CN1313379C - Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore - Google Patents
Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore Download PDFInfo
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- CN1313379C CN1313379C CNB2005100300168A CN200510030016A CN1313379C CN 1313379 C CN1313379 C CN 1313379C CN B2005100300168 A CNB2005100300168 A CN B2005100300168A CN 200510030016 A CN200510030016 A CN 200510030016A CN 1313379 C CN1313379 C CN 1313379C
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- iron oxide
- oxide red
- roasted
- dregs
- iron
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Abstract
The present invention discloses a method for preparing iron oxide red with sulfated roasted dregs of sulfur containing gold ore concentrate, which comprises the following steps: (1) 30 to 60% of sulfuric acid and the roasted dregs are added into a reaction kettle, the weight ratio of the sulfuric acid and the roasted dregs is 1 to 2-10, the sulfuric acid and the roasted dregs are stirred, a cosolvent is added, the weight ratio of the cosolvent and the roasted dregs is 1 to 1-100, a reaction is carried out for one to six hours in the temperature of 60 to 100DEG C, and after the reaction is completed, obtained filtrate and residue are filtered; (2) the filtrate obtained in the step (1) is neutralized by ammonia water, ph value of the filtrate is controlled to be of 1 to 2, and then, the ammonia water is added in the temperature of 50 to 90DEG C until iron ions are partially precipitated, and a flocculating reagent is added; (3) precipitates obtained in the step 2 are washed until no sulfate ion exists, and then, the precipitates are dried, calcined in the temperature of 300 to 700DEG C and milled to the particle size required by an iron oxide red pigment to obtain the iron oxide red. The present invention has the advantages that raw materials for preparing the iron oxide red are increased, and the tailing resource utilizing rate is improved; the gold is extracted by the improved subsequent cyaniding technology, and thereby, the efficiency of cyaniding gold extraction is improved three to four percentage points, and the energy consumption and the environmental pollution are reduced.
Description
Technical field
The present invention relates to a kind of industrial solid castoff resource utilization, minimizing and innoxious technology, particularly relate to a kind of intensified acid with gold ores containing sulfur sulfurization roasting slag molten after, prepare iron oxide red by leaching liquid, fully utilize the method for ferro element, reduce its environmental pollution.
Background technology
In the prior art, iron oxide red is a kind of very important chemical pigment or the magneticsubstance that uses in the industry.As patent CN1102626A, CN1177572A, general is raw material with byproduct iron vitriol, pickle solution, electrolysis anode sludge, sulfuric acid slag or the iron ore concentrate etc. of producing titanium dioxide, under the situation that iron sheet exists, prepare iron oxide red with oxidation style, the shortcoming of this method is that all to have used the high-quality iron sheet be raw material, causes easily that there is lack of raw materials or the prices of raw and semifnished materials are flown upward.In addition, the leaching rate method of acid leaching residue through the molten raising gold and silver of intensified acid proposed in the intensified acid of patent gold ores containing sulfur sulfurization roasting slag molten (application number 200410067020.7); The technology of utilizing of acid leaching residue routine is through cyanidation gold-extracted, it is higher to carry in the golden cyanogen slag ferric oxide, Z 250, lead and arsenic content, what have prepares iron oxide red inferior through magnetic separation, auxiliary material is done in being drawn by the cement mill of having, because high-temp combustion discharges dusty gass such as a large amount of sulfurous gas, white arsenic, atmosphere pollution.What have just is deposited near the mine, causes spontaneous combustion, atmosphere pollution easily; Simultaneously, the harmful cyanide ion, the metal ion that contain in the cyanogen slag also easily flow in the water or in the soil, cause environmental pollution, therefore are necessary it is handled, and turn waste into wealth.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing iron oxide red with gold ores containing sulfur sulfurization roasting slag, to remedy the deficiencies in the prior art and defective, so that enlarge the raw material that iron oxide red is produced, reduce the harm of acid leaching residue to environment, meet the needs of production.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of method for preparing iron oxide red with gold ores containing sulfur sulfurization roasting slag, comprise the steps: that (1) adds 30～60% sulfuric acid and fired slags in reactor, the weight ratio of the two is 1: 2～10, stir, add solubility promoter, the weight ratio of solubility promoter and fired slags is 1: 1～100, reacted 1～6 hour down at 60～100 ℃, the after-filtration that reacts completely obtains filtrate and residue; 2) filtrate that step (1) is obtained neutralizes with ammoniacal liquor, and control pH value is 1～2, adds ammoniacal liquor down at 50～90 ℃ then, to the iron ion partly precipitated, adds flocculation agent; (3) throw out that step (2) is obtained, wash to the sulfate radical-free ion, dry then, and 300～700 ℃ of calcinings down, be milled down to the granularity of iron oxide red pigment requirement, obtain iron oxide red, wherein, described solubility promoter is to contain 1%-25% b diammonium edta sodium (EDTA), 1%-30%CuO, 20%-30%Fe
2O
3, 40%-60%SiO
2And 0-9%Al
2O
3The mixture of forming.
