Method of processing copper-vanadium wastes from purification of titanium tetrachloride

FIELD: chemistry.

SUBSTANCE: solid copper-vanadium wastes are leached with water to obtain copper-vanadium pulp, to which is added calcium hypochloride or clarified pulp from gas treatment facilities from titanium-magnesium production with concentration of active chlorine equal to 15-90 g/dm3, with ratio of calcium hypochlorite to the copper-vanadium pulp of (1.5-2.0):1. The pulp is held while stirring for 2-5 hours. Hydrochloric acid is added while stirring until achieving solution pH of 2.0-3.0. The suspension is filtered and the copper (II) solution is fed into a cementing apparatus. The precipitate in the form of a mixture of a reducing agent and copper powder is separated into copper powder and a reducing agent. The copper powder is washed, filtered and dried and iron impurities are removed by magnetic separation. After decantation, the reducing agent is returned to the cementing step.

EFFECT: high copper extraction and improved processing properties of the obtained copper powder.

10 cl, 3 ex

 

The invention relates to ferrous metallurgy, namely metallurgy of titanium, in particular the production of titanium tetrachloride to the recycling of waste generated during the purification of titanium tetrachloride.

One of the methods of purification of titanium tetrachloride from the impurities of vanadium is a chemical method of cleaning a copper powder. The treatment receiving waste - copper-vanadium water containing such valuable components such as copper and vanadium, the disposal of which allows to obtain the finished product and to reduce the emission of harmful components into the environment.

A method of refining chloride slurries of titanium dioxide production, containing titanium, copper and vanadium (autospid of the USSR №1228503, publ. 10.02.2000, bull. No. 4), including leaching waste water water treatment suspension oxidant is chlorine for 60 min, precipitation of hydroxides of the metals of the alkaline reagent is ammonium hydroxide to pH environment of 9.5, separating the precipitate from the solution by filtration and separation of copper from the filtrate by treatment with hydrogen chloride or hydrochloric acid. The precipitate was separated by filtration, washed and dried. The result is a finished product in the form of copper oxychloride. This allows to simplify the technology and to expand the range of products in the form of copper oxychloride.

The disadvantage of this method is that it aims to p the torching of bivalent copper oxychloride, which is a semi-finished product and allows you to get the cementation of copper in the form of marketable products. Use as oxidant ammonium hydroxide leads to the formation of ammonium compounds, which leads, in turn, to additional operations for the disposal and recycling of wastewater, increasing the cost of production of copper oxychloride.

A known method of producing copper powder from a copper-containing chloride solutions (patent RF №2052324, epubl), the number of General features adopted by the closest analogue is the prototype. Copper-vanadium sludge is formed during chemical purification of titanium tetrachloride, dissolved in water at a ratio of 1:3. The solution is injected sodium chloride and/or potassium chloride to the overall concentration of 50-300 kg/m3and hydrochloric acid in the amount of 10-50 kg/m3. The operation of the deposition of copper is carried out in column comentator with the filing of the original solution in the lower part. As metal-reducing use of iron scrap in the form of chips of low-carbon non-alloy steel, of calculation of 0.9-1.1 kg per 1 kg of copper contained in the solution. The resulting powder was washed with 20% hydrochloric acid and then dried in a vacuum drying apparatus at a temperature of 40-80°C for 40-60 minutes. The degree of extraction of copper is of 99.98% with a residual concentration of copper in solution of 0.01 kg/who 3.

The disadvantage of this method of processing copper-vanadium waste treatment process of titanium tetrachloride is that the presence of sodium chloride and/or potassium in the solution reduces the progression of monovalent copper in the divalent. This leads to the fact that the residual copper concentration in the exhaust solutions remains high (see table a patent specification No. 2052324, the index of the last column - 0,01-0,02 kg/m3or in terms of 10-20 mg/DM3). This leads to the pollution of waste water copper compounds that are environmentally harmful to the environment. In addition, particle cementation of copper receive dendritic form - in the form of crystals tree, branching forms, resulting in non-uniform and very fine friable granules (more than 95% of powdered copper get the size 0,016 mm), making it difficult to use, as well as packaging and transport (too much dust).

The technical result is to eliminate the disadvantages of the prototype and allows to increase the degree of extraction of the copper-vanadium waste of divalent copper and thereby reduce the content of copper compounds in the exhaust solutions, improve the particle size of copper powder stable shape and larger in size composition (0,315 mm), thereby to improve the technical properties of the powder is obraznoi copper.

