CN104888969B - Nonferrous metal ore flotation collecting agent with mercapto-oximido structure and application thereof - Google Patents
Nonferrous metal ore flotation collecting agent with mercapto-oximido structure and application thereof Download PDFInfo
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- CN104888969B CN104888969B CN201510201017.8A CN201510201017A CN104888969B CN 104888969 B CN104888969 B CN 104888969B CN 201510201017 A CN201510201017 A CN 201510201017A CN 104888969 B CN104888969 B CN 104888969B
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Abstract
The invention discloses a nonferrous metal ore flotation collecting agent with a mercapto-oximido structure and the application thereof. The flotation collecting agent has a mercapto group and an oximido group and is used as nonferrous metal ore flotation collecting agent for flotation separation, so nonferrous metallic minerals in nonferrous metal ore can be highly efficiently recycled. Thus, it is achieved that one kind of flotation collecting agent is capable of simultaneously recycling sulfide minerals and oxide minerals in nonferrous metal ore, and recycling rate of nonferrous metal minerals in nonferrous metal ore is greatly increased. The nonferrous metal ore flotation collecting agent is especially suitable for recycling of nonferrous metal of mixed minerals containing sulfide minerals and oxide minerals simultaneously, recycling processes of nonferrous metal are simple, highly practical and practicably, and industrially application requirements are met.
Description
Technical field
The present invention relates to a kind of nonferrous metals ore flotation collector with sulfydryl-oximido new structure and its have coloured gold
Application in category mineral floating, belongs to metalliferous mineral flotation technology field.
Background technology
Flotation is the main method that metalliferous mineral is reclaimed from metallic ore, and flotation collector is then that floatation separation is carried
Take one of key technology of valuable mineral component.Flotation collector directly affects mineral surfaces in the adsorption of mineral surfaces
Hydrophobicity and floatation process.Research and development collecting agent composition for flotation of coal, improves the hydrophobicity of mineral grain, for raising metal synthetical recovery
Rate has important function.
Thiol compound is the good collecting agent of sulfide mineral, and oximido class compound has good collecting to oxide mineral
Performance.Conventional sulfydryl class collecting agent has sulfur nitrogen (dithiocar-bamate), xanthate (dithiocarbonate), black powder (two hydrocarbon
Base dithiophosphatess), these sulfydryl collecting agent, particularly xanthate are the general collecting agents of metal sulfide ore, with collecting
The characteristics of ability is strong, selectivity is good.Oximido class compound is cupric oxide ore, cassiterite, Rare Earth Mine, iron mine, bauxite, tungsten ore, titanium
The oxide mineral collecting agent such as iron mine, nickel minerals, zinc ore.(publication number CN103301951A, " 2- ethyl -2- hexene aldoximes are in ore deposit for patent
Application process in thing flotation ", Zhong Hong, Haifeng Xu, Wang Shuai, Huang Zhiqiang, Liu Guangyi, Cao Zhanfang, 2013 years Septembers 18 of publication date
Day) application process of the 2- ethyl -2- hexene aldoximes in mineral floating is disclosed, the collecting agent is to copper-sulphide ores, vulcanization-oxidization
Copper mine, tungsten ore and cassiterite have good collecting ability.Document [Nagaraj, D.R.and
P.Somasundaran.Commercial chelating extractants as collectors:flotation of
Copper minerals using LIX reagents, Trans.AIME, 266, pp.1892 (1979) .] report, by
Nagaraj and Somasundaran has found Lix65N (trans -2- hydroxyls -5- nonylbenzophenone oximes) and Lix63 (5,8- diethyls
Base -7- hydroxy-dodecanoic base -6- oximes) there is good collecting to act on to cuprite, black copper ore (tenorite) and chrysocolla.Separately
Outward, document [A.P.Washington.Hydroxyoximes and their use in flotation, Minerals,
1988,43 (182), 46-50.] in Washington think that alkyl salicylaldoxime is the good collecting agent of Copper Ores direct flotation,
Document [D.W.Fuerstenau, R.Herrera-Urbina, D.W.McGlashan.Studies on the
applicability of chelating agents as universal collectors for copper
Minerals.International Journal of Mineral Processing, 2000,58,15-33.] in,
Fuerstenau etc. has commented on the adaptability of Chelating Collectors flotation copper mineral, show that Saldox. is the effective of copper oxide mineral
Collecting agent.