As optimized technical scheme: described flocculation agent is selected from one or more in alum, alchlor, green vitriol (ferrous sulfate), iron trichloride or the organic floculant.
In order to reduce cost, solubility promoter recycles after can reclaiming, and is reused for the iron in the leaching acid leaching residue; Produce the filtrate of iron oxide red and also can and distill, reclaim ammoniacal liquor and alkali, utilized again with alkali reaction.
The invention has the beneficial effects as follows: utilize fired slags leaching back leaching liquid to prepare iron oxide red, can reach following effect: (1) has enlarged the raw material of preparation iron oxide red, increases the tailings resource utilization; (2) improve follow-up cyanidation technology and carry gold, improve three to four percentage points of cyanidation gold-extracted efficient, cut down the consumption of energy; (3) reduced environmental pollution.
Description of drawings
Fig. 1 prepares the process flow sheet of iron oxide red for fired slags leaching of the present invention back leaching liquid
Embodiment
Below in conjunction with accompanying drawing the present invention is further elaborated.With reference to accompanying drawing 1.
Embodiment 1
In having the reactor of agitator, add 60% sulfuric acid, start stirrer and stir, disposable adding fired slags, the weight ratio of fired slags and sulphuric acid soln is 2: 1, the weight ratio of fired slags and solubility promoter is 1: 1, and the composition of solubility promoter is 1% b diammonium edta sodium, 30%CuO, 20%Fe
2O
3, 40%SiO
2And 9%Al
2O
3, under 80 ℃ of temperature, react 6h, the iron leaching rate is 100%, the leaching rate of gold and silver is more than 98%.Filter, it is 1 that filtrate is neutralized to the pH value with ammoniacal liquor, adds the flocculation agent iron trichloride, removes precipitation, separates solubility promoter, adds ammoniacal liquor to iron ion then again and precipitate fully under 50 ℃.Again after filtration, filtrate being used to reclaimed ammoniacal liquor and alkali, and filter residue is through washing, dry, calcining under 300 ℃.Iron oxide red after the calcining reaches the granularity that iron oxide red pigment requires through ore grinding, promptly can obtain the high-quality iron oxide red, and its quality index (seeing attached list 1) is better than the target level of product quality that GB GB1863-89 requires.
Embodiment 2
In having the reactor of agitator, add 30% sulfuric acid, starting stirrer stirs, disposable adding fired slags, the weight ratio of fired slags and sulphuric acid soln are 10: 1, and the weight ratio of fired slags and solubility promoter is that 50: 1, the composition of solubility promoter are 25% b diammonium edta sodium, 1%CuO, 30%Fe
2O
3, 60%SiO
2Temperature of reaction is that 100 ℃, reaction times are 1h, iron leaching rate 100%, and the leaching rate of gold and silver is more than 98%.The leaching thing filters, and system temperature is dropped to room temperature, filters then.It is 1.3 that filtrate is neutralized to the pH value with alkali, adds flocculation agent alum, removes precipitation, separates solubility promoter, adds ammoniacal liquor to iron ion then again and precipitate fully under 90 ℃.Process is filtered, and filtrate being used to reclaimed ammoniacal liquor and alkali, and filter residue is through washing, dry, calcining under 680 ℃.Iron oxide red after the calcining reaches the granularity that iron oxide red pigment requires through ore grinding, both can obtain being better than the high-quality iron oxide red of the target level of product quality that GB GB1863-89 requires.
Embodiment 3
In having the reactor of agitator, add 45% sulfuric acid, starting stirrer stirs, disposable adding fired slags, the weight ratio of fired slags and sulphuric acid soln are 5: 1, and the weight ratio of fired slags and solubility promoter is that 100: 1, the composition of solubility promoter are 10% b diammonium edta sodium, 2%CuO, 15%Fe
2O
3, 50%SiO
2And 5%Al
2O
3Temperature of reaction is 60 ℃, and the reaction times is 5h, iron leaching rate 100%, and the leaching rate of gold and silver is more than 98%.The leaching thing filters, and system temperature is dropped to room temperature, filters then.Filtrate neutralizes with alkali, to the pH value be 1.5, add the flocculation agent polyacrylamide, remove precipitation, separate solubility promoter, under 90 ℃, add ammoniacal liquor to iron ion then again and precipitate fully.Process is filtered, and filtrate being used to reclaimed ammoniacal liquor and alkali, and filter residue is through washing, dry, calcining under 500 ℃.Iron oxide red after the calcining reaches the granularity that iron oxide red pigment requires through ore grinding, both can obtain being better than the high-quality iron oxide red of the target level of product quality that GB GB1863-89 requires.
