CN113846230B - Treatment method for improving solid-liquid separation effect after acid leaching treatment of titanium slag - Google Patents
Treatment method for improving solid-liquid separation effect after acid leaching treatment of titanium slag Download PDFInfo
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- CN113846230B CN113846230B CN202111244951.XA CN202111244951A CN113846230B CN 113846230 B CN113846230 B CN 113846230B CN 202111244951 A CN202111244951 A CN 202111244951A CN 113846230 B CN113846230 B CN 113846230B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/124—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
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- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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Abstract
The invention relates to a treatment method for improving the solid-liquid separation effect after acid leaching treatment of titanium slag, which comprises the following steps: the titanium slag is sequentially subjected to pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing, and then the titanium-containing liquid is obtained through solid-liquid separation. According to the treatment method provided by the invention, the titanium slag is treated in a specific treatment process, so that the solid-liquid separation efficiency of the treated slurry is obviously improved, and the solid-liquid separation time is obviously shortened under the condition of achieving the same amount of separated liquid.
Description
Technical Field
The invention relates to the field of material treatment, in particular to a treatment method for improving the solid-liquid separation effect of titanium slag after acid leaching treatment.
Background
At present, titanium resources are mainly added in vanadium-titanium magnetite, and ilmenite and vanadium-titanium magnetite concentrate can be obtained from vanadium-titanium magnetite raw ore through ore dressing. Wherein, ilmenite can be used as a raw material of titanium products such as sulfate process titanium white, artificial rutile and the like; the iron ore concentrate is mainly used for iron making, and the process flow is a blast furnace-converter method or a non-blast furnace method. Long flow of blast furnace-converter method, and CaTiO of titanium 3 The slag enters the blast furnace slag, cannot be utilized, and is stored in a large amount, so that the waste of resources is caused, and the environmental problem is easily caused; the non-blast furnace method has poor economy and high energy consumption, and the problem of titanium utilization is still not solved.
For example, CN106854702A discloses a new method for separating iron, vanadium and titanium in vanadium-titanium-iron ore concentrate by one-step conversion, which comprises the following steps: (1) Mixing and roasting vanadium-titanium-iron ore concentrate and additive with a reducing agent to obtain vanadium-containing pig iron and a vanadium-titanium-rich material; (2) Leaching the vanadium-rich titanium material in water, and filtering to obtain a vanadium-containing solution and titanium slag. Through a sodium-modification reduction coupling new process, a low-temperature molten-state multiphase reaction separation new system is constructed, the reduction of iron, the sodium modification of vanadium and the melting separation process of iron and vanadium-rich titanium slag are realized in one step, and three products including vanadium-containing pig iron, vanadium-containing solution and titanium slag are produced. Compared with the traditional flow of 'blast furnace-converter' or 'direct reduction-melting separation/grinding separation', the method has the remarkable advantages of short process flow, investment saving of fixed assets, low production cost, small environmental pollution, high comprehensive recovery rate and the like, provides a new technology for high-efficiency comprehensive utilization of the vanadium-titanium-iron ore resources, and has wide application prospect.
CN106222349A discloses a method and a device for treating iron-containing raw materials by using a molten pool smelting furnace, wherein the iron-containing raw materials are mixed with a reducing agent, added into the molten pool smelting furnace, oxygen-enriched air is blown into the molten pool, and smelting is carried out at 1200-1600 ℃ to realize the separation of iron and slag and obtain titanium slag. Compared with the traditional 'sintering/pelletizing-blast furnace smelting' or 'rotary hearth furnace reduction-electric furnace melting', the method has the remarkable advantages of short flow, strong raw material adaptability, high product quality, low energy consumption, small pollution and the like, is expected to provide a new technical direction for high-efficiency comprehensive utilization of iron-containing resources, and has wide application prospect.
However, the existing method for performing solid-liquid separation after acidolysis of titanium slag has the defects of poor separation effect and low separation efficiency.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a treatment method for improving the solid-liquid separation effect after acid leaching treatment of titanium slag, and solves the problems of low efficiency and poor separation effect during solid-liquid separation of acid leaching solution of titanium slag.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a treatment method for improving the solid-liquid separation effect of titanium slag after acid leaching treatment, which comprises the following steps: the titanium slag is sequentially subjected to pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing, and then the titanium-containing liquid is obtained through solid-liquid separation.
