CN101972707A - Preparation method and application of pyrite inhibitor - Google Patents

Preparation method and application of pyrite inhibitor Download PDF

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Publication number
CN101972707A
CN101972707A CN2010102756725A CN201010275672A CN101972707A CN 101972707 A CN101972707 A CN 101972707A CN 2010102756725 A CN2010102756725 A CN 2010102756725A CN 201010275672 A CN201010275672 A CN 201010275672A CN 101972707 A CN101972707 A CN 101972707A
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sulfur
inhibitor
solution
iron mineral
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CN101972707B (en
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魏宗武
陈建华
穆枭
陈晔
兰丽红
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Guangxi University
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Guangxi University
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Abstract

一种硫铁矿物抑制剂的制备方法,是将14~16g对硝基苯胺加入到120~150ml体积浓度为20%硫酸溶液中,加热使其溶解,再在冰浴中冷却至10℃,在此温度下缓慢加入25~30ml质量百分浓度为25%的亚硝酸钠溶液得到产物1。将12~15g 4,4′-二氨基苯磺酰苯胺与15~20ml1mol/L盐酸配制成溶液并在冰浴中冷却至10℃,与产物1在pH9~10条件下偶合得到产物2,把产物2与15~20ml1mol/L间苯二胺在pH10~11条件下偶合得黑色易溶于水的粉末即为所述硫铁矿物抑制剂。本发明对硫铁矿物有很好的抑制作用,对铅矿物中的金或银矿物无影响,并且药剂用量少,无毒无污染。A kind of preparation method of sulfur iron mineral suppressor, is that 14~16g p-nitroaniline is added in 120~150ml volume concentration and is 20% sulfuric acid solution, heating makes it dissolve, then cools to 10 ℃ in ice bath, At this temperature, 25-30 ml of sodium nitrite solution with a mass percent concentration of 25% was slowly added to obtain product 1. Prepare a solution of 12-15g 4,4'-diaminobenzenesulfonanilide and 15-20ml 1mol/L hydrochloric acid and cool it to 10°C in an ice bath, and couple with product 1 at pH 9-10 to obtain product 2. The product 2 is coupled with 15-20 ml of 1mol/L m-phenylenediamine under the condition of pH 10-11 to obtain a black powder easily soluble in water, which is the sulfur iron mineral inhibitor. The invention has good inhibitory effect on pyrite minerals, has no influence on gold or silver minerals in lead minerals, and has less dosage of medicament, and is non-toxic and pollution-free.

