CN112707432A - Method for comprehensively utilizing artificial rutile mother liquor in zinc concentrate treatment - Google Patents
Method for comprehensively utilizing artificial rutile mother liquor in zinc concentrate treatment Download PDFInfo
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- CN112707432A CN112707432A CN202011580229.9A CN202011580229A CN112707432A CN 112707432 A CN112707432 A CN 112707432A CN 202011580229 A CN202011580229 A CN 202011580229A CN 112707432 A CN112707432 A CN 112707432A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/04—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/06—Preparation of sulfur; Purification from non-gaseous sulfides or materials containing such sulfides, e.g. ores
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
Abstract
The invention discloses a comprehensive utilization method of artificial rutile mother liquor treated by zinc concentrate, which comprises the step of carrying out pressure oxidation leaching on the zinc concentrate and the artificial rutile mother liquor. The advantages are that: (1) the artificial rutile mother liquor is used for pressurizing, oxidizing and leaching zinc concentrate, zinc in the zinc concentrate reacts with hydrochloric acid to generate a zinc chloride product, sulfur and iron are oxidized to generate elemental sulfur and iron oxide, and hydrochloric acid in the mother liquor and valuable substances in the zinc concentrate are effectively utilized. (2) The zinc concentrate is leached by pressure oxidation of the artificial rutile mother liquor, so that the technical problems of environmental protection and economy of acid and iron treatment in the treatment process of the artificial rutile mother liquor are solved. (3) The invention can obviously reduce the mother liquor treatment cost in the production process of the artificial rutile, reduce the environment-friendly waste treatment amount of the artificial rutile mother liquor, and reduce the production cost and the environment-friendly treatment cost. The invention has obvious economic benefit and feasible technology, thereby having better market popularization benefit.
Description
Technical Field
The invention relates to a chlorination-process titanium dioxide production technology, in particular to a byproduct treatment technology in the chlorination-process titanium dioxide production.
Background
The production and research of titanium dioxide at home and abroad show that theoretically, the titanium dioxide is feasible by directly using the titanium concentrate, and even the TiCl is directly chloridized by using the titanium concentrate to prepare TiCl4And FeCl3But FeCl as a by-product in the direct chlorination3Less use, if the direct chlorination process is adopted for production, FeCl3The large amount of the organic silicon compound is an environmental protection obstacle, pollutants are formed if the organic silicon compound is not treated, the environmental protection is affected, and the technical and economic indexes of the treatment process are affected if the organic silicon compound is treated, so that the organic silicon compound cannot be accepted by the market for industrial production at present. With the improvement of the national environmental protection requirement, the titanium dioxide produced by the chlorination process is taken as a recommended production process, and high-grade titanium-rich materials, high-titanium slag or artificial rutile are required to be adopted. The fluidized chlorination process is smooth, the chlorination residue is less, the treatment amount of three wastes is less, the environmental protection cost can be reduced, the economic benefit is good, and the method is adopted by foreign well-known enterprises. Even in the production of titanium dioxide by a sulfuric acid method, the acid-soluble titanium slag is used, so that the use amount of sulfuric acid can be reduced by using the acid-soluble titanium slag, the treatment amount of waste acid and wastewater is reduced, and the environmental protection cost and the corresponding environmental protection pressure can be reduced, so that the enrichment of titanium concentrate is an important link in the production of titanium dioxide in future. Ilmenite (FeTiO)3) Medium TiO 22The theoretical content is 52.63%, and ilmenite is divided into rock ore and placer ore in nature. The grade of the titanium concentrate selected from the rock ore is generally 42-48%, and the grade of the titanium concentrate selected from the placer ore is generally 50-64%.
In the world, more than 20 enrichment methods have been researched and proposed for the research on the enrichment method of titanium concentrate, and each treatment method has unique characteristics. But can be roughly classified into two types-dry and wet. The dry method comprises an electric furnace smelting method, a plasma smelting method, a selective chlorination method and other thermal reduction methods; the wet process comprising partial reductionHydrochloric acid leaching and partial reduction-sulfuric acid leaching (total acid leaching), full reduction-tarnishing and full reduction-FeCl3Leaching, and other chemical separation processes. However, at present, only the electric furnace melting method, the acid leaching method and the reduced corrosion method are industrially applied.