According to the treatment method provided by the invention, the titanium slag is treated in a specific treatment process, so that the solid-liquid separation efficiency of the treated slurry is obviously improved, and the solid-liquid separation time is obviously shortened under the condition of achieving the same amount of separation liquid.
As a preferable technical scheme of the invention, the titanium slag comprises the following components in percentage by mass: 20-30% of silicon dioxide and 8-12% of alumina.
In the present invention, the content of silica in the titanium slag is 20 to 30% by mass, and may be, for example, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, or the like, but is not limited to the above-mentioned values, and other combinations not shown in the above-mentioned range are also applicable.
In the present invention, the content of alumina in the titanium slag is 8 to 12% by mass, and may be, for example, 8%, 8.2%, 8.4%, 8.6%, 8.8%, 9%, 9.2%, 9.4%, 9.6%, 9.8%, 10%, 10.2%, 10.4%, 10.6%, 10.8%, 11%, 11.2%, 11.4%, 11.6%, 11.8%, or 12%, but is not limited to the above-mentioned values, and other combinations not specifically mentioned in this range are also applicable.
As the preferable technical scheme of the invention, the pretreatment is to mix the titanium slag, water and acid;
preferably, the mass ratio of water to titanium slag in the pretreatment is (2-3): 1, and for example, 2.
In the invention, the mixing sequence of the titanium slag, the water and the acid in the pretreatment can be that the titanium slag is firstly mixed with the water, and then a certain amount of acid is added to ensure that the final pH value of the slurry is 4-7, or the iron slag and a certain amount of mixed liquid of the acid and the water are mixed for treatment.
Preferably, the end point of the pretreatment is a slurry pH of 4 to 7, which may be, for example, 4, 4.2, 4.4, 4.6, 4.8, 5, 5.2, 5.4, 5.6, 5.8, 6, 6.2, 6.4, 6.6, 6.8 or 7, etc., but is not limited to the recited values, and other combinations not recited within this range are equally applicable.
In the invention, the first acid treatment object is filter residue obtained by solid-liquid separation after pretreatment.
In a preferred embodiment of the present invention, the temperature of the first acid treatment is 60 to 80 ℃, and may be, for example, 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃ or 80 ℃, but is not limited to the values listed, and other combinations not listed within the range are also applicable.
Preferably, the first acid treatment time is 30 to 180min, for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 30min, 130min, 140min, 150min, 160min, 170min, or 180min, etc., but is not limited to the recited values, and other combinations not recited within this range are also applicable.
Preferably, the mass ratio of the titanium slag to the first acid in the first acid treatment is (1-2): 1, and for example, 1.
Preferably, the first acid has a mass concentration of 50 to 98%, for example, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, or 98%, etc., but is not limited to the recited values, and other combinations not recited within this range are also applicable.
In a preferred embodiment of the present invention, the second acid treatment agent includes a second acid and a first auxiliary agent.
In a preferred embodiment of the present invention, the amount of the second acid added in the second acid treatment is 0.5 to 1 times the mass of the titanium slag, and may be, for example, 0.5 times, 0.55 times, 0.6 times, 0.65 times, 0.7 times, 0.75 times, 0.8 times, 0.85 times, 0.9 times, 0.95 times, or 1 time, but is not limited to the above-mentioned values, and other combinations not shown in this range are also applicable.
Preferably, the second acid treatment has a mass concentration of 10 to 20% of the second acid, for example, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5%, 15%, 15.5%, 16%, 16.5%, 17%, 17.5%, 18%, 18.5%, 19%, 19.5%, or 20%, and the like, but is not limited to the values listed, and other combinations not listed within this range are also applicable.
Preferably, the first auxiliary agent comprises 1 or a combination of at least 2 of white carbon black, diatomite, charcoal powder or cellulose.