Description

A kind of preparation method and application thereof of troilite thing inhibitor
One, technical field
The present invention relates to a kind of preparation method of troilite thing inhibitor, be applicable to that the plumbous sulfur mineral that contains gold or silver in the vulcanized lead mineral separates, and obtains to contain gold or silver lead ore concentrate.
Two, background technology
In plumbous sulfur mineral FLOTATION SEPARATION process, the general employing adds a large amount of lime to press down sulphur as the inhibitor of troilite thing floating plumbous, thus make plumbous sulphur content from, obtain lead concentrate; But when containing gold or silver in the lead minerals, can not make troilite thing inhibitor with lime, this is because in floatation process, lime is to containing gold or the silver mineral inhibitory action is apparent in view, gold or silver are suppressed inevitably, lose in mine tailing, so not only make resource fail to obtain fully comprehensive the recovery, also reduced the income of enterprise.
Three, summary of the invention
The object of the present invention is to provide a kind of preparation method of troilite thing inhibitor, the troilite thing inhibitor that is prepared into this method can suppress the troilite thing, and gold in the lead minerals or silver are not produced inhibitory action, and gold or silver are enriched in the lead concentrate.
The present invention achieves the above object by the following technical solutions: a kind of preparation method of troilite thing inhibitor, comprise the steps: that it is in 20% sulfuric acid solution that 14~16g paranitroanilinum is joined 120~150ml volumetric concentration, heating makes its dissolving, in ice bath, be cooled to 10 ℃ again, under this temperature, slowly add 25~30ml mass percentage concentration and be 25% sodium nitrite solution and obtain product 1, with 12~15g 4,4 '-diaminobenzene sulfonanilide and 15~20ml1mol/L hydrochloric acid is mixed with solution and is cooled to 10 ℃ in ice bath, obtain product 2 with product 1 coupling under pH9~10 conditions, coupling under pH10~11 conditions gets black powder soluble in water and is described troilite thing inhibitor product 2 and 15~20ml1mol/L m-phenylene diamine (MPD).
The application of described troilite thing inhibitor in plumbous sulphur associated mineral FLOTATION SEPARATION, after earlier ore ore grinding to mineral monomer being dissociated, transferring slurry pH with sodium carbonate is 8~9, in the floatation process, add described troilite thing inhibitor by 250~350g/t, and then add 100~150g/t diethyldithiocarbamate as plumbous collecting agent and 80~100g/t2 oil as foaming agent.
During use, earlier described troilite thing inhibitor is mixed with mass percentage concentration and is 1~2% the aqueous solution.
Concrete advantage of the present invention is:
Described troilite thing inhibitor has the good restraining effect to the troilite thing, and gold in the lead minerals or silver mineral are not produced inhibitory action, and dosing is few, nontoxic pollution-free.
Four, the specific embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1
A kind of preparation method's of troilite thing inhibitor a example may further comprise the steps:
It is in 20% sulfuric acid solution that the 14g paranitroanilinum is joined the 120ml volumetric concentration, and heating makes its dissolving, is cooled to 10 ℃ again in ice bath, slowly adds the 25ml mass percentage concentration and is 25% sodium nitrite solution under this temperature and obtain product 1.
With 12g 4,4 '-diaminobenzene sulfonanilide and 15ml1mol/L hydrochloric acid is mixed with solution and is cooled to 10 ℃ in ice bath, obtain product 2 with product 1 coupling under the pH9 condition, product 2 and the coupling under the pH10 condition of 15ml1mol/L m-phenylene diamine (MPD) are got black powder soluble in water be described inhibitor.
Embodiment 2
Another example of the preparation method of troilite thing inhibitor of the present invention, may further comprise the steps: it is in 20% sulfuric acid solution that the 16g paranitroanilinum is joined the 150ml volumetric concentration, heating makes its dissolving, in ice bath, be cooled to 10 ℃ again, under this temperature, slowly add the 30ml mass percentage concentration and be 25% sodium nitrite solution and obtain product 1.
With 15g 4,4 '-diaminobenzene sulfonanilide and 20ml1mol/L hydrochloric acid is mixed with solution and is cooled to 10 ℃ in ice bath, obtain product 2 with product 1 coupling under the pH10 condition, product 2 and the coupling under the pH11 condition of 20ml1mol/L m-phenylene diamine (MPD) are got black powder soluble in water be described inhibitor.
Embodiment 3
Troilite thing inhibitor the application example in plumbous sulphur FLOTATION SEPARATION of present embodiment for adopting embodiment 1 or 2 to be prepared into.
1, raw mineral materials:
Raw mineral materials is for containing gold sulfuration lead ore, wherein leaded 5.34%, sulphur 7.62%, golden 1.56g/t, and material phase analysis shows that lead minerals mainly exists with the galena form, other has a small amount of bournonite; Sulfur mineral mainly exists with the pyrite form, and other has a small amount of magnetic iron ore, and gold is distributed in the lead minerals.
2, regime of agent and operating condition: after earlier ore ore grinding to mineral monomer being dissociated, transferring slurry pH with sodium carbonate is 8~9, by one roughing scan for twice and the technological process of triple cleaning carry out plumbous sulphur content from, add the described troilite thing of 100g/t inhibitor during one roughing, and then add the 70g/t diethyldithiocarbamate as plumbous collecting agent and 60g/t2 oil as foaming agent, scan for twice and adopt described troilite thing inhibitor 50g/t, diethyldithiocarbamate 20g/t, No. 2 oily 20g/t, triple cleaning adopts described troilite thing inhibitor 100g/t, carried out 150t/d industry expanding test in a year, giving ore deposit grade lead 5.34%, sulphur 7.62%, under the gold 1.56g/t condition, obtaining leaded is 57.21%, contain the plumbous Gold Concentrate under Normal Pressure of golden 16.30g/t%, lead recovery reaches 88.72%, and gold recovery reaches 86.52%.
Embodiment 4
Troilite thing inhibitor the Another Application example in plumbous sulphur FLOTATION SEPARATION of present embodiment for adopting embodiment 1 or 2 to be prepared into.
1, raw mineral materials:
Raw mineral materials is an argentiferous sulfuration lead ore, wherein leaded 3.79%, sulphur 8.27%, silver-colored 50.24g/t, and material phase analysis shows lead minerals based on jamesonite, other has a small amount of galena; Sulfur mineral is based on pyrite, and other has a small amount of mispickel, and silver is distributed in the lead minerals.
2, regime of agent and operating condition: after earlier ore ore grinding to mineral monomer being dissociated, transferring slurry pH with sodium carbonate is 8~9, by one roughing scan for twice and the technological process of triple cleaning carry out plumbous sulphur content from, add the described troilite thing of 150g/t inhibitor during one roughing, and then add the 100g/t diethyldithiocarbamate as plumbous collecting agent and 70g/t2 oil as foaming agent, scan for twice and adopt described troilite thing inhibitor 100g/t, diethyldithiocarbamate 30g/t, No. 2 oily 20g/t, triple cleaning adopts described troilite thing inhibitor 100g/t, carried out 150t/d industry expanding test in a year, the result shows effectively separation of lead sulfur mineral of the above medicament condition of employing, obtains plumbous silver preparation concentrate; Giving under ore deposit grade lead 1.79%, sulphur 8.27%, the silver-colored 50.24g/t condition, obtaining leadedly being 27.67%, the plumbous silver preparation concentrate of argentiferous 763.75g/t, lead recovery reaches 90.21%, and silver raising recovery rate reaches 88.78%.

