CN101514031A - Titanium ore acidolysis method through sulfuric acid process - Google Patents
Titanium ore acidolysis method through sulfuric acid process Download PDFInfo
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Abstract
The invention relates to an improved method for the titanium ore acidolysis through sulfuric acid in the process of producing titanium white through a sulfuric acid process. The method is characterized in that: the method comprises the following steps: firstly premixing dilute waste acid produced by titanium white production after concentration and trash extraction with the titanium ore; and then adding the premixed ore slurry into an acidolysis pot, and then adding concentrated sulfuric acid so as to initiate a main reaction through the dilution heat produced by the added concentrated acid. The method has the advantages of: 1) improving the reutilization amount of titanium white waste acid and reducing the cost of concentrated waste acid; 2) removing a sulfuric acid cooling link so as to simplify the operation; 3) improving the operational conditions of premixing and acidolysis so as to reduce the risk of technical accidents; and 4) strengthening the premixing intensity, improving the premixing effect, so that the acidolysis reaction is sufficient and the acidolysis rate is remarkably improved.
Description
Technical field
The present invention relates to improving one's methods of a kind of sulfuric acid process titanium ore acidolysis, particularly the production method that is used for the sulfuric acid method titanium pigment hydrolysis procedure is returned in the sulfur waste acid that produces in the sulfuric acid method titanium pigment production process.
Technical background
Titanium dioxide is a kind of fine white pigment, is widely used in fields such as coating, plastics, papermaking, printing ink, chemical fibre, food, electronics, and global output surpassed 5,000,000 tons in 2006, was a kind of important inorganic chemical product.Producing Titanium Dioxide is used sulfuric acid process and two kinds of production technique of chlorination process usually, sulfate process titanium dioxide technology starts from before and after the '20s in last century, because raw material is obtained easily, technology comparative maturity and being extensive use of at home, but the comprehensive utilization of the rare spent acid (about concentration 25%) that contains a large amount of impurity that produces in the sulfate process titanium dioxide production process is the difficult problem that sulfate process titanium dioxide is produced always.In early days, American-European countries once entered high sea with rare spent acid, at present, most of producer with in lime or the carbide slag and after, carry out slag and handle, both wasted resource, polluted environment again.
A lot of enterprises are devoted to the comprehensive utilization of rare spent acid always, and part enterprise utilizes spent acid to make products such as phosphate fertilizer.Certainly, the production that spent acid is directly used in sulfate process titanium dioxide also has a plurality of approach, tradition acidolysis operation is: the vitriol oil and breeze pre-mixing in the acidolysis pot before the acidolysis after the pre-dilution of employing, behind breeze and the vitriol oil thorough mixing, in the acidolysis pot, add rare spent acid again, water in the spent acid and sulfuric acid are had an effect and a large amount of heat of giving birth to, and cause main reaction with steam heating again.There is following problem in this operating process: at first, for the ease of the infiltration of the vitriol oil to perovskite powder, the vitriol oil must dilute in advance, after the part or all of vitriol oil is diluted (concentration that generally is diluted to 88-93%) in advance, it is complex acid, should further the cooling of the vitriol oil after dilution ability and whole breezes be carried out pre-mixing, the step complexity.Secondly, because what the vitriol oil and breeze carried out is solid-liquid reaction, be the effect that solid-liquid reaction is obtained, improve the acidolysis rate of follow-up acidolysis process, must be with the abundant premix of solid-liquid, but the acidolysis main reaction takes place during owing to the sulfuric acid of worrying 88-93% and breeze premix, generally pre-mixing intensity and pre-mixing time all are controlled in the lower scope, so just influenced premixing effect, be unfavorable for obtaining high acidolysis rate, even under this lower mixture strength, careless slightly, for example breeze is ground meticulously, the reactive behavior of titanium ore sulfuric acid high or that use with does not in advance have accidentalia such as sufficiently cooled all can cause causing the acidolysis main reaction in advance in the premix stage, causes the accident.And, this scheme is the leaching water with solid formation behind the initiation water of rare spent acid replacement acidolysis reaction or the acidolysis reaction, this method since rare spent acid without concentrating and removal of impurities, under acidolysis reaction is had relatively high expectations the prerequisite of sulfuric acid concentration, can not use in a large number, and a large amount of impurity of bringing into also can influence subsequent handling operation and quality product, and therefore, rare spent acid of Producing Titanium Dioxide system generation at present has only few part can directly turn back to recycle in the Producing Titanium Dioxide system.
