CN1313379C - Prepn process of iron red with salfated roasted dreg of sulfur containing aurin ore - Google Patents

Abstract

The invention discloses a method for preparing iron red by sulphating roasting slag with sulfur-containing gold concentrate, which comprises the following steps: (1) adding 30-60% sulfuric acid and roasting slag into a reaction kettle, and the weight ratio of the two is 1: 2-10, stirring, adding co-solvent, the weight ratio of co-solvent and calcined slag is 1: 1-100, reacting at 60-100 °C for 1-6 hours, and filtering to obtain filtrate and residue after the reaction is complete; (2 ) neutralize the filtrate obtained in step (1) with ammonia water, control the pH value to 1-2, then add ammonia water at 50-90° C., until the iron ions are partially precipitated, and add flocculant; (3) step (2) The obtained precipitate is washed until there is no sulfate ion, then dried, calcined at 300-700°C, and ground to the particle size required by the iron red pigment to obtain iron red. (1) Enlarging the raw materials for preparing iron red and increasing the utilization rate of tailings resources; (2) improving the follow-up cyanidation process for gold extraction, increasing the efficiency of cyanidation gold extraction by three to four percentage points, and reducing energy consumption; (3) reducing environmental pollution.

Description

A kind of method of preparing iron red by sulfated roasting slag of sulfur-containing gold concentrate

technical field

The present invention relates to a kind of industrial solid waste recycling, reduction and harmless technology, in particular to a method of using sulfur-containing gold concentrate to prepare iron red from the leaching solution after intensive acid dissolution of sulphated roasting slag. Carry out the method of comprehensive utilization iron element, reduce its environmental pollution.

Background technique

In the prior art, iron red is a very important chemical pigment or magnetic material used in industry. Such as patent CN1102626A, CN1177572A, generally use ferrous sulfate heptahydrate, a by-product of titanium dioxide production, pickling solution, electrolytic anode slime, sulfuric acid slag or iron concentrate, etc. as raw materials, and prepare iron red by oxidation method in the presence of iron sheet The disadvantage of this method is that high-quality iron sheets are used as raw materials, which may easily cause a shortage of raw materials or a high price of raw materials. In addition, in the enhanced acid dissolution of sulfur-containing gold concentrate sulphated roasting slag (application number 200410067020.7), the method for improving the leaching rate of gold and silver by acid leaching slag is proposed through enhanced acid leaching; the conventional utilization process of acid leaching slag is through Gold extraction by cyanidation, the content of ferric oxide, iron ferric oxide, lead and arsenic in the cyanide slag of gold extraction is relatively high, some of which are prepared by magnetic separation to produce inferior iron red, and some are pulled by cement plants to make auxiliary materials, because of high temperature combustion Release a large amount of polluting gases such as sulfur dioxide and arsenic trioxide, polluting the atmosphere. Some are piled up near the mine, which is easy to cause spontaneous combustion and pollute the atmosphere; at the same time, the harmful cyanide ions and metal ions contained in the cyanide slag are also easy to flow into the water or soil, causing environmental pollution, so it is necessary to deal with it. Turning waste into treasure.

Contents of the invention

The technical problem to be solved by the present invention is to provide a method for preparing iron red with sulfur-containing gold concentrate sulfated roasting slag, to make up for the deficiencies and defects of the prior art, so as to expand the raw materials for iron red production and reduce the impact of acid leaching slag on Environmental hazards to meet the needs of production.

In order to solve the above-mentioned technical problems, the technical solution adopted in the present invention is: a method for preparing iron red with sulfur-containing gold concentrate sulphated roasting slag, comprising the following steps: (1) adding 30 to 60% of Sulfuric acid and calcined slag, the weight ratio of the two is 1: 2 ~ 10, stirring, adding a cosolvent, the weight ratio of cosolvent and calcined slag is 1: 1 ~ 100, reacting at 60 ~ 100 ° C for 1 ~ 6 hours, After the reaction is complete, filter to obtain the filtrate and residue; 2) neutralize the filtrate obtained in step (1) with ammonia water, control the pH value to 1-2, then add ammonia water at 50-90°C until the iron ions are partially precipitated, and add flocculation (3) The precipitate obtained in step (2) is washed until there is no sulfate ion, then dried, and calcined at 300-700°C, and ground to the particle size required by the iron red pigment to obtain iron red, wherein, The co-solvent contains 1%-25% sodium ethylenediammonium tetraacetate (EDTA), 1%-30% CuO, 20%-30% Fe ₂ O ₃ , 40%-60% SiO ₂ and 0-9 % Al ₂ O ₃ mixture.

As a preferred technical solution: the flocculant is selected from one or more of alum, aluminum oxide, green vitriol (ferrous sulfate), ferric chloride, or organic flocculants.

In order to reduce costs, the co-solvent can be recycled and reused to leach the iron in the acid leaching residue; the filtrate from the production of iron red can also be reacted with alkali and distilled to recover ammonia and alkali and be reused.

The beneficial effects of the present invention are: using the roasting slag to leaching the leaching solution to prepare iron red can achieve the following effects: (1) expanding the raw materials for preparing iron red and increasing the utilization rate of tailings resources; (2) improving the subsequent cyanidation Process gold extraction, improve the efficiency of cyanidation gold extraction by three to four percentage points, reduce energy consumption; (3) reduce environmental pollution.