Claims (3)

1.一种硫铁矿物抑制剂的制备方法,其特征在于,该制备方法的步骤为:将14~16g对硝基苯胺加入到120~150ml体积浓度为20%硫酸溶液中,加热使其溶解,再在冰浴中冷却至10℃,在此温度下缓慢加入25~30ml质量百分浓度为25%的亚硝酸钠溶液得到产物1,将12~15g 4,4′-二氨基苯磺酰苯胺与15~20ml1mol/L盐酸配制成溶液并在冰浴中冷却至10℃,与产物1在pH9~10条件下偶合得到产物2,把产物2与15~20ml1mol/L间苯二胺在pH10~11条件下偶合得黑色易溶于水的粉末即为所述硫铁矿物抑制剂。1. a preparation method of sulfur-iron mineral inhibitor, is characterized in that, the step of this preparation method is: join 14~16g p-nitroaniline into 120~150ml volume concentration be in the 20% sulfuric acid solution, heating makes it Dissolve, then cool in an ice bath to 10°C, slowly add 25-30ml of sodium nitrite solution with a mass percent concentration of 25% at this temperature to obtain product 1, and mix 12-15g of 4,4'-diaminobenzenesulfonate Anilide and 15-20ml 1mol/L hydrochloric acid were prepared into a solution and cooled to 10°C in an ice bath, and product 1 was coupled with product 1 at pH 9-10 to obtain product 2, and product 2 was mixed with 15-20ml 1mol/L m-phenylenediamine in The black powder easily soluble in water obtained by coupling under the condition of pH 10-11 is the sulfur-iron mineral inhibitor. 2.权利要求1制备得的硫铁矿物抑制剂在铅硫浮选分离中的应用,其特征在于,浮选时矿浆pH值为8~9,浮选过程中,按250~350g/t加入所述硫铁矿物抑制剂。2. the application of the sulfur-iron mineral suppressor prepared in claim 1 in lead-sulfur flotation separation, is characterized in that, during flotation, the ore slurry pH value is 8~9, and in the flotation process, by 250~350g/t Add the pyrite mineral inhibitor. 3.根据权利要求2所述硫铁矿物抑制剂在铅硫浮选分离中的应用,其特征在于,使用时,先将所述硫铁矿物抑制剂配制成质量百分浓度为1~2%的水溶液。3. according to the application of the described sulfur-iron mineral depressant in lead-sulfur flotation separation according to claim 2, it is characterized in that, when in use, first described sulfur-iron mineral depressant is mixed with mass percent concentration and is 1~2. 2% aqueous solution.
CN2010102756725A 2010-09-08 2010-09-08 Preparation method and application of pyrite inhibitor Expired - Fee Related CN101972707B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103657861A (en) * 2013-12-11 2014-03-26 广西大学 Preparation method of nickel sulfide mineral inhibitor and application thereof
CN103691575A (en) * 2013-12-17 2014-04-02 广西大学 Preparation method of lead sulfide mineral inhibitor
CN103721856A (en) * 2013-12-17 2014-04-16 广西大学 Garnet inhibitor preparation method
CN104399594A (en) * 2014-11-21 2015-03-11 广西大学 Preparation method and application of flotation separation inhibitor of zinc-sulfur minerals
CN104718027A (en) * 2012-04-12 2015-06-17 瓦勒股份有限公司 A method for improving selectivity and recovery in the flotation of nickel sulphide ores that contain pyrhotite by exploiting the synergy of multiple depressants
CN106423579A (en) * 2016-11-02 2017-02-22 广西大学 Preparation method of calcium carbonate mineral inhibitor

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104718027A (en) * 2012-04-12 2015-06-17 瓦勒股份有限公司 A method for improving selectivity and recovery in the flotation of nickel sulphide ores that contain pyrhotite by exploiting the synergy of multiple depressants
CN104718027B (en) * 2012-04-12 2017-07-18 淡水河谷公司 The method for improving selectivity and the rate of recovery in the flotation of the nickel sulfide ores containing magnetic iron ore by using the synergy of various inhibitors
CN103657861A (en) * 2013-12-11 2014-03-26 广西大学 Preparation method of nickel sulfide mineral inhibitor and application thereof
CN103657861B (en) * 2013-12-11 2015-07-22 广西大学 Preparation method of nickel sulfide mineral inhibitor and application thereof
CN103691575A (en) * 2013-12-17 2014-04-02 广西大学 Preparation method of lead sulfide mineral inhibitor
CN103721856A (en) * 2013-12-17 2014-04-16 广西大学 Garnet inhibitor preparation method
CN103721856B (en) * 2013-12-17 2015-12-02 广西大学 A kind of preparation method of Garnet inhibitor
CN103691575B (en) * 2013-12-17 2016-01-20 广西大学 A kind of preparation method of vulcanized lead mineral inhibitor
CN104399594A (en) * 2014-11-21 2015-03-11 广西大学 Preparation method and application of flotation separation inhibitor of zinc-sulfur minerals
CN106423579A (en) * 2016-11-02 2017-02-22 广西大学 Preparation method of calcium carbonate mineral inhibitor
CN106423579B (en) * 2016-11-02 2018-11-20 广西大学 A kind of preparation method of calcium carbonate mineral inhibitor

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Inventor after: Wei Zongwu

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