CN102690952A - Method for preparing iron oxide red by carrying out reducing roasting on high-sulfur gold concentrate and enhancing acid solution - Google Patents

Method for preparing iron oxide red by carrying out reducing roasting on high-sulfur gold concentrate and enhancing acid solution Download PDF

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CN102690952A
CN102690952A CN2012102002483A CN201210200248A CN102690952A CN 102690952 A CN102690952 A CN 102690952A CN 2012102002483 A CN2012102002483 A CN 2012102002483A CN 201210200248 A CN201210200248 A CN 201210200248A CN 102690952 A CN102690952 A CN 102690952A
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iron oxide
oxide red
reducing roasting
gold concentrate
formulations prepared
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刘维
张杜超
刘昭成
欧阳彪
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Central South University
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Central South University
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Abstract

The invention discloses a method for preparing iron oxide red by carrying out reducing roasting on high-sulfur gold concentrate and enhancing acid solution. In order to increase recovery rate of gold and fully utilize resources as well as realize comprehensive recovery of valuable metals, iron high-value utilization and hydrochloric acid regeneration, the method comprises the steps of: oxidizing partial Fe<2+> in an acid-soluble lixivium into Fe<3+> for removing arsenic and silicon in the solution; clarifying under the action of a flocculating agent; and then replacing copper in supernatant by adopting iron, and carrying out spraying and thermal decomposition on a refined FeCl2 solution generated after replacement to obtain iron oxide red and hydrochloric acid. According to the invention, As and Si in the acid-soluble lixivium can be respectively removed to below 50ppm and 4ppm; the recovery rate of copper is more than 99 percent, and the regeneration rate of hydrochloric acid is more than 99 percent.

