CN101584979A - The inverse bonded extraction column of polymer and use the method for this post extracting gold from alkaline cyanide liquid - Google Patents
The inverse bonded extraction column of polymer and use the method for this post extracting gold from alkaline cyanide liquid Download PDFInfo
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- CN101584979A CN101584979A CNA2009100946351A CN200910094635A CN101584979A CN 101584979 A CN101584979 A CN 101584979A CN A2009100946351 A CNA2009100946351 A CN A2009100946351A CN 200910094635 A CN200910094635 A CN 200910094635A CN 101584979 A CN101584979 A CN 101584979A
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Abstract
The present invention relates to the inverse bonded extraction column of a kind of polymer and the method for extracting gold in alkaline cyanide liquid.High molecular polymer is that the bonding groups forms on the stromal surface the inverse bonded material of polymer is as solid phase extraction column stuffing.Mol ratio in quaternary ammonium cation CTMAB and golden Au in the alkaline cyanide liquid is 1: 1-3: 1 ratio adds quaternary ammonium cation CTMAB and makes working solution; Regulating working solution pH is 9.4-14; Working solution is carried by the inverse bonded solid-phase extraction column of polymer with pump, and the gold ion associated matter that aurum cyanogen anionic complex in the working solution and quaternary ammonium cation CTMAB generate is extracted post absorption; The reach capacity gold ion associated matter of available ethanol eluate desorb extraction on-column enrichment behind the state of absorption.The present invention uses the inverse bonded material filling of polymer extraction column, this filler is compared with bonded silica gel, the pH wide ranges that is suitable for, can under alkali condition, stablize use, be fit to the working environment of extracting gold from alkaline cyanide liquid, golden extraction efficiency greatly improves, and the single extraction rate of gold surpasses 95%, the enrichment multiple is up to 200-500 times, and golden loading capacity is greater than 16mg/g.
Description
Technical field
The invention belongs to technical field of wet metallurgy, be specifically related to the inverse bonded extraction column of a kind of polymer and use the method for this post extracting gold from alkaline cyanide liquid.
Background technology
Cyaniding is to extract the economy of gold and easy method from ore, concentrate or mine tailing, and it has, and cost is low, gold recovery is high, to series of advantages such as ore adaptability are strong, and therefore up to the present it is still at home and abroad occupied an leading position in the process for extracting gold.From the treatment process of cyaniding leachate enrichment gold, adopt traditional zinc replacement or charcoal absorption at present mostly.Because these two kinds of methods are not high enough to the selectivity of gold, the gold mud that is obtained (intermediate products) also needs to cause the production cycle long through complicated follow-up refining treatment, and environmental pollution increases, cost up.Because solvent extraction can overcome above-mentioned shortcoming, since the eighties in last century, directly extracting gold becomes the focus that domestic and international scientific worker studies from alkaline cyanide liquid.But Au (CN) 2-can only be in weak alkaline medium (pH＞9.4) stable existence.Therefore except that the QUATERNARY AMMONIUM SALT system, the practical application effect of other extraction system is all not good enough.People such as Chen Jing are in the begin one's study method of from alkaline cyanide liquid extracting gold of nineteen ninety-five, and proposed earlier to add water at 1: 1 by mol ratio with gold with surfactant cetab (CTMAB), extract the new extraction system of Au (CN) 2-then with the TBP of sulfonated kerosene dilution, but find in the process of the test because gold concentration is too low, even adopted custom-designed three grades of pillars extraction, the commercial Application of liquid-liquid extraction still has certain difficulty.Solid phase extraction techniques is a kind of enrichment and the isolation technics that fast development is in recent years got up.Because the advantage that solid phase extraction techniques is outstanding, they are example enrichment and pre-separation in analytical chemistry, and a plurality of industries such as the separation of medicine and purifying have all obtained extensive use, and wherein most widely used is anti-phase SPE.Anti-phase solid-phase extraction column extracting gold from alkaline cyanide liquid of prior art because the pH scope that its reversed-phase bonded silica material uses is narrower, uses work materials easily to lose efficacy in alkaline solution, and therefore extracting gold just can't realize from alkaline cyanide liquid.The inventor is through long-term practice research for this reason, developed a kind of polymer-bound reversed material and be the solid-phase extraction column of filler and from alkaline cyanide liquid the method for extracting gold, obtained good test effect.
Summary of the invention
First purpose of the present invention is to provide a kind of inverse bonded solid-phase extraction column of polymer that is applicable to the high efficiency extracting gold of alkaline solution.
Another object of the present invention is to provide a kind of method of utilizing the inverse bonded solid-phase extraction column of polymer extracting gold from alkaline cyanide liquid.