The electric furnace smelting method is a mature method, the process is simple, the by-product metallic iron can be directly applied, solid and liquid waste materials are not generated in the production process, electric furnace gas generated in smelting can be recycled, three wastes are few, the factory floor area is small, the method is the most economical and efficient method for preparing titanium-rich materials by titanium concentrate at present, but the method has limitation, the smelting process mainly comprises separation and iron removal, the capacity for removing nonferrous impurities is poor, even the ash content of a reducing agent added in smelting enters slag, the power consumption is large, and the method is generally used in areas with sufficient electric power; the acid leaching method is the most effective method for removing impurities, and can effectively remove impurity iron and most of CaO, MgO and Al2O3MnO and other impurities to obtain TiO2The artificial rutile with higher mass fraction can be applied to all titanium concentrates in the world due to the best leaching effect of acid in the hydrochloric acid method, and can realize the regeneration, recovery and cyclic utilization of hydrochloric acid, but equipment needs to be made of special anticorrosive materials, the waste acid treatment energy consumption is high, and a cheap energy medium is needed to be selected for treatment; the by-product of the sulfuric acid method is ferrous sulfate, and the sulfuric acid leaching capacity is poor, so that the method is suitable for treating the titanium concentrate with higher grade. The acid leaching method has large quantity of three wastes and complex secondary flow path, thereby limiting the application of the acid leaching method; the reduction rust method takes coal as a reducing agent and fuel during reduction, only a small amount of hydrochloric acid or ammonium chloride is consumed during rust, the generated red mud and wastewater are close to neutrality and easy to treat, and the method is a method with less pollution and lower cost, but is only suitable for treating high-grade placer because the impurity removal capability is the weakest in all methods; the ferric chloride leaching method is that firstly the ferric oxide in the ilmenite is completely reduced into iron, and then the ferric chloride solution is used for leaching and removing iron to ensure that TiO2The enrichment method is obtained, and the process has low impurity removal capability and does not obtain industrial application; the selective chlorination method utilizes the difference of the chlorination thermodynamic properties of each component in the ilmenite to control the chlorinationThe chlorination condition during metallurgy only leads the ferric oxide component to be preferentially chloridized, separated and removed, but the obtained product has low grade, low technical and economic index and poor environmental protection condition, and the process is not adopted and applied by the market at present.
In different production process routes of the artificial rutile, the hydrochloric acid method artificial rutile production process has the advantages of high leaching speed, strong impurity removal capability, high product quality, suitability for treating various mineral sources and the like, becomes a mainstream process, and realizes industrialization very early.
In the production process of the synthetic rutile by the hydrochloric acid method, about 22-31% of hydrochloric acid is generally adopted to selectively leach iron oxide and most of CaO, MgO and Al in titanium concentrate2O3The impurities are mixed, washed and calcined to obtain the TiO-containing material2High-grade artificial rutile with the content of 90-96 percent. In the process of manufacturing the artificial rutile by the hydrochloric acid method, 5-7 t/acid-containing mother liquor, namely the artificial rutile mother liquor, is generated when 1 ton of rutile products are produced on average; the existing treatment process (lime neutralization method and pyrolysis method) has long process, large energy consumption, serious equipment corrosion and high comprehensive treatment cost, and restricts the large-scale application of the production process of the synthetic rutile by the hydrochloric acid method.
The national "sixty-five" and "seventy" have studied a lot on the comprehensive utilization and treatment of mother liquor of artificial rutile, such as utilizing acid-leaching mother liquor to introduce chlorine and oxidize to prepare liquid ferric trichloride, preparing iron powder by salting out crystallization method, treating mother liquor to produce iron red and brine by combination method, but because of many factors such as its technology, economy, market capacity, etc., have not been realized the industrialization is applied all the time, the hydrochloric acid regeneration mode adopted at present is recycled and recycled, but because of being limited by hydrochloric acid regeneration process, the hydrochloric acid concentration after regeneration is low, unfavorable to leaching and using circularly, meanwhile, the iron content in the mother liquor of leaching is low, acid regeneration treatment needs to evaporate a large amount of moisture, lead to the treatment process energy consumption is high, the cost is high, influence the technological economic benefits of rutile production.