Description

A kind of method of high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red
Technical field
The present invention relates to a kind of smelting process of gold ores containing sulfur, particularly a kind of with dissolving the method that the gained leach liquor prepares iron oxide red with the hydrochloric acid intensified acid after the reducing roasting of gold ores containing sulfur fluidized bed roasting slag.
Background technology
China exists sulfurous iron ore type and mispickel type gold mine in a large number, can be high sulphur gold concentrate with its enrichment through flotation operation, is difficult to directly adopt cyanide process therefrom to extract gold and silver.Fluidized bed roasting can generate SO with the sulphur oxidation in the concentrate 2Be used for relieving haperacidity, adopt the arsenic of two sections fluidized bed roastings in especially can the deep removal gold ore, in China's high sulphur gold concentrate smelting process, be used widely.But owing to passed through high-temperature calcination process; Gold in the calcining by flux body parcel, makes that gold leaching rate was difficult to improve when follow-up cyaniding was handled in pyroprocess, contain gold after the cyaniding in the tailings still at 10～20g/t; Gold recovery less than 80%, serious waste of resources.
Summary of the invention
In order to improve the recovery of gold; Make full use of resource; Realize comprehensive recovery, iron high-value-use and the regeneration of hydrochloric acid of valuable metal, the present invention aims to provide a kind of method of high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red, this method Fe in the calcining that will seethe with excitement earlier 2O 3Be reduced to FeO, adopt hydrochloric acid to leach then and obtain pH, thereby realize FeCl from hydrochloric acid stripping reduced calcine gained at the leach liquor more than 2 2Reclaim valuable metal in the solution and prepare high-quality iron oxide red.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is:
A kind of method of high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red comprises the steps:
1) the sulfur containing aurin ore-roasting is carried out reducing roasting under about reductive agent;
2) adopt strong acid solution to carry out acidleach the calcining after the reducing roasting;
3) reduced calcine after the acidleach is filtered, the pH of leaching solution after filtering is transferred to more than 2.5, in leach liquor, add flocculation agent then, bubbling air is the Fe of 0.2～2g/L with concentration 2+Be oxidized to Fe 3+, generate cotton-shaped Fe (OH) 3, coagulation time 20～120min, As and Fe in the leach liquor 3+Generate FeAsO 4Deposition, the silicon in the leach liquor generates cotton-shaped silica gel, cotton-shaped Fe (OH) under the effect of flocculation agent 3FeAsO in the absorption 4Grow up for being easy to sedimentary reticulate body behind deposition and the cotton-shaped silica gel, and precipitate; Its reaction principle is:
4Fe 2++O 2+4H +＝4Fe 3++2H 2O
Fe 3++AsO 4 3-＝FeAsO 4
Fe 3++3H 2O＝Fe(OH) 3+3H +
4) contain cupric ion in the supernatant of post precipitation, adopt the copper in the iron displacement supernatant, filter then, promptly obtain copper sponge and refining FeCl respectively 2Solution;
5) will make with extra care FeCl 2The solution thermolysis of at high temperature spraying, heat decomposition temperature is 500 ℃～1000 ℃, and reaction as follows takes place:
4FeCl 2+4H 2O+O 2＝2Fe 2O 3+8HCl
Fe 2O 3Be iron oxide red.
In the step 3) of the present invention, the leach liquor after the said filtration transfers to its pH value more than 2.5 with ammoniacal liquor.
In the step 3) of the present invention, add in the said leach liquor that pH is more than 3.5 behind the flocculation agent, bubbling air is with the Fe of concentration 0.5～1g/L 2+Be oxidized to Fe 3+, coagulation time 30min～60min.
Described HCl adopts the water spray to absorb, and obtains hydrochloric acid, and hydrochloric acid is returned step 2) in carry out acidleach.
In the step 4), the step of said iron displacement copper does, in the deposition supernatant, adds iron, and said iron consumption is 1～3 times of theoretical consumption, under ℃ temperature of normal temperature～80, reduces 0.5～10h.Further, said iron consumption is 1.5～2 times of theoretical consumption, 50 ℃～60 ℃ of displacement temperature, recovery time 4h～6h.
As a kind of preferred, said flocculation agent is the SEPIGEL 305 of massfraction 0.1～5%, and further, the massfraction of said SEPIGEL 305 is 0.5～0.8%.
In the step 5), said spraying heat decomposition temperature is preferably 600 ℃～850 ℃.
Step 2 of the present invention) in, said strong acid solution is the HCl solution of massfraction 5～40%.
Among the present invention, described reductive agent is the carbonaceous reducing agent of massfraction 5%～80%.Said carbonaceous reducing agent is preferably coal dust or coke powder, and when carbonaceous reducing agent was coal dust, pulverized coal consumption was 150～500kg/t calcining, and when carbonaceous reducing agent was coke powder, the coke powder consumption was 100～400kg/t calcining.Described reductive agent can also be the gas base reductant of volume(tric)fraction 1%～50%.Said gas base reductant is preferably coal gas, hydrogen or Sweet natural gas; When selecting coal gas, gas concentration is 3%～20%; When selecting hydrogen, density of hydrogen is 1%～5%; When selecting Sweet natural gas, concentration of natural gas is 5%～30%.