But most flotation collecting medicaments of the prior art are individually for the sulphide ore in nonferrous metallic ores
Thing or oxide mineral research and development, it is impossible to while effectively collecting sulfide mineral or oxide mineral, particularly pair simultaneously containing rich
The mixing nonferrous metallic ores of sulfur-richization and oxide mineral, reclaim difficult, cause the wasting of resources.
The content of the invention
For the defect that non-ferro metals floatation collecting agent of the prior art is present, it is offer one that the purpose of the present invention is
The collecting agent composition for flotation of coal with mercapto groups and oximido group is planted, the flotation collector can efficient flotation separation collecting simultaneously point
Extracting sulfide minerals of nonferrous and oxide mineral in nonferrous metallic ores, be particularly well-suited to simultaneously flotation collecting contain sulfuration and
The efficient flotation separation of the non-ferrous metal in the Ores such as oxidation mixed copper, nickel, zinc is reclaimed.
It is to provide the nonferrous metals ore flotation collecting with sulfydryl-oximyl structure that another object of the present invention is
The application of Non-ferrous minerals is reclaimed in agent flotation in nonferrous metallic ores, is particularly well-suited to vulcanize and aoxidize non-ferrous metal mixing
The high efficiente callback of the non-ferrous metal in mineral.
In order to realize the technical purpose of the present invention, the technical scheme is that what is be accomplished by：
The invention provides a kind of nonferrous metals ore flotation collector with sulfydryl-oximyl structure, the nonferrous metals ore
Flotation collector has formula I or formula II or formula III structure：
Wherein,
R1、R2、R5And R6It is each independently selected from C2～C12Alkyl；
R3For C1～C12Alkylene；
R4For hydrogen atom or C1～C12Alkyl.
In the preferred nonferrous metals ore flotation collector with sulfydryl-oximyl structure, R1、R2、R5And R6Independently of one another
Selected from C2～C12Alkyl；R3For C1～C12Alkylene alkyl or alkylene；R4For hydrogen atom or C1～C12Alkyl.
More preferably in the nonferrous metals ore flotation collector with sulfydryl-oximyl structure, R1、R2、R5And R6It is each independent
Ground is selected from ethyl, propyl group, isopropyl, butyl, isobutyl group, sec-butyl, amyl group, isopentyl, neopentyl, n-hexyl, isohesyl, just
Octyl group, iso-octyl or secondary octyl.Preferred R1、R2、R5And R6Sulfydryl-oximido knot is more beneficial for for length than convenient alkyl
The nonferrous metals ore flotation collector of structure improves the hydrophobicity and its dispersive property in the slurry of mineral grain.
More preferably in the nonferrous metals ore flotation collector with sulfydryl-oximyl structure, R3For methylene.R3For methylene
Base is more beneficial for the collaboration chelation between sulfydryl and oximido, all has suction to the sulfide and/or oxide of non-ferrous metal
Attached effect.
More preferably there is R in the nonferrous metals ore flotation collector of sulfydryl-oximyl structure4For hydrogen atom or methyl.
Present invention also offers the application of the described nonferrous metals ore flotation collector with sulfydryl-oximyl structure, will
Nonferrous metals ore flotation collector with sulfydryl-oximyl structure is applied to the non-ferrous metal in flotation collecting nonferrous metallic ores
Mineral.
Preferred application process is carried out in ore grinding and/or floatation process in nonferrous metallic ores, and addition is included with mercapto
The nonferrous metals ore flotation collector of base-oximyl structure is after interior floating agent is sized mixing then floating by foam flotation method
Select Non-ferrous minerals.
In preferred application process, nonferrous metallic ores be oxidation-copper sulfide composite ore, oxidation-zinc sulfide composite ore or
Oxidation-nickel sulfide composite ore.
The metallic ore flotation routinely of the nonferrous metals ore flotation collector with sulfydryl-oximyl structure of the present invention
The consumption of floating agent needed for journey is added.
The process of the flotation nonferrous metallic ores of the present invention is existing maturation process.