The patent application publication No. CN 1657426A discloses a method for recovering and treating mother liquid of artificial rutile. The method is to heat and concentrate the artificial rutile mother liquor to ensure thatThe concentration of the ferric chloride is increased, and then the ferric chloride is sprayed into a roasting furnace for roasting, the ferric chloride is subjected to thermal decomposition reaction under the high-temperature oxidation atmosphere to form hydrogen chloride gas and solid oxide mainly containing ferric oxide, and the hydrogen chloride gas is absorbed by water to obtain regenerated hydrochloric acid. Although the method realizes the recycling of chloride ions, the energy consumption is high, about 640 ten thousand calories of heat are required for processing mother liquor generated by one ton of synthetic rutile, and the energy consumption is reduced to 800Nm of natural gas3On the left and right, and 70% of the heat of the treatment method is consumed by the latent heat of evaporation of water, under the policy and regulation that energy conservation is always advocated in the country for a long time, the method is obviously not sustainable; more importantly, the method does not purify and separate ferric chloride in the mother solution, so that the roasted product Fe is obtained2O3Contains more impurities such as chloride ions, MgO, CaO and the like, Fe2O3The purity can only reach about 90 percent, and the density is only 500kg/m3And the cost of packaging, stacking and transporting is high, so that the iron-smelting raw material is difficult to be directly used as the iron-smelting raw material.
The CMI company of Belgian Europe recently proposed that the artificial rutile mother liquor is treated by a fluidized bed calcination method, micron-sized ferric oxide powder is adopted as an induced crystallization center during calcination, the density of ferric oxide is greatly improved, the content of chloride ions is reduced, and the by-product can be directly used for smelting pig iron. However, the method has the defects of high energy consumption, high equipment investment and the like, and is difficult to popularize in areas with high energy price.
Patent No. ZL 90105886.6 discloses a method for extracting superfine ferric oxide from dilute hydrochloric acid rutile mother liquor. Adding scrap iron with the particle size of 2-25 mm into a rutile waste mother, treating at the temperature of 30-100 ℃ until the pH value is about 3.8, adding polyacrylamide for precipitation, oxidizing clear liquid by chlorine gas, adding a solution containing iron chloride into ammonia water in a semi-continuous mode under strong stirring at the temperature of 25-70 ℃ until the pH value is 5-8 to generate an amorphous ferric hydroxide colloid precipitate, preparing the precipitate into a slurry containing 0.5-15% of Fe, sequentially adding scrap iron, ferric salt, a surfactant and a substance with positive charge for treatment and filtration, drying and grinding a filter cake to prepare superfine ferric oxide yellow, and calcining the obtained ferric oxide yellow in a calcining furnace to obtain the ferric oxide powder. Although the method can obtain high-quality iron oxide yellow or iron oxide red, the process flow is long and complex, the operation control requirement is extremely high, toxic ammonia gas and chlorine gas are used, chlorine elements cannot be recycled, and a large amount of waste liquid containing chlorine ions as a byproduct can bring serious pollution to the environment.
The invention with the patent number ZL 89105794.3 discloses a method for continuously producing high-purity ferric oxide by ferrous salt, which comprises the steps of taking waste (or waste liquid) containing the ferrous salt as a raw material, adding the waste (or waste liquid) and prepared seed crystals into a group of mechanical stirring aeration tanks which are connected in series after purification treatment, adding ammonia gas to adjust the pH value to be 2.5-6, maintaining the temperature of the solution to be 75-90 ℃, and oxidizing and neutralizing ferrous ions to form crystalline alpha-Fe2O3The product, the separated ammonium-containing solution reacts with lime or magnesia in an ammonia distillation tank, and the recovered ammonia is returned to the neutralization oxidation tank for recycling. Although the method obtains the ferric oxide and the ammonia gas can be regenerated, the process flow is very complicated, the chlorine element is still not recycled, and a large amount of waste liquid containing calcium chloride and magnesium chloride is produced as a byproduct, thereby polluting the environment.