Preferably, the amount of the first auxiliary agent added in the second acid treatment is 0.04 to 0.16 times, for example, 0.04 times, 0.05 times, 0.06 times, 0.07 times, 0.08 times, 0.09 times, 0.1 times, 0.11 times, 0.12 times, 0.13 times, 0.14 times, 0.15 times, or 0.16 times the mass of the titanium slag, but is not limited to the above-mentioned values, and other combinations not listed in this range are also applicable.
In a preferred embodiment of the present invention, the temperature of the second acid treatment is 65 to 80 ℃ and may be, for example, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 80 ℃, 81 ℃, 82 ℃, 83 ℃, 84 ℃ or 85 ℃, but is not limited to the above-mentioned values, and other combinations not shown in the above range are also applicable.
Preferably, the second acid treatment time is 30 to 180min, for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 30min, 130min, 140min, 150min, 160min, 170min, or 180min, etc., but is not limited to the recited values, and other combinations not recited within this range are equally applicable.
As a preferable technical scheme of the invention, the second auxiliary agent is added 5-7min before the stirring treatment.
Preferably, the second adjuvant comprises 1 or a combination of at least 2 of polyethylene glycol, alkyl benzene sulfonate or triethanolamine.
In the present invention, the molecular weight of the polyethylene glycol is not less than 6000, and may be, for example, 6000, 6100, 6200, 6300, 6400, 6500, 6600, 6700, 6800, 6900, 7000, 7100, 7200, 7300, 7400, 7500, 7600, 7800, 8000 or 8500, etc., but not limited to the values mentioned, and other combinations not listed within the range are also applicable.
Preferably, the alkylbenzene sulfonate has 12 to 18 carbon atoms, such as 12, 13, 14, 15, 16, 17 or 18, but not limited to the recited values, and other combinations not recited within this range are also applicable.
Preferably, the second auxiliary agent has a mass concentration of 3 to 10%, for example, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, or 10%, etc., but is not limited to the recited values, and other combinations not recited within this range are also applicable.
Preferably, the second auxiliary agent is added in an amount of 0.02 to 0.2 times the volume of the slurry obtained by the second acid treatment, for example, 0.02 times, 0.03 times, 0.04 times, 0.05 times, 0.06 times, 0.07 times, 0.08 times, 0.09 times, 0.1 times, 0.11 times, 0.12 times, 0.13 times, 0.14 times, 0.15 times, 0.16 times, 0.17 times, 0.18 times, 0.19 times, or 0.2 times, and the like, but is not limited to the values listed, and other combinations not listed in this range are also applicable.
In a preferred embodiment of the present invention, the stirring treatment is carried out for 10 to 20min, for example, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min, or 20min, but not limited to the above-mentioned values, and other combinations not listed in this range are also applicable.
Preferably, the stirring treatment temperature is 60-80 ℃, for example can be 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃ or 80 ℃ and so on, but not limited to the cited numerical value, in the range of other not listed combinations are also applicable.
Preferably, the rotation speed of the stirring treatment is 200-300r/min, such as 200r/min, 210r/min, 220r/min, 230r/min, 240r/min, 250r/min, 260r/min, 270r/min, 280r/min, 290r/min or 300r/min, but not limited to the values listed, and other combinations not listed in this range are equally applicable.
In a preferred embodiment of the present invention, the temperature of the standing is 10 to 80 ℃ and may be, for example, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃, but is not limited to the values listed, and other combinations not listed within this range are also applicable.
Preferably, the time of the standing is 30-120min, for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min or 120min, etc., but not limited to the recited values, and other combinations not recited in the range are also applicable.