At the problems referred to above, patent CN1376635A, CN1171777C etc. disclose some to sulfate process titanium dioxide rare spent acid concentrate, the method for removal of impurities, as spraying earlier concentrate, cooling, the vitriol oil (be generally 98% commercial acid) that separates spent acid after the removal of impurities and 93%-98% be mixed, thereby with diluting concentrated sulfuric acid is 90%-93%, and be cooled to below 45 ℃, the acid that is mixed after will diluting again mixes with breeze, after slurry behind the premix adds the acidolysis pot, add suitable water, cause the acidolysis main reaction.After spent acid is concentrated to more than 48%, most of impurity can be separated out in crystallization, further concentrate the consumption that returns that then can improve spent acid, it is dense high more to concentrate back acid, the utilization of spent acid is also big more, and cost is also high more, generally speaking, rare spent acid is concentrated to more than 70%, recycles after producing spent acid all could being returned the acidolysis system and the fresh vitriol oil that replenishes mixing.
The flow process of should existing concentrating waste acid returning usefulness still can't overcome following shortcoming: 1) owing to require to drop into the initial concentration that the sulfuric acid concentration of acidolysis pot is higher than acidolysis reaction, general requirement is greater than the acidolysis reaction initial concentration more than 4%, after guaranteeing adding initiation water, produce enough heat of dilution initiation main reactions, therefore, rare spent acid for satisfying arts demand, has successively experienced concentrating and dilution, cooling and heat-processed in utilizing process, cause the energy consumption height, complex process; 2) owing to the higher unsafe problems of using in the premix stage of sulfuric acid concentration is not resolved, therefore in the premix process, higher or excessive agitation, premix overlong time as the dense and sour temperature of tartaric acid, the capital is caused the acidolysis main reaction and is had an accident in the premix process, for preventing that accident from taking place, need in complex acid and premix process, cool off sulfuric acid and slip, and to control mixture strength and time, premixing intensity and time is insufficient often to influence premixing effect, thereby influences the acidolysis rate of follow-up acidolysis process; 3) the higher premix slip inconvenience pump delivery of acid concentration, in case generation excessive agitation, cause the acidolysis main reaction, so the premix groove must be arranged on the position that is higher than the acidolysis pot, be convenient to the premix slip is directly put into the acidolysis pot, yet the investment of premix groove of pulp being imported the higher position is big, energy consumption is high.
Summary of the invention
The present invention is intended to overcome the shortcoming of above-mentioned background technology, and improving one's methods of a kind of sulfuric acid process titanium ore acidolysis is provided, and improves to return and uses the spent acid usage quantity, saves cost, simplifies technology, and avoids accident, handled easily.
For realizing purpose of the present invention, the applicant has proposed a kind of operating process of new sulfuric acid process titanium ore acidolysis here: at first that the rare spent acid of the by product in the sulfate process titanium dioxide production is dense through tentatively carrying, after the removal of impurities, without complex acid operation directly and breeze carry out premix, then, pre-mixed slurry is dropped into the acidolysis pot, add the vitriol oil, utilize the spent acid in the vitriol oil and the slurry to mix the heat of dilution initiation main reaction that the back produces, and stipulated the concentration range of spent acid and concentrated acid, to guarantee after the vitriol oil adds, total acid content and sulfuric acid initial concentration can satisfy the processing requirement of acidolysis reaction in the acidolysis pot, can produce enough heats of dilution again simultaneously and cause the acidolysis main reaction.Said process has saved complex acid and process for cooling link, replaces the adding dilution water to cause the acidolysis main reaction with adding the vitriol oil.
Improving one's methods of sulfuric acid process titanium ore acidolysis of the present invention may further comprise the steps:
A. at first, with rare acid-spending strength raising of sulfate process titanium dioxide by-product,, remove impurity so that utilize the raising of sulfuric acid concentration;
B. the spent acid after, the removal of impurities dense through tentatively carrying that steps A is obtained quantitatively drops into the premix trough rim and stirs the limit and add titanium ore, until this batch ore deposit is added, continues to stir and makes the abundant mixing of slip;
C. then, the pre-mixed slip that step B obtains is put into the acidolysis pot, add the vitriol oil while stirring, utilize the spent acid in the vitriol oil and the slurry to mix the heat of dilution initiation acidolysis main reaction that produces;
D. carry out follow-up slaking, leaching, restoring operation according to a conventional method.
Wherein rare spent acid that uses derives from one of sulfate process titanium dioxide production and washes operation in the steps A, through concentration operation or add the vitriol oil and carry and concentration being improved after dense, preferably brings up to 48%-65%.The solid impurity of separating out in can be with steps A before entering step B is removed with solid separation methods such as press filtrations.