The invention patent with publication number CN 103159263A discloses a method for comprehensive utilization of artificial rutile mother liquor in zinc concentrate treatment, which comprises heating and pre-concentrating the artificial rutile mother liquor to make Fe in the mother liquor3+After the concentration is increased to more than 150g/L, the mixed iron source reacts in a fluidized bed reactor filled with HCl gas to increase the iron concentration of mother liquor, then the acidolysis solution is filtered, frozen and crystallized to obtain ferric trichloride crystals, and finally the crystals are roasted to obtain high-grade iron oxide red. The method has the advantages of simple process flow, easy operation, low energy consumption for treating the mother liquor, realization of the recycling of chlorine element in the mother liquor, recycling of all substances in the mother liquor, less by-products, energy conservation and environmental protection, purification and separation of ferric chloride in the mother liquor, and roasting to prepare high-grade iron red for market demand. The invention adopts the sulfuric acid residue or other iron-containing tailings to react with the mother liquor after the pre-evaporation, solves the problem of overlarge acidity in the mother liquor, and improves the quality of the mother liquorThe iron concentration in the rutile making mother liquor obtains a large amount of ferrous chloride and simultaneously utilizes the sulfate slag or other iron-containing tailings and the like, but the method has the problems that the obtained ferrous chloride has high impurity content, equipment is greatly corroded when the iron red is prepared by burning decomposition, and secondary pollution is easily caused by waste liquid and solid waste and the like.
The invention patent with publication number CN104528834A discloses a new method for resource utilization of artificial rutile mother liquor, which is to carry out resource utilization on TiO in the mother liquor2Colloid, mechanical impurities and partial residual metal ions are treated, the pretreated mother liquor is concentrated and crystallized to obtain ferrous crystals, the ferrous crystals are redissolved by deionized water, iron powder is added for reduction, and modified activated carbon is added for adsorption to obtain a pure ferrous oxide solution; preparing sodium carbonate solution, adding a certain amount of heavy metal precipitator into the sodium carbonate solution, and then adding activated carbon for purification treatment. Carrying out coprecipitation reaction on a pure ferrous solution and a sodium carbonate solution under certain conditions, simultaneously introducing air for oxidation, filtering and separating after the reaction is finished to obtain a filter cake, calcining the filter cake at a certain temperature, cooling, grinding to obtain an iron oxide red primary product, coating the iron oxide red primary product, and carrying out jet milling treatment to obtain a pigment-grade iron oxide red finished product. The method can obtain pigment-grade high-quality iron oxide red, and solves the problem of poor economic benefit of the conventional artificial rutile mother liquor treatment technology.
The invention discloses a novel method for recycling artificial rutile mother liquor, which is disclosed as CN105110784A, and comprises the steps of pretreating the mother liquor, concentrating and crystallizing the pretreated mother liquor to obtain ferrous chloride crystals, redissolving the ferrous chloride crystals by deionized water, adding iron powder for reduction, filtering, purifying and adsorbing the solution, separating to obtain a pure ferrous chloride solution, adding manganese salt and zinc salt in a stoichiometric ratio, carrying out chemical coprecipitation reaction on a mixed salt solution, filtering and separating to obtain a filter cake after the reaction is finished, washing, filtering, drying, precalcining, grinding, adding a binder and an additive for forming, and sintering at a high temperature under a certain calcination gradient to finally obtain manganese-zinc ferrite. The manganese-zinc ferrite with high reaction activity and excellent magnetic property can be obtained by the method, the problem that the quality of manganese, zinc and byproducts which are difficult to separate in the conventional artificial rutile mother liquor is poor is solved, and the utilization rate of elements in the mother liquor is improved.