Embodiment 4
In having the reactor of agitator, add 56% sulfuric acid, starting stirrer stirs, disposable adding fired slags, the weight ratio of fired slags and sulphuric acid soln are 5: 1, and the weight ratio of fired slags and solubility promoter is that 30: 1, the composition of solubility promoter are 1% b diammonium edta sodium, 30%CuO, 10%Fe
2O
3, 50%SiO
2And 1%Al
2O
3Temperature of reaction is that 95 ℃, reaction times are 6h, and iron leaching rate 100%, the leaching rate of gold and silver are more than 98%.The leaching thing filters, and it is 1 that filtrate is neutralized to the pH value with alkali, adds flocculation agent starch, removes precipitation, separates solubility promoter, adds ammoniacal liquor to iron ion again and precipitate fully under 70 ℃.Process is filtered, and filtrate being used to reclaimed ammoniacal liquor and alkali, and filter residue is through washing, dry, calcining under 700 ℃.Iron oxide red after the calcining reaches the granularity that iron oxide red pigment requires through ore grinding, both can obtain being better than the high-quality iron oxide red that GB GB1863-89 requires.The quality index of table 1 iron oxide red product
| Project | Product quality indicator of the present invention | GB GB1863-89 |
| Color | Approximate～little | Approximate～little |
| TC, calcium oxide (%) | 0.1 | ＜0.3 |
| Relative color strength (%) | 96 | 95 |
| 105 ℃ of volatile matters (%) | 0.01 | 1.0 |
| The water solubles (%) | 0.1 | 0.2 |
| Oil number (ml/100g) | 20 | 15～25 |
| Iron level, ferric oxide % | 95.3 | 95 |
| Lead chromate | Negative | Negative |
Claims (2)
1. method for preparing iron oxide red with gold ores containing sulfur sulfurization roasting slag, it is characterized in that: comprise the steps: that (1) adds 30～60% sulfuric acid and fired slags in reactor, the weight ratio of the two is 1: 2～10, stir, add solubility promoter, the weight ratio of solubility promoter and fired slags is 1: 1～100, reacts 1～6 hour down at 60～100 ℃, and the after-filtration that reacts completely obtains filtrate and residue; (2) filtrate that step (1) is obtained neutralizes with ammoniacal liquor, and control pH value is 1～2, adds ammoniacal liquor down at 50～90 ℃ then, to the iron ion partly precipitated, adds flocculation agent; (3) throw out that step (2) is obtained washs to the sulfate radical-free ion, and is dry then, and, be milled down to the granularity of iron oxide red pigment requirement 300～700 ℃ of calcinings down, obtain iron oxide red, wherein, described solubility promoter is to contain 1%-25% b diammonium edta sodium, 1%-30%CuO, 20%-30%Fe
2O
3, 40%-60%SiO
2And 0-9%Al
2O
3The mixture of forming.
2. method according to claim 1 is characterized in that: described flocculation agent is selected from one or more in alum, alchlor, green vitriol, iron trichloride or the organic floculant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100300168A CN1313379C (en) | 2005-09-27 | 2005-09-27 | Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100300168A CN1313379C (en) | 2005-09-27 | 2005-09-27 | Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1772628A CN1772628A (en) | 2006-05-17 |
| CN1313379C true CN1313379C (en) | 2007-05-02 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100300168A Expired - Fee Related CN1313379C (en) | 2005-09-27 | 2005-09-27 | Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore |
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| CN (1) | CN1313379C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690952A (en) * | 2012-06-18 | 2012-09-26 | 中南大学 | Method for preparing iron oxide red by carrying out reducing roasting on high-sulfur gold concentrate and enhancing acid solution |
| CN104164570B (en) * | 2014-07-25 | 2016-08-24 | 河南中原黄金冶炼厂有限责任公司 | A kind of preprocess method of noble metal smelting slag |
| CN105779776A (en) * | 2014-12-24 | 2016-07-20 | 李瑶 | Method for recycling gold from roasting residues or roasting-leaching residues of gold concentrate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1351963A (en) * | 2001-11-09 | 2002-06-05 | 清华大学 | Technological process for preparing iron oxide red from cyaniding gold extraction slag |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1351963A (en) * | 2001-11-09 | 2002-06-05 | 清华大学 | Technological process for preparing iron oxide red from cyaniding gold extraction slag |
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| CN1772628A (en) | 2006-05-17 |
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