Among the step B and the concentration of the employed acid of titanium ore premix be lower than the acidolysis reaction initial sulfuric acid concentration, described acid be dense by rare spent acid of sulfate process titanium dioxide by-product is carried, obtain after removing miscellaneous operation.In step C, add the vitriol oil to cause acidolysis reaction, the concentration of the described vitriol oil is higher than the initial sulfuric acid concentration of acidolysis reaction, and vitriol oil add-on should make total acid content and acid concentration in the acidolysis pot satisfy the requirement of acidolysis process.
The spent acid amount G that drops among step B and the step C
1With vitriol oil amount G
2Be than f, acidolysis reaction initial sulfuric acid concentration C with the best sour ore deposit of acidolysis reaction
3, always throw ore deposit amount G and acid-spending strength C
1With vitriol oil concentration C
2Calculate to obtain as known conditions, wherein sour ore deposit ratio, initial sulfuric acid concentration, always to throw the ore deposit amount definite according to the titanium ore characteristic by the technologist, and calculation formula is:
C
1*G
1+C
2*G
2＝G*f ①；
(G
1+G
2)C
3＝G*f ②。
Wherein, causing main reaction employed in step C is the vitriol oil, can be without the prediluted vitriol oil, even can directly use oleum, and vitriolic concentration is 92%-98.5%.
The sour ore deposit here is meant the mass ratio in sulfuric acid (with 100% densitometer) and ore deposit than f, and sour ore deposit is generally 1.5-1.6 than f, acidolysis reaction initial acid concentrations C
3Generally be controlled at 82%-90%, concrete numerical value depends primarily on the quality and the reactive behavior in ore deposit.
The process procedures such as having saved complex acid and cooling of improving one's methods of sulfuric acid process titanium ore acidolysis of the present invention, reduced energy consumption, simplified technology, owing in the premix groove of step B, used rare spent acid and titanium ore premix, avoided sour dense, the too high safety problem that causes of acid temperature, made stirrings, do time in advance, the control of intensity becomes unusual simple light, no longer needs cooling step, just can realize premix safely, improve premixing effect, thereby improve the acidolysis rate of follow-up acidolysis process.And under the not high situation of acid concentration, the transportation of premix slip becomes simply, safety, has reduced energy consumption.
Description of drawings
Fig. 1 is the process flow sheet of sulfuric acid process titanium ore acidolysis of the present invention;
Label declaration in the accompanying drawing:
Wherein 1 is cooling crystallizer, and 2 is pressure filter, and 3 is dense spent acid groove, and 4 is the premix groove, and 5 are the acidolysis pot.
Embodiment
Now the processing method of sulfuric acid process titanium ore acidolysis of the present invention is described in detail in conjunction with Fig. 1.But the restriction that protection scope of the present invention is not described by following specific embodiment.
With concentration 25% rare spent acid of sulfate process titanium dioxide by-product and concentration the vitriol oil greater than the acid concentration that is mixed, the sulfuric acid of concentration 93%-98% for example, join in the cooling crystallizer 1 and be mixed, the concentration that is mixed remains on 48-65%, with water coolant with sour temperature control below 55 ℃, send into pressure filter 2 with the acid that pump will be mixed, flow into dense spent acid groove 3 after removing impurity, then need not above-mentioned steps with the concentrating waste acid that additive method concentrates, removal of impurities obtains, directly put into dense spent acid groove 3, only require that its concentration and temperature are controlled between the 48-65% too with below 55 ℃.Spent acid is put into the premix groove 4 from dense spent acid groove 3, started agitator, in premix groove 4, add perovskite powder then and mix; Mixed slurry is driven in the acidolysis pot 5, and in the acidolysis pot, adds vitriol oil initiation main reaction.