First purpose of the present invention is achieved in that with the high molecular polymer to be matrix, form polymer antibonding condensation material at its surface bond groups, described high molecular polymer be in the cross-linked polymer of polystyrene, polydivinylbenezene, polystyrene-divinylbenzene base any one or more than one; Described groups is C
2, C
4, C
8, C
18, C
22Alkyl in any one or more than one.
Another object of the present invention is achieved in that specifically and comprises: the mol ratio in quaternary ammonium cation CTMAB and golden Au in the alkaline cyanide liquid is 1: 1-3: 1 ratio adds quaternary ammonium cation CTMAB and makes working solution; Regulating working solution pH is 9.4-14; Working solution is carried by the inverse bonded solid-phase extraction column of polymer with pump, and the gold ion associated matter that aurum cyanogen anionic complex in the working solution and quaternary ammonium cation CTMAB generate is extracted post absorption; The reach capacity gold ion associated matter of available ethanol eluate desorb extraction on-column enrichment behind the state of absorption.
About loading capacity.Loading capacity (the milligram number of every gram filler energy extracting gold) is the important parameter of balancing method actual application value, and loading capacity is high more, the Jin Yueduo of each operation energy enrichment, and operating efficiency is high more.In order to take into account practical application in industry, sum up extraction and amplify the influence rule of back to loading capacity, the inventor is to 8mm diameter * 10mm column length, and the common solid phase extraction column of filling material 0.5g amplifies, made 12mm diameter * 15mm column length respectively, filling material 1.7g; 16mm diameter * 20mm column length, filling material 4.1g; 20mm diameter * 25mm column length, filling material 7.8g; 40mm diameter * 50mm column length, the solid-phase extraction column of filling material 63g.With gold concentration is 1.0 * 10
-5Mol/L, 5.0 * 10
-5Mol/L, 2.0 * 10
-4The solution of mol/L is crossed post, under the condition of guaranteeing recovery of extraction 〉=95%, has measured loading capacity, the results are shown in Table-1.Can find out from table-1 data, for three concentration being tested, with the increase of amount of filler, the proportional increase of extraction quantity of gold.It is constant that loading capacity keeps substantially.
Table-1 amount of filler is to the influence of golden extraction quantity and loading capacity
Amplify about flow velocity.Experimental result shows:, filling tight ness rating identical extraction column identical for filler, and under uniform pressure, when column length fixedly the time, the mistake column flow rate increases progressively with the increase of post cross-sectional area; When post cross-sectional area fixedly the time, cross column flow rate with the increase of column length linear decrease, correlation is:
Along with post amplifies, on-column enrichment gold amount amount increases, and the volume of required eluent also increases, and linear substantially, crosses column flow rate and elution flow rate in the practical application and can amplify by this rule.。
About of the influence of column length/diameter to concentration effect.With diameter is the extraction column that the polypropylene needle tubing of 10mm has loaded different length: 1.0mm diameter * 0.25m column length, filling material 0.28g; 1.0mm diameter * 0.5m column length, filling material 0.54g; 1.0mm diameter * 1.0m column length, filling material 1.1g; 1.0mm diameter * 1.5m column length, filling material 1.62g; 1.0mm diameter * 2.0m column length, filling material 2.3g; 1.0mm diameter * 5.0m column length, filling material 6.2g:1.0mm diameter * 10mm column length, the 11.8g filler is expected in filling, and has measured the loading capacity of different size post.Column length is seen Fig. 2 to the influence of loading capacity.
The above results shows: (1) increases with the extraction column amount of filler, and the extraction column extraction quantity increases, and loading capacity remains unchanged substantially.(2) amplify the back cross column flow rate with the increase of post cross-sectional area linear increment; When post cross-sectional area fixedly the time, cross column flow rate with the increase of column length linear decrease.(3) when the wash-out gold, with the expansion of post, enrichment gold amount increases, and the volume of required eluent also increases, and is linear substantially.(4) for the post of different size, the diameter/length of extraction column is than in 1/1 maximum of loading capacity between 1/2 time, and after extraction column amplified, the diameter/length ratio of post should be controlled in this scope, to keep the filler optimum rate of utilization.
Because the present invention uses the inverse bonded material filling of polymer extraction column, this filler is compared with bonded silica gel, and the pH wide ranges that is suitable for can be stablized use under alkali condition, be suitable for the working environment of extracting gold from alkaline cyanide liquid, and extraction efficiency greatly improves.
Description of drawings
Fig. 1 is the relation of golden enriching quantity and eluent consumption.
Fig. 2 is the relation of diameter/column length to loading capacity.
The specific embodiment
The invention will be further elaborated below in conjunction with specific embodiment, is interpreted as these embodiment and only is used to the present invention is described and is not used in and limit the scope of the invention.Be interpreted as in addition after the content of having read the present invention's instruction, those skilled in the art can make various changes or modifications the present invention, and these are changed and fall within the protection domain that the application's claims are limited equally.