The nonferrous metals ore flotation collector with sulfydryl-oximyl structure of the present invention can be obtained by the following method：
By the halo aldoxime or ketoxime of formula IV structure and the dithiocar-bamate or the Huang of the structure of formula VI of the structure of formula V
The dithiophosphatess of ortho acid salt or the structure of formula VII carry out substitution reaction, halo aldoxime or ketoxime and dithiocar-bamate,
The ratio of the amount of the material of xanthates or dithiophosphatess is 1:0.8～2, reaction temperature is -20 DEG C～50 DEG C, the response time
For 0.5～8 hour, the nonferrous metals ore flotation collector with sulfydryl-oximyl structure such as formula I or formula II or formula III is generated；
Wherein, R3For C1～C12Alkylene；R4For hydrogen atom or C1～C12Alkyl；X is F-、Cl-、Br-Or I-；R1、
R2、R5And R6It is each independently selected from C2～C12Alkyl；M is Na+、K+Or NH4 +。
The halo aldoxime or ketoxime, the dithiocar-bamate of the structure of formula V, the structure of formula VI of the formula IV structure of the present invention
Xanthates, the dithiophosphatess of the structure of formula VII be that conventional raw material can be obtained according to existing maturation method, or
Directly it is commercially available.
Hinge structure, the invention has the beneficial effects as follows：Obtain a kind of simultaneously with mercapto groups and oximido base first
The flotation collector of group, and realize list in the FLOTATION SEPARATION of nonferrous metals ore as nonferrous metals ore collectors application
Plant sulfide and oxide mineral that floating agent is reclaimed in nonferrous metallic ores simultaneously.The flotation collector has sulfydryl simultaneously
Functional group and oximido functional group, the collaboration chelated metal ions ability between Liang Zhong functional groups strengthens, and can strengthen simultaneously to having
The sulfide mineral of non-ferrous metal and the adsorption of oxide mineral interface metal ion, considerably increase in nonferrous metallic ores
The response rate of Non-ferrous minerals, is particularly well-suited to the mixed mineral of the sulfide mineral containing non-ferrous metal and oxide mineral simultaneously
Recovery.Nonferrous metals recycling process is simple, efficient, practical, meets commercial Application requirement.
Description of the drawings
【Fig. 1】The infrared spectrum of the N obtained in embodiment 1, N- dibutyl dithiocaarbamate acetone oxime；
【Fig. 2】The infrared spectrum of the N obtained in embodiment 2, N- dibutyl dithiocaarbamate aldoxime；
【Fig. 3】The infrared spectrum of O- isobutyl groups xanthic acid acetone oxime obtained in embodiment 3；
【Fig. 4】The infrared spectrum of the O obtained in embodiment 4, O '-dibutyl dithio triosephosphate oxime.
Specific embodiment
The following example is intended to further illustrate present invention, but the scope of the claims in the present invention protection not by concrete
The restriction of embodiment.
Unless otherwise specified all of parts and percentages refer both to quality in embodiment.
Embodiment 1
The preparation of N, N- dibutyl dithiocaarbamate acetone oxime：
By 15.63 parts of N, N- NB sodium dibutyl dithiocarbamates add under agitation 6.72 parts of chlorine third that temperature is 20 DEG C
In ketoxime, the mixed solution of 36 parts of methanol, after adding at 20 DEG C stirring reaction 2h.Filter, filtrate water after vacuum distillation
Elution is pure to obtain white solid, as N, N- dibutyl dithiocaarbamate acetone oximes.Yield is 95%.Product Infrared Characterization
As shown in Figure 1.
Embodiment 2
The preparation of N, N- dibutyl dithiocaarbamate aldoxime：
By 15.63 parts of N, N- NB sodium dibutyl dithiocarbamates add under agitation 4.68 parts of chloroethenes that temperature is 20 DEG C
In aldoxime, the mixed solution of 36 parts of methanol, after adding at 20 DEG C stirring reaction 2h.Filter, filtrate water after vacuum distillation
Wash and be dried to obtain dark red oil, as N, N- dibutyl dithiocaarbamate aldoxime.Yield is 96%.Product is red
It is outer to characterize as shown in Figure 2.
Embodiment 3
The preparation of O- isobutyl group xanthic acid acetone oximes
17.2 parts of sodium isobutyl xanthans are added under agitation the 10.75 parts of chlroacetone oximes, 36 parts of first that temperature is 20 DEG C
In the mixed solution of alcohol, after adding at 20 DEG C stirring reaction 2h.Filter, filtrate is washed purification after vacuum distillation and obtains white
Color solid, as O- isobutyl groups xanthic acid acetone oxime.Yield is 90%.Product Infrared Characterization is as shown in Figure 3.