The early artificial rutile mother liquor treatment technology almost recovers iron in the artificial rutile mother liquor without considering the recovery and utilization of chlorine, and the by-product contains a large amount of calcium and magnesium chloride salt which brings secondary pollution to the environment; the method for regenerating hydrochloric acid by spray roasting is mature, but equipment is easy to corrode and high in energy consumption, the concentration of the recovered regenerated acid is generally lower than 18%, the regenerated acid can be recycled after acid preparation, and the obtained iron oxide is high in impurity content, contains chlorine radicals and is low in recovery value. The processing cost is far from being offset.
The three patents with publication numbers of CN 103159263A, CN104528834A and CN105110784A all adopt a concentration and crystallization technology to separate and obtain relatively pure ferrous chloride, and then the ferrous chloride is calcined or chemically processed by using the ferrous chloride as a raw material to obtain iron oxide red or ferrite byproducts with higher value, so as to offset the comprehensive treatment cost of the artificial rutile mother liquor. In order to ensure the leaching efficiency in the production process of the artificial rutile, the mineral acid ratio is generally maintained at 1: 3-1: 4.5 (22% -26% hydrochloric acid), the theoretical excess of hydrochloric acid is over 50%, so that the mother liquor contains a large amount of residual acid and the concentration of iron ions is low, a large amount of water needs to be evaporated during crystallization separation, and in order to improve the crystallization efficiency, the refrigeration treatment is also needed, and the processes all need to consume a large amount of energy and increase the treatment cost.
Zinc concentrate is used as an important raw material of a zinc compound, sulfuric acid is generally adopted for pressure oxidation leaching to obtain a zinc sulfate solution, and various zinc products are obtained through electrolysis and smelting after purification treatment; the zinc chloride which is an important chemical raw material is usually obtained by oxidizing and roasting zinc oxide or zinc concentrate into oxide and then reacting the oxide with hydrochloric acid in the zinc chloride process, and the industrial zinc oxide raw material has high cost; the zinc concentrate releases oxysulfide during oxidation, which causes great damage to environmental protection.
Disclosure of Invention
The invention provides a comprehensive utilization method for treating artificial rutile mother liquor by using zinc concentrate, which aims to reduce the treatment cost of the artificial rutile mother liquor and solve the problem of environmental pollution in the process of producing zinc chloride by using zinc concentrate as a raw material.
The technical scheme adopted by the invention is as follows: the comprehensive utilization method of the artificial rutile mother liquor in the treatment of zinc concentrate comprises the step of carrying out pressure oxidation leaching on the zinc concentrate and the artificial rutile mother liquor.
As a further improvement of the invention, the usage ratio of the zinc concentrate to the synthetic rutile mother liquor is as follows: 1-5 mL of artificial rutile mother liquor is used for every 1g of zinc concentrate.
As a further improvement of the invention, the oxidant used in the pressure oxidation leaching process is oxygen.
As a further improvement of the invention, the pressure in the pressure oxidation leaching process is 0.5-1.0 MPa.
As a further improvement of the method, the pressure oxidation leaching reaction temperature is 120-180 ℃, and the reaction time is 2-5 h.
The invention can be implemented according to the following steps:
s1, weighing zinc concentrate and artificial rutile mother liquor in proportion, and putting into a pressure leaching tank;
s2, adjusting the reaction temperature to 120-180 ℃, and introducing oxygen into the pressure leaching tank in the whole leaching process to ensure that the pressure in the tank is 0.5-1.0 MPa until the leaching reaction is completed;
s3, carrying out solid-liquid separation on the reaction product to obtain a filtrate and a solid-phase substance, wherein the filtrate is a zinc chloride solution;
s4, obtaining elemental sulfur and ferric oxide through solid phase material selection.
The sorting method can adopt cyclone separation.