As a preferred technical solution of the present invention, the processing method includes the following steps: sequentially carrying out pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing on the titanium slag, and then carrying out solid-liquid separation to obtain a titanium-containing liquid;
the titanium slag comprises the following components in percentage by mass: 20-30% of silicon dioxide, 8-12% of aluminum oxide;
the pretreatment is to mix titanium slag, water and acid; the mass ratio of water to titanium slag in the pretreatment is (2-3) to 1; the end point of the pretreatment is that the pH value of the slurry is 4-7;
the temperature of the first acid treatment is 60-80 ℃; the time of the first acid treatment is 30-180min; the mass ratio of the titanium slag to the first acid in the first acid treatment is (1-2) to 1; the mass concentration of the first acid is 50-98%;
the second acid treatment reagent comprises a second acid and a first auxiliary agent; the adding amount of the second acid in the second acid treatment is 0.5-1 time of the mass of the titanium slag; the mass concentration of the second acid in the second acid treatment is 10-20%; the first auxiliary agent comprises 1 or at least 2 of white carbon black, diatomite, charcoal powder or cellulose; the addition amount of the first auxiliary agent in the second acid treatment is 0.04-0.16 times of the mass of the titanium slag; the temperature of the second acid treatment is 65-80 ℃; the time for treating the second acid is 30-180min;
adding a second auxiliary agent 5-7min before the stirring treatment is finished; the second auxiliary agent comprises 1 or a combination of at least 2 of polyethylene glycol, alkyl benzene sulfonate or triethanolamine; the number of carbon atoms of the alkylbenzene sulfonate is 12-18; the mass concentration of the second auxiliary agent is 3-10%; the addition amount of the second auxiliary agent is 0.02-0.2 times of the volume of the slurry obtained by the second acid treatment; the stirring treatment time is 10-20min; the temperature of the stirring treatment is 60-80 ℃; the rotating speed of the stirring treatment is 200-300r/min;
the standing temperature is 10-80 ℃; the standing time is 30-120min.
In the invention, the titanium slag is slag obtained after vanadium is eluted by alkali molten slag water after iron is extracted from the vanadium titano-magnetite by a sodium salt reduction-melting coupling process, the process realizes iron reduction melting and sodium salt oxidation of vanadium, and the titanium slag has good activity and is easy to extract.
In the present invention, the acid used may be inorganic acid such as sulfuric acid, hydrochloric acid or nitric acid, or other organic acid capable of achieving the effect, such as oxalic acid, citric acid or malic acid.
In the invention, the impurity element types in the titanium slag are determined according to the raw ore composition of the titanium slag.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) The invention provides a method for improving the filtering performance of slurry treated by high-silicon aluminum titanium slag, which can be directly carried out in the acid leaching and aging stage without additional equipment investment and is simple and easy to operate.
(2) The invention uses less additive, has low treatment cost, can greatly improve the production efficiency and has high cost performance. The time for solid-liquid separation is shortened by more than 50% when the same liquid volume is reached in the solid-liquid separation.
(3) According to the invention, the acid treatment and stirring process containing a specific auxiliary agent is adopted, so that the solid-liquid separation efficiency of the pickle liquor is improved. Solves the problem that titanium slag acidolysis titanium slurry of the sodium modification method of the high-silicon aluminum vanadium titano-magnetite is difficult to filter, and paves the way for the industrial implementation of the comprehensive application of the vanadium titano-magnetite.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a treatment method for improving the solid-liquid separation effect after acid leaching treatment of titanium slag, which comprises the following steps: sequentially carrying out pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing on the titanium slag, and then carrying out solid-liquid separation to obtain a titanium-containing solution;
the titanium slag comprises the following components in percentage by mass: 25% of silicon dioxide, 10% of aluminum oxide, and the balance of 40% of titanium oxide and impurity elements of Fe, ca, mg, al and Si;
the pretreatment is to mix titanium slag, water and sulfuric acid; the mass ratio of water to titanium slag in the pretreatment is 2.5; the end point of the pretreatment is that the pH value of the slurry is 4;
the temperature of the first acid treatment is 70 ℃; the time of the first acid treatment is 100min; the mass ratio of the titanium slag to the first acid (sulfuric acid) in the first acid treatment is 1.5; the mass concentration of the first acid (sulfuric acid) is 75%;
the reagent for treating the second acid is a second acid (sulfuric acid) and a first auxiliary agent; the adding amount of second acid (sulfuric acid) in the second acid treatment is 0.75 time of the mass of the titanium slag; the mass concentration of the second acid (sulfuric acid) in the second acid treatment is 15%; the first auxiliary agent is diatomite and charcoal powder in a mass ratio of 1; the addition amount of the first additive in the second acid treatment is 0.0.1 time of the mass of the titanium slag; the temperature of the second acid treatment is 72 ℃; the time for the second acid treatment is 180min;
adding a second auxiliary agent 6min before the stirring treatment is finished; the second auxiliary agent is triethanolamine; the mass concentration of the second auxiliary agent is 7%; the addition amount of the second auxiliary agent is 0.1 time of the volume of the slurry obtained by the second acid treatment; the stirring treatment time is 15min; the temperature of the stirring treatment is 70 ℃; the rotating speed of the stirring treatment is 250r/min;
the standing temperature is 45 ℃; the standing time is 77min.