Embodiment 4
O, O '-dibutyl dithio triosephosphate oxime preparation：
By 22.8 parts of O, O '-ammonium dibutyl dithiophosphate adds under agitation 10.75 parts of chlroacetones that temperature is 20 DEG C
In oxime, the mixed solution of 36 parts of methanol, after adding at 20 DEG C stirring reaction 2h.Filter, filtrate is washed after vacuum distillation
It is dried to obtain pale yellow oily liquid, as O, O '-dibutyl dithio triosephosphate oxime.Yield is 94%.The infrared table of product
Levy as shown in Figure 4.
It is the nonferrous metals ore flotation collecting with sulfydryl-oximyl structure prepared using embodiment 1～4 to implement 5～13
Agent is applied to the flotation collecting of Non-ferrous minerals.
Embodiment 5
Flotation of N, the N- dibutyl dithiocaarbamate acetone oxime to Chalkopyrite：
In N, N- dibutyl dithiocaarbamates acetone oxime is 5 × 10-5Mol/L, pH values of pulp is 8～9, N2Gas velocity is
200mL/min, is the Chalkopyrite flotation of -0.076mm～+0.038mm 3 minutes to particle diameter, now the flotation recovery rate of Chalkopyrite
Reach 87.71%.
Embodiment 6
Flotation of N, the N- dibutyl dithiocaarbamate acetone oxime to malachite：
In N, N- dibutyl dithiocaarbamate acetone oximes concentration is 5 × 10-5Mol/L, pH values of pulp is 8～9, N2Air-flow
Speed is 200mL/min, is the malachite flotation of -0.076mm～+0.038mm 3 minutes to particle diameter, and the now flotation of malachite is returned
Yield is 81.40%.
Embodiment 7
Flotation of the O- isobutyl group xanthic acid acetone oximes to Chalkopyrite：
It is 5 × 10 in O- isobutyl group xanthic acid acetone oximes concentration-5Mol/L, pH values of pulp be 8～9, foaming agent (MIBC) it is dense
Spend for 15mg/L, N2Gas velocity is 200mL/min, is the Chalkopyrite flotation of -0.076mm～+0.038mm 3 minutes to particle diameter, this
When Chalkopyrite flotation recovery rate be 84.35%.
Embodiment 8
Flotation of the O- isobutyl group xanthic acid acetone oximes to malachite：
It is 3 × 10 in O- isobutyl group xanthic acid acetone oximes concentration-4Mol/L, pH values of pulp be 8～9, foaming agent (MIBC) it is dense
Spend for 15mg/L, N2Gas velocity is 200mL/min, is the malachite flotation of -0.076mm～+0.038mm 3 minutes to particle diameter, this
When malachite flotation recovery rate be 81.68%.
Embodiment 9
O, O '-flotation of the dibutyl dithio triosephosphate oxime to Chalkopyrite：
In O, O '-dibutyl dithio triosephosphate oxime concentration is 5 × 10-5Mol/L, pH values of pulp is 8～9, foaming agent
(MIBC) concentration is 15mg/L, N2Gas velocity is 200mL/min, is that the Chalkopyrite of -0.076mm～+0.038mm is floated to particle diameter
Select 3 minutes, now the flotation recovery rate of Chalkopyrite is 92.38%.
Embodiment 10
O, O '-flotation of the dibutyl dithio triosephosphate oxime to malachite：
In O, O '-dibutyl dithio triosephosphate oxime concentration is 1 × 10-4Mol/L, pH values of pulp is 8～9, foaming agent
(MIBC) concentration is 15mg/L, N2Gas velocity is 200mL/min, is that the malachite of -0.076mm～+0.038mm is floated to particle diameter
Select 3 minutes, now the flotation recovery rate of malachite is 81.56%.
Embodiment 11
Oxidation-copper sulfide ore float test
Yunnan oxidation-copper sulfide ore sample ore, wherein Ore cupric 0.61% or so, copper oxide mineral account for 76%, sulfur
Change copper mineral and account for 24%.
Experiment process is one roughing；Mog：- 0.074mm accounts for 83.7%；Agentia condition：Nine water amount of sodium sulfide
1600 g tons, slurry pH is 9.0, remaining agentia condition and its results are shown in Table 1.The result of the test of table 1 shows, using this
The bright nonferrous metals ore collecting agent with sulfydryl-oximyl structure is obtained than sulfydryl collecting agent butyl xanthate or itself and Saldox. group
Close the higher copper flotation recovery rate of collecting agent.The nonferrous metals ore with sulfydryl-oximyl structure for illustrating present invention preparation is caught
Receive the effect with Synergistic chelated metal ions between simultaneous mercapto groups and oximido group in agent.