Embodiment 1
1) vitriol oil of rare spent acid of 24.6% concentration of sulfate process titanium dioxide by-product and 98% ratio in 1:0.707 is added in the cooling crystallizer 1, mixing back concentration is 55%, the acid that mixes fully is cooled to 53 ℃, in crystallizer 1, continue slaking 2 hours, separate out impurity, then, after with pressure filter 2 solid impurity being removed, the clear liquid dense spent acid groove 3 of packing into.
2) sour ore deposit ratio and the acidolysis reaction initial concentration of determining by the characteristic of used ilmenite concentrate is respectively 1.55 and 84%, and calculating the spent acid dosage is 18 tons.Therefore, 18 tons of dense spent acid are put into premix groove 4 from dense spent acid groove 3, start premix groove agitator, add 30 tons of 47% good ilmenite concentrates of mill, mixed 10 minutes.
3) with pump the slurry that mixes is squeezed in the acidolysis pot 5, the acidolysis the bottom of a pan feeds pressurized air and stirs, and according to calculation result, 37.3 tons of the vitriol oils of adding 98% cause main reaction.
4) after main reaction finishes, stop to stir, slaking 2 hours adds 72 tons in leaching water at twice, leaches 4 hours, stirs with pressurized air during leaching.
5) add 110 kilograms of iron powders, carry out restoring operation, behind the adding iron powder, stirred 1 hour with pressurized air, then, blowing is to subsequent processing.
Embodiment 2
1) will put into dense spent acid groove 3 through titanium dioxide waste acid by sulfuric acid process concentrated, removal of impurities, its concentration is 62%, and temperature is 55 ℃.
2) sour ore deposit ratio and the acidolysis reaction initial concentration of determining by the characteristic of used ilmenite concentrate is respectively 1.57 and 86%, and calculating the spent acid dosage is 18.3 tons.Therefore, 18.3 tons dense spent acid are put into premix groove 4 from dense spent acid groove 3, start premix groove agitator, add 30 tons of 46.5% good ilmenite concentrates of mill, mix after 10 minutes.
3) with pump the slurry that mixes is squeezed into from premix groove 4 in the acidolysis pot 5, the acidolysis the bottom of a pan feeds pressurized air and stirs, and by calculation result, adds 36.5 ton 98% the vitriol oil, causes main reaction.
4) after main reaction finishes, stop to stir, slaking 2 hours adds 72 tons in leaching water at twice, leaches 4.5 hours, stirs with pressurized air during leaching.
5) add 110 kilograms of iron powders, carry out restoring operation, behind the adding iron powder, stirred 1 hour with pressurized air, then, blowing is to subsequent processing.
Adopt method of the present invention, by carrying dense to useless diluted acid earlier, concentration is controlled at greater than 48%, after being separated out, most impurity crystallization removes, concentration is controlled at below 65%, the premix slip that can guarantee to make with this acid can produce enough heats of dilution and cause main reaction, simultaneously after adding the vitriol oil, at this below concentration, in the time of guaranteeing that spent acid and breeze carry out premix, the acidolysis main reaction can not take place even temperature reaches 70 ℃, obviously reduced accident risk yet, and can suitably increase premixing intensity and time, improve premixing effect, add sour dense better below 65%, thereby improved acidolysis rate the breeze effect of impregnation may.
Because the premix slip that obtains according to the inventive method is difficult for the acidolysis main reaction takes place, and also provides convenience for the storage and the conveying of premix slip.For example, the premix groove can be arranged on ground, breeze is directly put into premix groove and spent acid premix from feed bin, with pump slip is sent into the acidolysis pot then, so just replaced prior art that the premix groove is arranged on the elevated way, will not use machinery or gas delivery in elevated premix groove by breeze, it is simple and energy-conservation relatively that course of conveying becomes.Cause acidolysis reaction with concentrated acid and not only saved foregoing complex acid operation,, the present invention do not cause water because utilizing water to do acidolysis yet, so strengthened the usage quantity of spent acid, with embodiments of the invention 2 is example, guaranteeing identical acidolysis reaction acid ore deposit ratio, acidolysis reaction initial concentration and acidolysis are thrown under the amount situation of ore deposit, to add about 2.5 tons of water with common method and do acidolysis initiation water, after guaranteeing to add initiation water, reach 86% acidolysis reaction initial concentration, complex acid concentration must guarantee to reach 90.0%, then corresponding spent acid utilization is kept to 11.6 from 18.3, return with spent acid and drop to 15% with 24% of sour total amount from accounting for acidolysis, if keep the ratio that spent acid uses, the concentration that then needs will return with acid brings up to 72%, causes energy consumption to increase.