The inverse bonded solid-phase extraction column of polymer of the present invention is to be that polymer antibonding condensation material that stromal surface bonding groups forms is a filler with the high molecular polymer.Described high molecular polymer be in the cross-linked polymer of polystyrene, polydivinylbenezene, polystyrene-divinylbenzene base any one or more than one; Described groups is C
2, C
4, C
8, C
18, C
22Alkyl in any one or more than one.
Utilize the method for the inverse bonded solid-phase extraction column of polymer solid-phase extraction of gold from alkaline cyanide liquid, comprised post enrichment, the washing of carrying principal column, the elution step of carrying principal column specifically comprises:
Mol ratio in quaternary ammonium cation CTMAB and golden Au in A, the alkaline cyanide liquid is 1: 1-3: 1 ratio adds quaternary ammonium cation CTMAB and makes working solution;
B, adjusting working solution pH are 9.4-14;
C, working solution is carried by the inverse bonded solid-phase extraction column of polymer with pump, the gold ion associated matter that the aurum cyanogen anionic complex in the working solution and quaternary ammonium cation CTMAB generate is extracted post and adsorbs;
The reach capacity gold ion associated matter of available ethanol eluate desorb extraction on-column enrichment behind the state of D, absorption.
Described quaternary ammonium cation CTMAB be in cetrimonium bromide, chlorination myristyl trimethyl ammonium, chlorination cetyl benzyl ammonium ammonium, the cetylpyridinium chloride any one or more than one.
The inverse bonded solid phase extraction column stuffing of polymer be on the polystyrene substrate bonding be that the charcoal atomicity is C
2, C
4, C
8, C
18, C
22Alkyl in any.Solid-phase extraction column 8mm diameter * 10mm column length, with the ethanol activation, water flush away ethanol promptly can be used for the extraction of gold more earlier.Compound concentration is 1.0 * 10
-5～2.0 * 10
-4KAu between the mol/L (CN)
2Solution is regulated its pH 10.4, and is that 1: 2 ratio adds CTMAB in CTMAB: Au (I) mol ratio, and this solution is as treating extract.Treat during extraction that extract delivers into extraction column by pump, treat that it is that 2.5L enters saturation state that extract is crossed column volume, carry eluent ethanol 5mL, activated solution ethanol 10mL, oppositely extraction column is carried out wash-out, activation, again by residual ethanol on the pump transporting water flush away post.The enrichment multiple can reach 500 times under this condition, and the rate of recovery of gold reaches 96.2%.
The inverse bonded solid phase extraction column stuffing of polymer be on the polydivinylbenezene matrix bonding be that the charcoal atomicity is C
2, C
4, C
8, C
18, C
22Alkyl in any.Solid-phase extraction column 16mm diameter * 20mm column length, filling material 4.1g.With the ethanol activation, water flush away ethanol promptly can be used for the extraction of gold earlier.Compound concentration is 2.0 * 10
-5The KAu of mol/L (CN)
2Solution is regulated its pH 11.8, and is that 1: 1.5 ratio adds CTMAB in CTMAB: Au (I) mol ratio, and this solution is as treating extract.Treat during extraction that extract delivers into extraction column by pump, treat that it is that 10L enters saturation state that extract is crossed column volume, carry eluent ethanol 25mL, activated solution ethanol 25mL, oppositely extraction column is carried out wash-out, activation, again by residual ethanol on the pump transporting water flush away post.But enrichment multiple Da Keda is 400 times under this condition, and the rate of recovery of gold reaches 95.4%.
Embodiment 3
The inverse bonded solid phase extraction column stuffing of polymer be on the crosslinked polymer matrix of polystyrene-divinylbenzene base bonding be that the charcoal atomicity is C
2, C
4, C
8, C
18, C
22Alkyl in any.Solid-phase extraction column 40mm diameter * 50mm column length, filling material 63.5g; With the ethanol activation, water flush away ethanol promptly can be used for the extraction of gold more earlier.Compound concentration is 5.0 * 10
-5The KAu of mol/L (CN)
2Solution is regulated its pH 12.4, and is that 1: 1.5 ratio adds CTMAB in CTMAB: Au (I) mol ratio, and this solution is as treating extract.Treat during extraction that extract delivers into extraction column by pump, treat that it is that 40L enters saturation state that extract is crossed column volume, carry eluent ethanol 200mL, activated solution ethanol 100mL, oppositely extraction column is carried out wash-out, activation, again by residual ethanol on the pump transporting water flush away post.But enrichment multiple Da Keda is 100 times under this condition, and the rate of recovery of gold reaches 98.5%.