The invention has the beneficial effects that: 1) the invention overcomes the defects of the existing artificial rutile mother liquor treatment technology, and is characterized in that about 10 percent of residual hydrochloric acid in the used mother liquor is fully utilized, the artificial rutile leach mother liquor and the zinc concentrate are directly subjected to pressure oxidation leaching to eliminate toxic and harmful hydrogen sulfide gas generated by normal pressure leaching of the zinc concentrate, sulfur in the zinc concentrate is oxidized into elemental sulfur through pressure oxidation leaching, the elemental sulfur, iron in the mother liquor and iron in the zinc concentrate form solid phase substances to be separated out together, and elemental sulfur and iron oxide powder are obtained through separation; hydrolyzing the iron chloride in the mother liquor in the presence of oxide, separating out the iron oxide in a solid phase form, and separating out the chlorine in the mother liquor in a hydrochloric acid form; zinc in the zinc concentrate reacts with hydrochloric acid remained in the mother liquor and separated by hydrolysis to generate zinc chloride, and the zinc chloride is taken as a product for sale after being filtered, so that the treatment cost of the leached mother liquor in the production process of the artificial rutile is reduced, the utilization rate of the hydrochloric acid is improved, the waste discharge is reduced, and the method is an environment-friendly treatment method. 2) In the reaction process of the mother liquor and the zinc concentrate, only the zinc concentrate used for pressure oxidation leaching is consumed, oxygen in air is used for oxidation, the raw materials are easy to obtain, the zinc chloride solution obtained after the leaching reaction is an important chemical raw material, the added value is high, and meanwhile, the sulfur and iron in the zinc concentrate and the acid and iron in the mother liquor are both utilized, so that the method has high economic and technical benefits. 3) The test results show that: in the treatment process, 120g/L zinc chloride solution can be obtained; simple substance sulfur and ferric oxide can be obtained by selecting the leached solid phase substances. 4) The invention can obviously reduce the mother liquor treatment cost in the production process of the artificial rutile, reduce the environment-friendly waste treatment amount of the artificial rutile mother liquor, and reduce the production cost and the environment-friendly treatment cost.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
Preparing artificial rutile mother liquor:
the synthetic rutile mother liquor used in the examples was the mother liquor produced in situ: titanium concentrate is subjected to oxidation-reduction modification, and hydrochloric acid with the HCl mass fraction of 25% is used according to the acid-mineral (volume/mass) ratio: 3.0 leaching reaction, and then carrying out solid-liquid separation to obtain the product.
The first embodiment is as follows:
measuring 100mL of the artificial rutile mother liquor, putting the mother liquor into a polytetrafluoroethylene pressure leaching tank with the volume of 300mL, adding 30g of zinc concentrate, putting the pressure leaching tank into a drying oven with the temperature of 140 ℃ for constant temperature for 3 hours, introducing oxygen into the pressure tank in the whole leaching process to ensure that the pressure in the tank is 0.65Mpa, and then carrying out solid-liquid separation to obtain a filtrate which is a zinc chloride solution; and carrying out cyclone separation on the solid phase to obtain elemental sulfur and iron oxide.
Through detection, the zinc chloride solution contains 97.23g/L of zinc, the iron content is 1.08g/L, the content of HCL (hydrochloric acid) residue is 1.86 percent, and the recovery rate of zinc is 97.20 percent; the S content of the obtained elemental sulfur is 95.30 percent, the iron content is 2.24 percent, and the sulfur recovery rate is 95.20 percent; the total iron content of the obtained iron oxide was 59.84% and the sulfur content was 2.00%.
Example two:
measuring 150mL of the artificial rutile mother liquor, putting the mother liquor into a polytetrafluoroethylene pressure leaching tank with the volume of 300mL, adding 30g of zinc concentrate, putting the pressure leaching tank into a drying oven with the temperature of 140 ℃ for constant temperature for 3 hours, introducing oxygen into the pressure tank in the whole leaching process to ensure that the pressure in the tank is 0.65Mpa, and then carrying out solid-liquid separation to obtain a filtrate which is a zinc chloride solution; and carrying out cyclone separation on the solid phase to obtain elemental sulfur and iron oxide.