Claims (7)
1. the method for a sulfuric acid process titanium ore acidolysis said method comprising the steps of:
A. at first, rare acid-spending strength is improved,, remove impurity so that utilize the raising of sulfuric acid concentration;
B. the rare spent acid after, the removal of impurities dense through tentatively carrying that steps A is obtained quantitatively drops into the premix trough rim and stirs the limit and add titanium ore, until this batch ore deposit is added, continues to stir and makes the abundant mixing of slip;
C. then, the pre-mixed slip that step B obtains is put into the acidolysis pot, adding while stirring need not the prediluted vitriol oil, utilizes the spent acid in the vitriol oil and the slurry to mix the heat of dilution initiation acidolysis main reaction that produces;
D. carry out follow-up slaking, leaching, restoring operation.
2. the method for sulfuric acid process titanium ore acidolysis according to claim 1 is characterized in that among the step B and the concentration of the employed acid of titanium ore premix is lower than acidolysis reaction initial sulfuric acid concentration C
3, described acid be dense by rare spent acid of sulfate process titanium dioxide by-product is carried, obtain after removing miscellaneous operation.
3, the method for sulfuric acid process titanium ore acidolysis according to claim 1 is characterized in that among the step C causing the concentration C of the vitriol oil of acidolysis reaction
2The initial sulfuric acid concentration C that should be higher than acidolysis reaction
3
4. the method for sulfuric acid process titanium ore acidolysis according to claim 3, what it is characterized in that step C initiation main reaction use is the vitriol oil or oleum, the concentration C of the vitriol oil
2Be 92%-98.5%.
5. the method for sulfuric acid process titanium ore acidolysis according to claim 1 is characterized in that in steps A, and the concentration of described rare spent acid through carrying after dense is 48-65%.
6, the method for sulfuric acid process titanium ore acidolysis according to claim 1 is characterized in that the spent acid amount G that drops among step B and the step C
1With vitriol oil amount G
2, pass through the best sour ore deposit of acidolysis reaction than f, acidolysis reaction initial sulfuric acid concentration C according to following formula
3, always throw ore deposit amount G and acid-spending strength C
1With vitriol oil concentration C
2Calculate:
C
1*G
1+C
2*G
2＝G*f ①；
(G
1+G
2)C
3＝G*f ②。
7, according to the method for claim 2 or 3 described sulfuric acid process titanium ore acidolysis, its feature exists, acidolysis reaction initial sulfuric acid concentration C
3Generally be controlled at 82%-90%.
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| CN102050487A (en) * | 2010-12-31 | 2011-05-11 | 攀钢集团重庆钛业有限公司 | Acidolysis method in titanium dioxide production technology adopting sulfuric acid process |
| CN102830200A (en) * | 2012-08-21 | 2012-12-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for detecting titanium-containing mineral acidolysis rate |
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| CN103723765A (en) * | 2014-01-20 | 2014-04-16 | 韶关学院 | Method for preparing titanium dioxide through sulfuric acid method |
| CN103910381A (en) * | 2014-04-21 | 2014-07-09 | 济南裕兴化工有限责任公司 | Titanium dioxide solution production method capable of reducing acid consumption |
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| CN1376635A (en) * | 2002-05-09 | 2002-10-30 | 四川龙蟒集团有限责任公司 | Process for preparing phosphoric acid from waste sulfuric acid as by-product of titanium oxide powder by wet method |
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| CN113443649B (en) * | 2021-07-13 | 2022-11-29 | 攀钢集团研究院有限公司 | Intermittent acidolysis method of titanium slag |
| CN114084903A (en) * | 2021-12-20 | 2022-02-25 | 攀钢集团重庆钛业有限公司 | Continuous acidolysis method for titanium concentrate |
| CN115536061A (en) * | 2022-11-04 | 2022-12-30 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate from low-grade titanium ore |
| CN115536061B (en) * | 2022-11-04 | 2024-01-26 | 攀枝花东方钛业有限公司 | Method for preparing titanyl sulfate from low-grade titanium ore |
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| CN101514031B (en) | 2012-09-19 |
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