The inverse bonded solid phase extraction column stuffing of polymer be on the crosslinked polymer matrix of polystyrene-divinylbenzene base bonding be that the charcoal atomicity is C
2, C
4, C
8, C
18, C
22Alkyl in any.Actual mine feed liquid is picked up from Dali Midu gold mine, and the gold content in the feed liquid is 5.73 μ g/mL, and silver content is 3.62 μ g/mL, nickel content is 0.475 μ g/mL, and copper content is 0.631 μ g/mL, and zinc content is 46.12 μ g/mL, iron content is 0.638 μ g/mL, and cobalt content is 0.256 μ g/mL.The mine feed liquid adopts 8mm diameter * 10mm column length respectively, filling material 0.5g; 12mm diameter * 15mm column length, filling material 1.7g; 16mm diameter * 20mm column length, filling material 4.1g; 20mm diameter * 25mm column length, filling material 7.8g; 40mm diameter * 50mm column length, the extraction column of filling material 63g extracts.Measure loading capacity respectively, the results are shown in Table-2.-2 can find out that from table to actual mine feed liquid, the expansion with post enlarges extraction column to the extraction quantity of gold, the loading capacity of gold has minimizing slightly with the expansion of post, rule with test with the solution extraction of single gold in resulting rule identical.But and single gold (KAu (CN)
2) solution extraction compares, the loading capacity of gold significantly reduces in the extraction of actual mine feed liquid, and the loading capacity of each specification post has all descended more than 2.0 times, illustrates that coexisting ion during actual mine material is has also produced influence to the extraction of gold extraction.Enrichment on our coupled columns has been carried out wash-out, merges eluent and has measured the composition of gold mud.The content of each element is respectively in the gold mud: gold 13.68%, silver 6.07%, zinc 11.51%, nickel 0.44%, copper 0.55%, iron 0.06%, cobalt 0.16% illustrate that several coexistence elements all are extracted with gold, but extraction column still keeps higher loading capacity to gold.
Table-2 different size posts are to the extraction of gold in the actual feed liquid
| The extraction column specification | 8mm×10 mm | 12mm× 15mm | 16mm× 20mm | 20mm× 25mm | 40mm×50 mm |
| Dress amount of filler (g) | 0.51 | 1.7 | 4.1 | 17.8 | 63.5 |
| Actual extraction amount (mg) loading capacity (mg) | 4.63 9.07 | 13.02 7.66 | 27.9 6.81 | 117.4 6.60 | 402.5 6.34 |
Claims (3)
1, the inverse bonded solid-phase extraction column of a kind of polymer, with the high molecular polymer is matrix, form polymer antibonding condensation material at its surface bond groups, it is characterized in that: described high molecular polymer be in the cross-linked polymer of polystyrene, polydivinylbenezene, polystyrene-divinylbenzene base any one or more than one; Described groups is C
2, C
4, C
8, C
18, C
22Alkyl in any one or more than one.
2, a kind of method of utilizing the SPE from alkaline cyanide liquid of the inverse bonded solid-phase extraction column of the described polymer of claim 1 to carry gold comprised post enrichment, the washing of carrying principal column, and the elution step of carrying principal column specifically comprises:
Mol ratio in quaternary ammonium cation CTMAB and golden Au in A, the alkaline cyanide liquid is 1: 1-3: 1 ratio adds quaternary ammonium cation CTMAB and makes working solution;
B, adjusting working solution pH are 9.4-14;
C, working solution is carried by the inverse bonded solid-phase extraction column of polymer with pump, the gold ion associated matter that the aurum cyanogen anionic complex in the working solution and quaternary ammonium cation CTMAB generate is extracted post and adsorbs;
The reach capacity gold ion associated matter of available ethanol eluate desorb extraction on-column enrichment behind the state of D, absorption.
3, the SPE from alkaline cyanide liquid of the inverse bonded solid-phase extraction column of polymer as claimed in claim 2 carry the gold method, it is characterized in that: described quaternary ammonium cation CTMAB be in cetrimonium bromide, chlorination myristyl trimethyl ammonium, chlorination cetyl benzyl ammonium ammonium, the cetylpyridinium chloride any one or more than one.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457336A (en) * | 2014-09-04 | 2016-04-06 | 中国科学院大连化学物理研究所 | Solid-phase extraction method for copper ions |
| CN112007622A (en) * | 2015-07-27 | 2020-12-01 | 第六波创新公司 | Molecularly imprinted polymer beads for metal extraction and uses thereof |
-
2009
- 2009-06-23 CN CNA2009100946351A patent/CN101584979A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105457336A (en) * | 2014-09-04 | 2016-04-06 | 中国科学院大连化学物理研究所 | Solid-phase extraction method for copper ions |
| CN105457336B (en) * | 2014-09-04 | 2017-05-17 | 中国科学院大连化学物理研究所 | Solid-phase extraction method for copper ions |
| CN112007622A (en) * | 2015-07-27 | 2020-12-01 | 第六波创新公司 | Molecularly imprinted polymer beads for metal extraction and uses thereof |
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