueous phase mutually afterwards, and the concentration minusing of the palladium in organic facies is obtained. Take the organic facies being loaded with palladium, put in another separatory funnel, compare (A/O) 11 with organic facies by aqueous phase and add 0.2mol/LNH4SCN carries out back extraction, and mixed phase is stratification after 6 minutes, divides and measures the concentration of palladium in back extraction mutually mutually afterwards, and calculates NH4The back extraction ratio of SCN back extraction palladium, concrete data are in Table 3.
Embodiment 5
Take the Pd (CN) that Pd (II) concentration is 254.6mg/L4 2-Solution 20mL, in separatory funnel, regulates the solution ph 9.5 aqueous phase as extraction system. Preparation organic facies, wherein, organic facies cumulative volume is 20mL, and containing 8mL n-octyl alcohol in organic facies, surplus is with sulfonated kerosene for diluent, and in organic facies, the concentration of DDPB is 0.03mol/L. Organic facies adds aqueous phase (O/A=1 1), and mechanical oscillation is stratification after 8 minutes, divides and measures the concentration of palladium in aqueous phase mutually afterwards, and the concentration minusing of the palladium in organic facies is obtained. Take the organic facies being loaded with palladium, put in another separatory funnel, compare (A/O) 11 with organic facies by aqueous phase and add 0.3mol/LNH4SCN carries out back extraction, and mixed phase is stratification after 8 minutes, divides and measures the concentration of palladium in back extraction mutually mutually afterwards, and calculates NH4The back extraction ratio of SCN back extraction palladium, concrete data are in Table 3.
In table 3. alkaline cyanide liquid medium, DDPB extracts Pd situation
From table 3 it can be seen that dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium (DDPB) in the alkaline cyanide liquid medium that pH value is 9.5-11.5 to [Pd (CN)4]2-There are the extraction ability of excellence, NH4SCN can fine back extraction Pd.
Claims (5)
1. by dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium method of extraction of palladium from alkaline cyanide liquid, bag
Draw together following steps:
(1) will containing [Pd (CN)4]2-The pH value of feed liquid regulates within the scope of 9.5-11.5, as the aqueous phase of extraction system;
(2) organic facies being made up of extractant, diluent, synergic reagent is prepared, wherein,
With dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium for extractant, this extractant concentration in organic facies is 0.01 ~ 0.03mol/L;
Choosing any one kind of them as synergic reagent in n-amyl alcohol or hexanol or n-heptanol or n-octyl alcohol or Decanol, synergic reagent volume occupies the 20-40% (V/V) of machine phase volume;
Choosing any one kind of them as diluent in benzene or dimethylbenzene or normal heptane or sulfonated kerosene, diluent volume is the surplus of extractant, synergic reagent;
(3) comparing (O/A) 11 ~ 13 with aqueous phase by organic facies and aqueous phase and organic facies are put into mixed phase in separatory funnel, stratification, by [Pd (CN)4]2-Transfer to organic facies from aqueous phase;
(4) taking above step (3) and extract the organic facies of back loading palladium, put in another separatory funnel, comparing (A/O) 11 ~ 12 addition concentration with organic facies by aqueous phase is the NH of 0.1 ~ 0.3mol/L4SCN solution, [Pd (CN) in back extraction organic facies4]2-��
2. method according to claim 1, it is characterised in that step (3) is to put into organic facies in separatory funnel and aqueous phase vibration 4-8 point of kind of mixed phase, stratification.
3. method according to claim 1 and 2, it is characterised in that step (4) is NH further4[Pd (CN) in SCN solution back extraction organic facies4]2-The mixed phase time be 5-8 point of kind, stratification.
4. method according to claim 1 and 2, it is characterised in that step (3) and (4) point are measuring the concentration of Pd in aqueous phase mutually afterwards respectively, calculate extraction yield and the NH of dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium extraction Pd respectively with minusing4The back extraction ratio of SCN back extraction Pd.
5. method according to claim 3, it is characterised in that step (3) and (4) point are measuring the concentration of Pd in aqueous phase mutually afterwards respectively, calculate extraction yield and the NH of dodecyl dimethyl-2-benzene oxygen ethyl phosphonium bromide ammonium extraction Pd respectively with minusing4The back extraction ratio of SCN back extraction Pd.
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| CN1912156A (en) * | 2006-08-23 | 2007-02-14 | 暨南大学 | Method for extracting gold (I) from enriched alkaline cyanide gold immersing liquid |
| CN102417981A (en) * | 2011-11-22 | 2012-04-18 | 中国科学院过程工程研究所 | Method for extracting and separating platinum, palladium and rhodium by using ionic liquid-based three-liquid phase system |
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| CN1912156A (en) * | 2006-08-23 | 2007-02-14 | 暨南大学 | Method for extracting gold (I) from enriched alkaline cyanide gold immersing liquid |
| CN102417981A (en) * | 2011-11-22 | 2012-04-18 | 中国科学院过程工程研究所 | Method for extracting and separating platinum, palladium and rhodium by using ionic liquid-based three-liquid phase system |
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| 十二烷基三甲基氯化铵从碱性氰化液中固相萃取金的研究;解润芳等;《稀有金属》;20140131;第38卷(第1期);165-170 * |
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