Description of drawings

Fig. 1 is the process flow diagram of iron red prepared by leaching solution after roasting slag leaching of the present invention

Detailed ways

The present invention will be described in further detail below in conjunction with the accompanying drawings. Refer to accompanying drawing 1.

Example 1

Add 60% sulfuric acid in a reactor with a stirrer, start the stirrer to stir, add the calcined slag at one time, the weight ratio of the calcined slag and the sulfuric acid solution is 2:1, and the weight ratio of the calcined slag and the co-solvent is 1:1, The composition of co-solvent is 1% sodium edetate, 30% CuO, 20% Fe ₂ O ₃ , 40% SiO ₂ and 9% Al ₂ O ₃ , react at 80°C for 6 hours, and the iron leaching rate is 100%, the leaching rate of gold and silver is over 98%. Filtrate, neutralize the filtrate with ammonia water until the pH value is 1, add the flocculant ferric chloride to remove the precipitate, separate the co-solvent, and then add ammonia water at 50°C until the iron ions are completely precipitated. After filtering, the filtrate is used to recover ammonia water and alkali, and the filter residue is washed, dried and calcined at 300°C. The calcined iron red is ground to the particle size required by the iron red pigment, that is, high-quality iron red can be obtained, and its quality index (see attached table 1) is better than the product quality standard required by the national standard GB1863-89.

Example 2

Add 30% sulfuric acid in the reactor with stirrer, start the mixer to stir, add calcined slag at one time, the weight ratio of calcined slag and sulfuric acid solution is 10:1, the weight ratio of calcined slag and co-solvent is 50:1, The composition of co-solvent is 25% sodium edetate, 1% CuO, 30% Fe ₂ O ₃ , 60% SiO ₂ The reaction temperature is 100°C, the reaction time is 1h, the iron leaching rate is 100%, gold and silver The extraction rate is above 98%. The extract was filtered, the temperature of the system was lowered to room temperature, and then filtered. The filtrate was neutralized with alkali to a pH value of 1.3, flocculant alum was added to remove the precipitate, the co-solvent was separated, and then ammonia water was added at 90°C until the iron ions were completely precipitated. After filtration, the filtrate is used to recover ammonia water and alkali, and the filter residue is washed, dried and calcined at 680°C. The calcined iron red is ground to the particle size required by the iron red pigment, and high-quality iron red that is better than the product quality standard required by the national standard GB1863-89 can be obtained.

Example 3

Add 45% sulfuric acid in the reactor with stirrer, start the mixer to stir, add calcined slag at one time, the weight ratio of calcined slag and sulfuric acid solution is 5: 1, the weight ratio of calcined slag and co-solvent is 100: 1, The composition of co-solvent is 10% sodium edetate, 2% CuO, 15% Fe ₂ O ₃ , 50% SiO ₂ and 5% Al ₂ O ₃ The reaction temperature is 60°C, the reaction time is 5h, iron leaching The extraction rate of gold and silver is 100%, and the extraction rate of gold and silver is over 98%. The extract was filtered, the temperature of the system was lowered to room temperature, and then filtered. The filtrate was neutralized with alkali until the pH value was 1.5, and the flocculant polyacrylamide was added to remove the precipitate, and the auxiliary solvent was separated, and then ammonia water was added at 90°C until the iron ions were completely precipitated. After filtration, the filtrate is used to recover ammonia water and alkali, and the filter residue is washed, dried and calcined at 500°C. The calcined iron red is ground to the particle size required by the iron red pigment, and high-quality iron red that is better than the product quality standard required by the national standard GB1863-89 can be obtained.

Example 4

Add 56% sulfuric acid in the reactor with stirrer, start the mixer to stir, add calcined slag at one time, the weight ratio of calcined slag and sulfuric acid solution is 5: 1, the weight ratio of calcined slag and cosolvent is 30: 1, The composition of co-solvent is 1% sodium edetate, 30% CuO, 10% Fe ₂ O ₃ , 50% SiO ₂ and 1% Al ₂ O ₃ The reaction temperature is 95°C, the reaction time is 6h, iron leaching The extraction rate of gold and silver is 100%, and the extraction rate of gold and silver is over 98%. The extract is filtered, the filtrate is neutralized with alkali to a pH value of 1, flocculant starch is added to remove the precipitate, the co-solvent is separated, and ammonia water is added at 70°C until the iron ions are completely precipitated. After filtration, the filtrate is used to recover ammonia water and alkali, and the filter residue is washed, dried and calcined at 700°C. The calcined iron red is ground to the particle size required by the iron red pigment, and high-quality iron red superior to the requirements of the national standard GB1863-89 can be obtained. The quality index of table 1 iron red product project Product quality index of the present invention National standard GB1863-89 color Approximate ~ Micro Approximate ~ Micro Total Calcium, Calcium Oxide (%) 0.1 <0.3 Relative tinting strength (%) 96 95 Volatile matter at 105°C (%) 0.01 1.0 Water soluble matter (%) 0.1 0.2 Oil absorption (ml/100g) 20 15～25 Iron content, Fe2O3% 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.