Below the present invention is done further elaboration.
A kind of method of high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red comprises the steps:
PH of leaching solution is transferred to more than 2.5 with ammoniacal liquor, add 0.1～5% SEPIGEL 305 and make flocculation agent, blast atmospheric oxidation 0.2～2g/LFe 2+Be Fe 3+, generate cotton-shaped Fe (OH) 3, coagulation time 20～120min, As and Fe in the solution 3+Generate FeAsO 4Deposition, the silicon in the solution also generates cotton-shaped silica gel, colloid Fe (OH) under the effect of flocculation agent 3FeAsO in the absorption 4With grow up behind the silica gel for being easy to sedimentary reticulate body, and finally precipitate.Its reaction principle is:
4Fe 2++O 2+4H +＝4Fe 3++2H 2O
Fe 3++AsO 4 3-＝FeAsO 4
Fe 3++3H 2O＝Fe(OH) 3+3H +
The deposition supernatant contains copper, can adopt iron replacement to reclaim, and extraordinarily goes into iron filings, iron powder or scrap iron etc. by the required theory of displacement copper with iron amount 1～3, under ℃ temperature of normal temperature～80, reduces 0.5～10h, filters, and promptly obtains copper sponge and refining FeCl 2Solution.
Refining FeCl 2The solution thermolysis of at high temperature spraying, heat decomposition temperature is 500 ℃～1000 ℃, and reaction as follows takes place.
4FeCl 2+4H 2O+O 2＝2Fe 2O 3+8HCl
Fe 2O 3Be iron oxide red, HCl adopts the water spray to absorb, and obtains hydrochloric acid, and hydrochloric acid returns acidleach again, has realized sour regeneration and circulation.
Flocculation sediment preferred solution pH is more than 3.5 in aforesaid method, Fe 2+Be oxidized to Fe 3+Concentration is 0.5～1g/L, and flocculant addition is 0.5～0.8%, coagulation time 30～60min.
Preferred displacement uses the iron powder amount to be 1.5～2 times of theoretical consumptions in the aforesaid method, 50～60 ℃ of displacement temperature, recovery time 4～6h.
Preferred spraying heat decomposition temperature is 600～850 ℃.
Compared with prior art, the invention has the beneficial effects as follows:
(1) As and Si can remove to 50ppm with below the 4ppm respectively in the leach liquor.
(2) the refining FeCl in displacement back 2Cu can remove to more than the 20ppm in the solution, and copper recovery is greater than 99%.
(3) spraying thermolysis gained iron oxide red quality satisfies first grade standard among the GB/T 1863-2008, and the regeneration of hydrochloric acid rate is greater than 99%.
Description of drawings
Fig. 1 is the process flow sheet of an embodiment of the present invention.
Embodiment
Embodiment 1
A kind of method of high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red comprises the steps:
At first the sulfur containing aurin ore-roasting is mixed with reductive agent and be placed on the reducing roasting kiln roasting; And adopt hydrochloric acid to carry out acidleach the calcining after the reducing roasting; Then the reduced calcine after the acidleach is filtered, get 1m after the filtration 3Hydrochloric acid leachate, its composition are Fe 110g/L, As 0.95g/L, Si 0.098g/L, Cu1.8g/L.Ammoniacal liquor is regulated pH to 3.0, adds the 1kg SEPIGEL 305, and air blast is with Fe 2+Be oxidizing to its concentration and reduce to 109g/L, coagulation 35min, clarification filtration.Add the 2kg iron powder in the supernatant, displacement copper.Obtain iron oxide red Fe 700 ℃ of thermolysiss of spraying down 2O 3And hydrochloric acid.Iron oxide red satisfies first grade requirement among the GB/T 1863-2008, regeneration of hydrochloric acid rate 99.5%, copper recovery 99.5%.
Embodiment 2
A kind of method of high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red comprises the steps:
At first the sulfur containing aurin ore-roasting is mixed with reductive agent and be placed on the reducing roasting kiln roasting; And adopt hydrochloric acid to carry out acidleach the calcining after the reducing roasting; Then the reduced calcine after the acidleach is filtered, get 1m after the filtration 3Hydrochloric acid leachate, its composition are Fe 132g/L, As 1.25g/L, Si 0.11g/L, Cu3.3g/L.Ammoniacal liquor is regulated pH to 3.0, adds the 2.1kg SEPIGEL 305, and air blast is with Fe 2+Be oxidizing to its concentration and reduce to 130g/L, coagulation 60min, clarification filtration.Add the 8.5kg iron powder in the supernatant, displacement copper.Obtain iron oxide red and hydrochloric acid 950 ℃ of thermolysiss of spraying down.Iron oxide red satisfies first grade requirement among the GB/T 1863-2008, regeneration of hydrochloric acid rate 99.5%, copper recovery 99.8%.
The content that the foregoing description is illustrated is to be understood that to these embodiment and only is used to be illustrated more clearly in the present invention; And be not used in the restriction scope of the present invention; After having read the present invention, those skilled in the art all fall within the application's accompanying claims institute restricted portion to the modification of the various equivalent form of values of the present invention.