The problem to which the invention is directed, is the reduction of environmental pollution. In addition, the proposed method allows to obtain copper powder superior quality and as a result send to the consumer powdered copper permanent hronologicheskogo composition.

The problem is solved in that in the method of processing copper-vanadium waste treatment process of titanium tetrachloride, comprising leaching the waste water to form a copper-vanadium pulp, processing the obtained slurry with hydrochloric acid, submission to the solution of reducing agent to obtain a precipitate metallic copper, washing and drying the precipitate to obtain the finished product, before applying hydrochloric acid to the slurry under stirring served calcium hypochlorite with a concentration of active chlorine, equal 15-90 g/DM3, stand under stirring for 2-5 hours, then added with stirring, hydrochloric acid until the pH of the solution equal to 2.0 to 3.0, the resulting suspension is filtered, the solution of divalent copper is served in comentator on the surface of the reducing agent, the mixture is heated to a temperature of 40-60°C and under stirring to carry out the recovery process, separating by filtration the precipitate in the form of a mixture of reducing agent and copper powder, the residue is separated by decanting method on a copper powder and restore the spruce, copper powder is treated with a stabilizer, washed, filtered, dried and purified from the impurities of iron magnetic separation.

In addition, as of calcium hypochlorite use bleached pulp of the gas treatment plant of titanium production. In addition, the ratio of calcium hypochlorite to the copper-vanadium pulp is (1,5-2,0):1.

In addition, the reducing agent fed to the recovery process in a quantity above the stoichiometric 1.0-2.0 times.

In addition, processing stabilizer is carried out at a mass ratio of copper powder:stabilizer equal to 1:(100-1000).

In addition, the stabilizer is used mylonaft.

In addition, the stabilizer is used as soap.

In addition, the stabilizer is used glycerin.

In addition, as the reductant used steel shavings.

In addition, the reducing agent after separation of the copper powder return to the stage grouting.

The use of calcium hypochlorite with a concentration of active chlorine, equal 15-90 g/DM3, submitting it to the slurry under stirring and extract with stirring for 2-5 hours allows to fully translate the copper compounds of monovalent form in the divalent form that allows you to more fully precipitate metallic copper from the dissolved soy is ineni copper and thereby reduce its content in the waste solutions from 10-20 up to 0.10-0.20 mg/DM 3.

Download in comentator reducing agent in a quantity above the stoichiometric 1.3-2.0 times and feed on the surface of the reductant solution of divalent copper process recovery when heated to a temperature of 40-60° allows you to more fully carry out the recovery process, and thereby reduce the content of copper compounds in the waste solutions from 10-20 up to 0.10-0.20 mg/DM3.

The process of washing the precipitate by decantation and the processing stabilizer of the copper powder allows you to increase the size of the granules and thereby improve the quality of commercial products.

Conducted by the applicant's analysis of the prior art, including searching by the patent and scientific and technical information sources and identify sources that contain information about the equivalents of the claimed invention, has allowed to establish that the applicant had not found the source, which is characterized by signs, identical all the essential features of the invention. The definition from the list of identified unique prototype as the most similar set of features analogue has allowed to establish the essential towards perceived by the applicant to the technical result of the distinctive features in the claimed method of processing copper-vanadium waste treatment process of titanium tetrachloride contained the claims. Therefore, the claimed invention meets the condition of "novelty."

To verify compliance of the claimed invention the term "inventive step", the applicant conducted an additional search of the known solutions to identify signs that match the distinctive features of the prototype of the characteristics of the claimed device. The stated signs are new and are not derived explicitly for the specialist, as in the prior art, as defined by the applicant, not identified impact provided the essential features of the claimed invention transformations to achieve a technical result. Therefore, the claimed invention meets the condition of "inventive step".

Industrial applicability the present invention is confirmed by examples of its specific implementation.

Example 1.

Copper-vanadium waste (TU 1718-436-05785388-2007) get in the cleaning process of technical titanium tetrachloride copper powder. The result is a solid residue of copper-vanadium water containing copper, chlorides of copper, compounds of titanium and vanadium in the form of oxides and oxychlorides, iron in chloride (see kN.: The production of titanium tetrachloride. - Baibekov M.K., Popov E, Cheprakov MM), metallurgy, 1980, p.53-63) according to the reactions:

CuTV+TiCl4=CuClTV+TiClI

TiClW +VOClI=TiClI+VOCl2TV

In a reactor equipped with a mechanical stirrer, pour 5,7 m3of water and with stirring load of 3.4 t shredded copper-vanadium waste composition, wt.%: Cu - 40, Ti - 4,7, V - 1,25, Fe - 0,16, CL - 40,5, the rest of the mixture. In the resulting slurry gradually under stirring for 5 hours metered 5.0 t solution of calcium hypochlorite waste from cleaning lime milk exhaust gases titanium-magnesium production with a concentration of active chlorine 84 DM3(THE 2147-466-05785388-2001) with a ratio of a solution of calcium hypochlorite to the copper-vanadium pulp, equal to 1.5:1. Calcium hypochlorite is obtained from the exhaust gas cleaning titanium-magnesium production with the milk of lime in the scrubber (see kN.: Production of magnesium. Ivanov A.I., Landres MB Prokofiev OV), metallurgy, 1979, s-362). The oxidation process odnoklasniki copper douglastown copper occurs by the reaction:

4CuCl+Ca(ClO)2+4HCl=4CuCl2+CaCl2+2H2O

After the filing of the calculated quantity of calcium hypochlorite slurry is maintained with stirring for 3 hours. Then for the dissolution of the formed hydroxides of copper and iron in the slurry is added under stirring in the amount of 0.9 tonnes of hydrochloric acid density of 1.1 g/cm3(THE 2122-480-05785388-2009) until the pH of 2.3. The resulting suspension fil the shape on the suction filter. The degree of transfer of copper from copper-vanadium oxide in a solution of divalent copper is 98%. Sediment composition, wt.%: Cu - 12,0, Fe - 1,2, Ti - 10,1, V - 3,5, Cl - 23,8, the rest is sent for further use as an additive in titanium-copper cast iron, and the filtrate, representing a solution duhalista copper with a concentration of 45 g/DM3directed to the process of cementation. The process of cementation is carried out in comentator in the form enamelled tank, equipped with a separated plate with holes and a steam jacket. Steel shavings (GOST 2787-75) in the amount of 1.8 tons in excess of the stoichiometry at 1.34 times, load in chementator, then on the surface of steel shavings pour a solution of divalent copper, the recovery process is carried out at a process temperature of 48°C duration 16 hours under stirring compressed air:

Cu2++Fe=Cu+Fe2+

As a result of processing a reducing agent steel - chips - chlorine ions pass into the ferric chloride and copper powder in a mixture with steel shavings deposited on the bottom of comentator. At the end of the recovery process, the mixture is filtered over a suction filter, the filtrate is sent to acid drainage and sediment in the form of a mixture of steel wool and copper powder repulper, again filtered. Then by the method of decanting, the precipitate is separated into copper powder and steel shavings. With the real chips are sent back to the recovery process. The obtained copper powder is weighed and the quantity 1 t sent for processing stabilizer such as mylanta (TU 0258-001-10105154-97) in an amount of 0.015 t and the mass ratio of copper powder:milonoff equal to 1:150. Then the precipitate is washed with water under stirring and filtered on a suction filter. Drying the copper powder is carried out in a vacuum drying Cabinet, then in a muffle furnace at a temperature of 85°C for 4 hours. After drying to remove the steel inclusions of copper powder is subjected to magnetic separation. The result is the cementation of copper in accordance with THE 1793-496-05785388-2009 "Copper cementation" of the following composition, wt.%: 90 Cu, 1,5 Fe, 0.20 chlorides, the rest of the mixture. The finished product is sent back to the cleaning process of technical titanium tetrachloride from vanadium or consumer.

Example 2.

All the same as in example 1, only the stabilizer is used as soap. The obtained copper powder is weighed and the quantity 1 t sent for processing stabilizer, such as soap (GOST 30266-95), in an amount of 0.01 t and the mass ratio of copper powder, soap, equal to 1:100. Then the precipitate is washed with water under stirring and filtered on a suction filter. Drying the copper powder is carried out in a vacuum drying Cabinet, then in a muffle furnace at a temperature of 85°C for 4 hours. After drying for removal the Oia steel inclusions of copper powder is subjected to magnetic separation. The result is the cementation of copper in accordance with THE 1793-496-05785388-2009 "Copper cementation" of the following composition, wt.%: 90 Cu, 1,5 Fe, 0.20 chlorides, the rest of the mixture. The finished product is sent back to the cleaning process of technical titanium tetrachloride from vanadium or consumer.

Example 3.