The separation effect in the solid-liquid separation after the treatment by the treatment method of the embodiment is obviously improved, and the separation time is shortened by 60% compared with the solid-liquid separation time in the case of directly performing the separation after leaching to reach the same liquid amount.
Example 2
The embodiment provides a treatment method for improving the solid-liquid separation effect after acid leaching treatment of titanium slag, which comprises the following steps: sequentially carrying out pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing on the titanium slag, and then carrying out solid-liquid separation to obtain a titanium-containing solution;
the titanium slag comprises the following components in percentage by mass: 30 percent of silicon dioxide, 8 percent of aluminum oxide, and the balance of 40 percent of titanium oxide and impurity elements of Fe, ca, mg, al and Si;
the pretreatment is to mix titanium slag, water and hydrochloric acid; the mass ratio of water to titanium slag in the pretreatment is 2; the end point of the pretreatment is that the pH value of the slurry is 6;
the temperature of the first acid treatment is 80 ℃; the time of the first acid treatment is 30min; the mass ratio of the titanium slag to the first acid (sulfuric acid) in the first acid treatment is 1; the mass concentration of the first acid (sulfuric acid) is 98%;
the reagent for treating the second acid is second acid (hydrochloric acid) and a first auxiliary agent; the adding amount of second acid (hydrochloric acid) in the second acid treatment is 0.5 time of the mass of the titanium slag; the mass concentration of the second acid (hydrochloric acid) in the second acid treatment is 10%; the first auxiliary agent is charcoal powder and cellulose with the mass ratio of 1; the addition amount of the first auxiliary agent in the second acid treatment is 0.04 times of the mass of the titanium slag; the temperature of the second acid treatment is 80 ℃; the time for treating the second acid is 100min;
adding a second auxiliary agent 5min before the stirring treatment is finished; the second auxiliary agent is sodium dodecyl benzene sulfonate; the mass concentration of the second auxiliary agent is 3%; the addition amount of the second auxiliary agent is 0.02 time of the volume of the slurry obtained by the second acid treatment; the stirring treatment time is 10min; the temperature of the stirring treatment is 60 ℃; the rotating speed of the stirring treatment is 200r/min;
the standing temperature is 80 ℃; the standing time is 30min.
The separation effect in the solid-liquid separation after the treatment by the treatment method of the embodiment is obviously improved, and the separation time is shortened by 50% compared with the solid-liquid separation time in the case of directly performing the separation after leaching to reach the same liquid amount.
Example 3
The embodiment provides a treatment method for improving the solid-liquid separation effect after acid leaching treatment of titanium slag, which comprises the following steps: sequentially carrying out pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing on the titanium slag, and then carrying out solid-liquid separation to obtain a titanium-containing liquid;
the titanium slag comprises the following components in percentage by mass: 20% of silicon dioxide, 12% of aluminum oxide, and the balance of 42% of titanium oxide and impurity elements of Fe, ca, mg, al and Si;
the pretreatment is to mix titanium slag, water and acid (nitric acid); the mass ratio of water to titanium slag in the pretreatment is 3; the end point of the pretreatment is that the pH value of the slurry is 7;
the temperature of the first acid treatment is 60 ℃; the time of the first acid treatment is 180min; the mass ratio of the titanium slag to the first acid (nitric acid) in the first acid treatment is 2; the mass concentration of the first acid (nitric acid) is 50%;
the reagent for treating the second acid is the second acid and the first auxiliary agent; the adding amount of second acid (nitric acid) in the second acid treatment is 1 time of the mass of the titanium slag; the mass concentration of the second acid (nitric acid) in the second acid treatment is 20%; the first auxiliary agent is white carbon black; the addition amount of the first auxiliary agent in the second acid treatment is 0.16 times of the mass of the titanium slag; the temperature of the second acid treatment is 65 ℃; the time for treating the second acid is 30min;
adding a second auxiliary agent 7min before the stirring treatment is finished; the second auxiliary agent is polyethylene glycol (molecular weight is 6000); the mass concentration of the second auxiliary agent is 10%; the addition amount of the second auxiliary agent is 0.2 time of the volume of the slurry obtained by the second acid treatment; the stirring treatment time is 5min; the temperature of the stirring treatment is 80 ℃; the rotating speed of the stirring treatment is 300r/min;
the standing temperature is 10 ℃; the standing time is 120min.