Claims (10)

1. the method for a high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red is characterized in that, comprises the steps:
1) the sulfur containing aurin ore-roasting is carried out reducing roasting under about reductive agent;
2) adopt strong acid solution to carry out acidleach the calcining after the reducing roasting;
3) reduced calcine after the acidleach is filtered, the pH of leaching solution after filtering is transferred to more than 2.5, in leach liquor, add flocculation agent then, bubbling air is the Fe of 0.2～2g/L with concentration 2+Be oxidized to Fe 3+, generate cotton-shaped Fe (OH) 3, coagulation time 20～120min, As and Fe in the leach liquor 3+Generate FeAsO 4Deposition, the silicon in the leach liquor generates cotton-shaped silica gel, cotton-shaped Fe (OH) under the effect of flocculation agent 3FeAsO in the absorption 4Grow up for being easy to sedimentary reticulate body behind deposition and the cotton-shaped silica gel, and precipitate; Its reaction principle is:
4Fe 2++O 2+4H +＝4Fe 3++2H 2O
Fe 3++AsO 4 3-＝FeAsO 4
Fe 3++3H 2O＝Fe(OH) 3+3H +
4) contain cupric ion in the supernatant of post precipitation, adopt the copper in the iron displacement supernatant, filter then, promptly obtain copper sponge and refining FeCl respectively 2Solution;
5) will make with extra care FeCl 2The solution thermolysis of at high temperature spraying, heat decomposition temperature is 500 ℃～1000 ℃, and reaction as follows takes place:
4FeCl 2+4H 2O+O 2＝2Fe 2O 3+8HCl
Fe 2O 3Be iron oxide red.
2. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 1 is characterized in that the leach liquor after the said filtration transfers to its pH value more than 2.5 with ammoniacal liquor.
3. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 1 is characterized in that, adds in the said leach liquor that pH is more than 3.5 behind the flocculation agent, and bubbling air is with the Fe of concentration 0.5～1g/L 2+Be oxidized to Fe 3+, coagulation time 30min～60min.
4. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 1 is characterized in that, HCl in the said step 5) adopts the water spray to absorb, and obtains hydrochloric acid, and hydrochloric acid is returned step 2) in carry out acidleach.
5. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 1; It is characterized in that; In the step 4), the step of said iron displacement copper is in the deposition supernatant, to add iron; Said iron consumption is 1～3 times of theoretical consumption, under ℃ temperature of normal temperature～80, reduces 0.5～10h.
6. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 5 is characterized in that said iron consumption is 1.5～2 times of theoretical consumption, 50 ℃～60 ℃ of displacement temperature, recovery time 4h～6h.
7. according to the method for claim 1 or 3 described high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide reds, it is characterized in that said flocculation agent is the SEPIGEL 305 of massfraction 0.1～5%.
8. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 7 is characterized in that the massfraction of said SEPIGEL 305 is 0.5～0.8%.
9. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 1 is characterized in that said spraying heat decomposition temperature is 600 ℃～850 ℃.
10. the method for high sulphur gold concentrate calcining reducing roasting intensified acid formulations prepared from solutions iron oxide red according to claim 1 is characterized in that said strong acid solution is the HCl solution of massfraction 5～40%.
CN2012102002483A 2012-06-18 2012-06-18 Method for preparing iron oxide red by carrying out reducing roasting on high-sulfur gold concentrate and enhancing acid solution Pending CN102690952A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107739838A (en) * 2017-09-06 2018-02-27 昆明理工大学 A kind of method for reclaiming iron from electric furnace zinc smelting bottom slag and being enriched with copper and tin
CN112143907A (en) * 2020-09-28 2020-12-29 山东国大黄金股份有限公司 Method for improving leaching rate of gold and silver in arsenic-containing gold concentrate

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1614041A (en) * 2004-10-11 2005-05-11 东华大学 Enhanced acid dissolve of acidizing fired slags of concentrated gold ores containing sulfur
CN1772628A (en) * 2005-09-27 2006-05-17 东华大学 Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1614041A (en) * 2004-10-11 2005-05-11 东华大学 Enhanced acid dissolve of acidizing fired slags of concentrated gold ores containing sulfur
CN1772628A (en) * 2005-09-27 2006-05-17 东华大学 Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107739838A (en) * 2017-09-06 2018-02-27 昆明理工大学 A kind of method for reclaiming iron from electric furnace zinc smelting bottom slag and being enriched with copper and tin
CN107739838B (en) * 2017-09-06 2019-09-27 昆明理工大学 A method of from electric furnace zinc smelting bottom slag recycling iron and enrichment copper and tin
CN112143907A (en) * 2020-09-28 2020-12-29 山东国大黄金股份有限公司 Method for improving leaching rate of gold and silver in arsenic-containing gold concentrate

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Application publication date: 20120926