The obtained copper powder is weighed and the quantity 1 t sent for processing stabilizer such as glycerol (GOST 6824-96, GOST 7482-96), in the amount of 0.001 t and the mass ratio of copper powder:glycerol = 1:1000. Then the precipitate is washed with water under stirring and filtered on a suction filter. Drying the copper powder is carried out in a vacuum drying Cabinet, then in a muffle furnace at a temperature of 85°C for 4 hours. After drying to remove the steel inclusions of copper powder is subjected to magnetic separation. The result is the cementation of copper in accordance with THE 1793-496-05785388-2009 "Copper cementation" of the following composition, wt.%: 90 Cu, 1,5 Fe, 0.20 chlorides, the rest of the mixture. The finished product is sent back to the cleaning process of technical titanium tetrachloride from vanadium or consumer.

Thus, the proposed method allows 20-25 times to reduce the amount of copper compounds in the exhaust solutions that improves the environment, reduces environmental payments C is environmental pollution. In addition, the proposed method allows to obtain copper powder stable shapes and larger sizes hronologicheskogo composition (0,315 mm), which improves the technical properties of powdered copper and allows you to send the consumer powdered copper constant granulometric composition.

1. A method of processing a copper-vanadium waste treatment process of titanium tetrachloride, comprising leaching the waste water to form a copper-vanadium pulp, processing the obtained slurry with hydrochloric acid, submission to the solution of reducing agent to obtain a precipitate metallic copper, washing and drying the precipitate to obtain the finished product, characterized in that before the treatment with hydrochloric acid in the slurry with constant stirring served calcium hypochlorite with a concentration of active chlorine, equal 15-90 g/DM3, stand under stirring for 2-5 hours, then added with stirring, hydrochloric acid until the pH of the solution equal to 2.0 to 3.0, the resulting suspension is filtered, the resulting solution of divalent copper is served in comentator on the surface of the reducing agent, the mixture is heated to a temperature of 40-60°C and under stirring to carry out the recovery process, the resulting suspension is filtered, the precipitate in the form of a mixture of reducing agent and copper powder separated by decanting method on a copper powder and a reducing agent, copper is Orasac process stabilizer, washed, filtered, dried and purified from the impurities of iron magnetic separation.

2. The method according to claim 1, characterized in that the quality of calcium hypochlorite use bleached pulp of the gas treatment plant of titanium production.

3. The method according to claims 1 or 2, characterized in that the ratio of calcium hypochlorite to the copper-vanadium pulp is (1,5-2,0):1.

4. The method according to claim 1, characterized in that the reducing agent fed to the recovery process in a quantity above the stoichiometric 1.0-2.0 times.

5. The method according to claim 1, characterized in that the processing stabilizer is carried out at a mass ratio of copper powder:stabilizer equal to 1:(100-1000).

6. The method according to any one of claims 1 or 5, characterized in that the stabilizer is used mylonaft.

7. The method according to any one of claims 1 or 5, characterized in that the stabilizer is used as soap.

8. The method according to any one of claims 1 or 5, characterized in that the stabilizer is used glycerin.

9. The method according to claims 1 or 4, characterized in that as the reductant used steel shavings.

10. The method according to claims 1 or 4, characterized in that the reducing agent after separation of the copper powder return to the stage of recovery.



 

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2 cl, 1 tbl, 3 ex

FIELD: metallurgy.

SUBSTANCE: inventions relate to gold extraction from solutions with low concentration at presence of ions of other metals, for instance cleaning solutions of gold-extracting plants, brines of potassium manufacturing, geothermal water, water of brine lakes and salt water. Essence consists in that through powder of metal-restorative it is passed gold-containing solution with low concentration at presence of ions of other metals during 2-240 hours. In the capacity of metal-restorative it is used lead-plated zinc powder of grade +0.001 mm - 2 mm with lead content 1-90 wt %. or powders of metals, used at temperature of solution not less than 50°C and selected from the group: Zn, Fe, Ni, Pb, Sn, Sb, of grade +0.1 mm - 5 mm. Additionally before cementation powders are placed in cartridge. Received after cementation gold-containing concentrate is separated by means of intensive mechanical agitation, it is treated by nitric or acetic acid. Gold sediment is separated by filtration, dried and molten with fluxing additives with receiving of crude metal.

EFFECT: increase of effectiveness and selectivity of gold extraction from solutions with low concentration.

3 cl, 1 dwg, 3 ex

FIELD: metallurgy.

SUBSTANCE: invention relates to hydrometallurgy and can be used for processing of concentrates, industrial products and solid wastes containing metals. Proposed process comprises leaching of cake 3 n, by HCl solution at 70°C and L:S ratio of 2. Note here that leaching is performed in the presence of table salt of concentration making at least 120-140 g/dm3.

EFFECT: intensified leaching, higher yield.

4 tbl, 2 ex

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