The flotation conditions and its result of table 1 certain oxidation-copper sulfide ore
Embodiment 12
Oxidation-nickel sulfide ores float test：
Gansu oxidation-nickel sulfide ores sample ore, wherein Ore nickeliferous 0.76% or so, nickel oxide mineral account for 21%, sulfur
Change copper mineral and account for 79%.
Mog：- 0.074mm accounts for 72.5%；Agentia condition：The g ton of nine water amount of sodium sulfide 300, N, N- dibutyl
The g ton of aminodithioformic acid aldoxime consumption 120,2#The g ton of oily foaming agent 15；The operation of Jing one roughings obtains nickeliferous
4.78% flotation rough concentrate, the response rate of nickel is 85.79%.
Embodiment 13
Oxidation-zinc sulfide Ore float test：
Sichuan oxidation-zinc sulfide ore stone ore sample, Ore contains zinc 5.3% or so, and wherein Zinc oxide minerals account for 53%, sulfuration
Zinc mineral accounts for 47%.
Mog：- 0.074mm accounts for 75%；Agentia condition：The g ton of nine water amount of sodium sulfide 500, amount of sodium silicate 800
G ton, the g ton of O- amyl group xanthic acid acetone oximes consumption 300,2#The g ton of oily foaming agent 20；The operation of Jing one roughings is obtained and contains zinc
23.7% flotation rough concentrate, the response rate of zinc is 81.23%.
Claims (8)
1. a kind of nonferrous metals ore flotation collector with sulfydryl-oximyl structure, it is characterised in that with formula I or formula II or
Formula III structure：
Wherein,
R1、R2、R5And R6It is each independently selected from C2～C12Alkyl；
R3For C1～C12Alkylene；
R4For hydrogen atom or C1～C12Alkyl.
2. the nonferrous metals ore flotation collector with sulfydryl-oximyl structure according to claim 1, it is characterised in that
R1、R2、R5And R6It is each independently selected from C2～C12Alkyl；R3For C1～C12Alkylene alkyl or alkylene；R4For C1~
C12Alkyl.
3. the nonferrous metals ore flotation collector with sulfydryl-oximyl structure according to claim 2, it is characterised in that
R1、R2、R5And R6Be each independently selected from ethyl, propyl group, isopropyl, butyl, isobutyl group, sec-butyl, amyl group, isopentyl, new penta
Base, n-hexyl, isohesyl, n-octyl, iso-octyl or secondary octyl.
4. the nonferrous metals ore flotation collector with sulfydryl-oximyl structure according to claim 2, it is characterised in that R3
For methylene.
5. the nonferrous metals ore flotation collector with sulfydryl-oximyl structure according to claim 2, it is characterised in that R4
For methyl.
6. the application of the nonferrous metals ore flotation collector with sulfydryl-oximyl structure described in any one of Claims 1 to 5,
Characterized in that, the Non-ferrous minerals being applied in flotation collecting nonferrous metallic ores.
7. application according to claim 6, it is characterised in that carry out ore grinding and/or floatation process in nonferrous metallic ores
In, after addition is sized mixing including the floating agent including the nonferrous metals ore flotation collector with sulfydryl-oximyl structure, then
Non-ferrous minerals are floatingly selected by foam flotation method.
8. application according to claim 6, it is characterised in that described nonferrous metallic ores are the mixing of oxidation-copper sulfide
Ore deposit, oxidation-zinc sulfide composite ore or oxidation-nickel sulfide composite ore.
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| US4587013A (en) * | 1984-11-28 | 1986-05-06 | American Cyanamid Company | Monothiophosphinates as acid, neutral, or mildly alkaline circuit sulfide collectors and process for using same |
| CN100594067C (en) * | 2006-12-30 | 2010-03-17 | 陈铁 | Beneficiation method of complex copper oxide ore |
| CN100558468C (en) * | 2007-05-23 | 2009-11-11 | 华锡集团车河选矿厂 | Novel technics of cassiterite clay flotation |
| CN101125311B (en) * | 2007-09-24 | 2010-09-01 | 昆明理工大学 | Vulcanizing-flotation combing method for treating zinc kiln slag |
| CN100571879C (en) * | 2007-12-17 | 2009-12-23 | 中国铝业股份有限公司 | A kind of dressing process for desiliconizing of mixed type bauxite |
| CN103691570A (en) * | 2013-12-06 | 2014-04-02 | 西北矿冶研究院 | Copper-nickel sulfide ore collecting agent |
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