Through detection, the obtained zinc chloride solution contains 64.69g/L of zinc, the iron content is 3.28g/L, the residual acid HCL is 2.64 percent, and the zinc recovery rate is 97.80 percent; the S content of the obtained elemental sulfur is 96.70 percent, the iron content is 1.68 percent, and the sulfur recovery rate is 96.62 percent; the total iron content of the obtained iron oxide was 61.64% and the sulfur content was 1.46%.
Example three:
measuring 100mL of the artificial rutile mother liquor, putting the mother liquor into a polytetrafluoroethylene pressure leaching tank with the volume of 300mL, adding 60g of zinc concentrate, putting the pressure leaching tank into a drying oven with the temperature of 140 ℃ for constant temperature for 3 hours, introducing oxygen into the pressure tank in the whole leaching process to ensure that the pressure in the tank is 0.65Mpa, and then carrying out solid-liquid separation to obtain a filtrate which is a zinc chloride solution; and carrying out cyclone separation on the solid phase to obtain elemental sulfur and iron oxide.
Through detection, the obtained zinc chloride solution contains 146.48g/L of zinc, the iron content is 2.49g/L, the content of HCL (residual acid) is 0.96 percent, and the recovery rate of zinc is 77.26 percent; the S content of the obtained elemental sulfur is 91.22%, the iron content is 4.58%, and the sulfur recovery rate is 72.35%; the total iron content of the obtained iron oxide was 25.80% and the sulfur content was 3.64%.
Claims (10)
1. The method for comprehensively utilizing the artificial rutile mother liquor in zinc concentrate treatment is characterized by comprising the following steps of: comprises the step of carrying out pressure oxidation leaching on zinc concentrate and synthetic rutile mother liquor.
2. The method for comprehensive utilization of the artificial rutile mother liquor processed by zinc concentrate according to claim 1, wherein the method comprises the following steps: the usage ratio of the zinc concentrate to the artificial rutile mother liquor is as follows: 1-5 mL of artificial rutile mother liquor is used for every 1g of zinc concentrate.
3. The method for comprehensive utilization of the artificial rutile mother liquor processed by zinc concentrate according to claim 1, wherein the method comprises the following steps: the oxidant adopted in the pressure oxidation leaching process is oxygen.
4. The method for comprehensive utilization of the artificial rutile mother liquor processed by zinc concentrate according to claim 1, wherein the method comprises the following steps: the pressure in the pressure oxidation leaching process is 0.5-1.0 MPa.
5. The method for comprehensive utilization of the artificial rutile mother liquor processed by zinc concentrate according to claim 1, wherein the method comprises the following steps: the pressure oxidation leaching reaction temperature is 120-180 ℃, and the reaction time is 2-5 h.
6. The method for comprehensively utilizing the artificial rutile mother liquor in the zinc concentrate treatment according to any one of claims 1 to 5, is characterized by comprising the following steps:
s1, weighing zinc concentrate and artificial rutile mother liquor in proportion, and putting into a pressure leaching tank;
s2, adjusting the reaction temperature to 120-180 ℃, and introducing oxygen into the pressure leaching tank in the whole leaching process to ensure that the pressure in the tank is 0.5-1.0 MPa until the leaching reaction is completed;
s3, carrying out solid-liquid separation on the reaction product to obtain a filtrate and a solid-phase substance, wherein the filtrate is a zinc chloride solution;
s4, obtaining elemental sulfur and ferric oxide through solid phase material selection.
7. The method for comprehensive utilization of the artificial rutile mother liquor processed by zinc concentrate as claimed in claim 7, wherein the method comprises the following steps: the sorting method is cyclone separation.
8. The zinc chloride solution prepared by the method for comprehensively utilizing the artificial rutile mother liquor treated by the zinc concentrate as claimed in any one of claims 1 to 7.
9. Elemental sulphur obtained by the process for the comprehensive utilization of artificial rutile mother liquor from zinc concentrate treatment as claimed in claim 6 or 7.
10. Iron oxide produced by the method of comprehensive utilization of the artificial rutile mother liquor treated by zinc concentrate as claimed in claim 6 or 7.
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