The separation effect in the solid-liquid separation after the treatment by the treatment method of the embodiment is obviously improved, and the separation time is shortened by 55% compared with the solid-liquid separation time in the case of directly performing the separation after leaching to achieve the same liquid amount.
Comparative example 1
The only difference from example 1 is that the first auxiliary and the second auxiliary are added simultaneously in the first acid treatment.
The separation effect of the solid-liquid separation after the treatment by the treatment method of the comparative example is obviously improved, and the separation time is shortened by 10 percent compared with the solid-liquid separation time under the condition of directly performing the separation after leaching to achieve the same liquid amount.
Comparative example 2
The only difference from example 1 is that the solid-liquid separation was not conducted before the solid-liquid separation, that is, the solid-liquid separation was conducted directly after the stirring treatment.
The separation effect of the solid-liquid separation after the treatment by the treatment method of the comparative example is obviously improved, and the separation time is shortened by 8% compared with the solid-liquid separation time under the condition that the separation is directly carried out after leaching to reach the same liquid amount.
Comparative example 3
The only difference from example 1 is that the second auxiliary agent is added in the first treatment and the first auxiliary agent is added in the stirring treatment.
The separation effect of the solid-liquid separation after the treatment by the treatment method of the comparative example is obviously improved, and the separation time is basically unchanged compared with the solid-liquid separation time under the condition that the separation is directly carried out after leaching to reach the same liquid amount.
Comparative example 4
The only difference from example 1 is that the first auxiliary and the second auxiliary are added simultaneously in the stirring process.
The separation effect of the solid-liquid separation after the treatment by the treatment method of the comparative example is obviously improved, and the separation time is shortened by 3% compared with the solid-liquid separation time under the condition of directly separating the leached liquid to the same liquid amount.
As can be seen from the results of the above examples and comparative examples, the scheme provided by the invention realizes the efficient solid-liquid separation of the treated slurry by adopting a specific treatment process for the titanium slag.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications, equivalent substitutions of selected elements of the present invention, additions of auxiliary elements, selection of specific forms, etc., are intended to fall within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (23)
1. A treatment method for improving the solid-liquid separation effect after acid leaching treatment of titanium slag is characterized by comprising the following steps: sequentially carrying out pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing on the high-silicon aluminum vanadium titano-magnetite sodium modification method titanium slag, and then carrying out solid-liquid separation to obtain a titanium-containing liquid;
the second acid treatment reagent comprises a second acid and a first auxiliary agent; the first auxiliary agent comprises 1 or at least 2 of white carbon black, diatomite, charcoal powder or cellulose;
adding a second auxiliary agent 5-7min before the stirring treatment is finished; the second auxiliary agent comprises 1 or a combination of at least 2 of polyethylene glycol, alkyl benzene sulfonate or triethanolamine.
2. The treatment method according to claim 1, wherein the titanium slag comprises, in mass percent: 20-30% of silicon dioxide and 8-12% of aluminum oxide.
3. The treatment method according to claim 1, wherein the pretreatment is a mixed treatment of titanium slag, water and acid.
4. The treatment method according to claim 3, wherein the mass ratio of water to titanium slag in the pretreatment is (2-3): 1.
5. The treatment method according to claim 1, wherein the end point of the pretreatment is a slurry pH of 4 to 7.
6. The treatment method according to claim 1, wherein the temperature of the first acid treatment is 60 to 80 ℃.
7. The treatment method according to claim 1, wherein the time of the first acid treatment is 30 to 180min.
8. The treatment method according to claim 1, wherein the mass ratio of the titanium slag to the first acid in the first acid treatment is (1-2): 1.
9. The treatment method according to claim 1, wherein the mass concentration of the first acid is 50 to 98%.
10. The process of claim 1 wherein the second acid is added in an amount of 0.5 to 1 times the mass of the titanium slag.
11. The process of claim 1, wherein the second acid treatment comprises a second acid mass concentration of 10 to 20%.
12. The treatment method according to claim 1, wherein the addition amount of the first auxiliary agent in the second acid treatment is 0.04-0.16 times of the mass of the titanium slag.
13. The process of claim 1, wherein the second acid treatment temperature is 65 to 80 ℃.
14. The process of claim 1, wherein the second acid is treated for a period of 30 to 180min.
15. The process of claim 1 wherein said alkylbenzene sulfonate has from 12 to 18 carbon atoms.
16. The treatment method according to claim 1, wherein the second auxiliary agent has a mass concentration of 3 to 10%.
17. The process of claim 1 wherein the second additive is added in an amount of from 0.02 to 0.2 times the volume of the slurry resulting from the treatment with the second acid.
18. The process according to claim 1, wherein the stirring treatment is carried out for a period of 10 to 20min.
19. The process according to claim 1, wherein the temperature of the agitation treatment is 60 to 80 ℃.
20. The process according to claim 1, wherein the stirring process is carried out at a speed of from 200 to 300r/min.
21. The process according to claim 1, wherein the temperature of the standing is 10 to 80 ℃.
22. The process according to claim 1, wherein the standing time is 30 to 120min.
23. The process according to any one of claims 1 to 22, characterized in that it comprises the following steps: sequentially carrying out pretreatment, solid-liquid separation, first acid treatment, second acid treatment, stirring treatment and standing on the high-silicon aluminum vanadium titano-magnetite sodium modification method titanium slag, and then carrying out solid-liquid separation to obtain a titanium-containing liquid;
the titanium slag comprises the following components in percentage by mass: 20-30% of silicon dioxide, 8-12% of aluminum oxide;
the pretreatment is to mix titanium slag, water and acid; the mass ratio of water to titanium slag in the pretreatment is (2-3) to 1; the end point of the pretreatment is that the pH value of the slurry is 4-7;
the temperature of the first acid treatment is 60-80 ℃; the time of the first acid treatment is 30-180min; the mass ratio of the titanium slag to the first acid in the first acid treatment is (1-2) to 1; the mass concentration of the first acid is 50-98%;
the second acid treatment reagent comprises a second acid and a first auxiliary agent; the adding amount of the second acid in the second acid treatment is 0.5-1 time of the mass of the titanium slag; the mass concentration of the second acid in the second acid treatment is 10-20%; the first auxiliary agent comprises 1 or at least 2 of white carbon black, diatomite, charcoal powder or cellulose; the addition amount of the first additive in the second acid treatment is 0.04-0.16 times of the mass of the titanium slag; the temperature of the second acid treatment is 65-80 ℃; the time for treating the second acid is 30-180min;
adding a second auxiliary agent 5-7min before the stirring treatment is finished; the second auxiliary agent comprises 1 or at least 2 of polyethylene glycol, alkyl benzene sulfonate or triethanolamine; the number of carbon atoms of the alkylbenzene sulfonate is 12-18; the mass concentration of the second auxiliary agent is 3-10%; the addition amount of the second auxiliary agent is 0.02-0.2 times of the volume of the slurry obtained by the second acid treatment; the stirring treatment time is 10-20min; the temperature of the stirring treatment is 60-80 ℃; the rotating speed of the stirring treatment is 200-300r/min;
the standing temperature is 10-80 ℃; the standing time is 30-120min.
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