CN103011272A - Method for concentrating and purifying titanium dioxide waste acid by using complex acid - Google Patents
Method for concentrating and purifying titanium dioxide waste acid by using complex acid Download PDFInfo
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- CN103011272A CN103011272A CN2012105404017A CN201210540401A CN103011272A CN 103011272 A CN103011272 A CN 103011272A CN 2012105404017 A CN2012105404017 A CN 2012105404017A CN 201210540401 A CN201210540401 A CN 201210540401A CN 103011272 A CN103011272 A CN 103011272A
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Abstract
The invention discloses a method for concentrating and purifying titanium dioxide waste acid by using complex acid. The method comprises the following specific steps of: titanium recovery: primarily concentrating waste acid produced in a titanium dioxide production process by using waste heat of calcining tail gas of a ring kiln to achieve the mass concentration being 25-32%, and then recovering titanium; acid mixing: uniformly mixing the waste acid subjected to titanium recovery and concentrated sulfuric acid in an acid mixing tank according to a mass proportion of (1.2-4):1 to obtain mixed acid; and crystallization: carrying out gradient cooling, crystallizing, curing and filtering on the mixed acid gradually in the acid mixing tank, and when the temperature of the mixed acid is reduced to 60-65 DEG C, pumping the mixed acid into a filter press for solid-liquid separation to obtain concentrated sulfuric acid and ferrous dregs. The method disclosed by the invention has the advantage of changing the traditional method for concentrating the titanium dioxide waste acid by depending on natural gas, steam, fire coal hot gas and other heat sources, is free from consuming a large amount of energy sources and capable of reducing the cost in waste acid concentration, and is high in recovery rate of the waste acid.
Description
Technical field
The present invention relates to a kind of concentration technique of spent acid, be specifically related to a kind of method of utilizing complex acid thickening-purification technology titanium pigment waste acid.
Background technology
The titanium dioxide formal name used at school is titanium dioxide, belongs to inert pigment, is considered to the in the world best a kind of white pigment of performance, is widely used in making the industries such as coating, synthon, senior white paint, white rubber, printing, metallurgy.
Titanium White Production By Sulfuric Acid Process technique, main raw material are titanium ore and sulfuric acid, have the advantages such as production cost is low, technology maturation, are a kind of methods that generally adopts in the existing titanium white production mode.But utilize the every production of sulfuric acid process 1t titanium dioxide, need to consume the above sulfuric acid of 4t, produce simultaneously 4.5 ~ 6t left and right sides wt (H
2SO
4) 20% ~ 25% spent acid, H in the spent acid
2SO
4Content also contains the FeSO of 8-16% generally at 20-25%
4, 1-3% MgSO
4, 0.8-3% Al
2(SO
4)
3, 0.1-1% MnSO
4, 0.8-1.5% TiOSO
4, 0.3-1.0% H
2TiO
3, various places are increasingly strict to environmental requirement in recent years, and some factory is owing to spent acid solution good being forced to stop production never.Therefore, for a large amount of spent acid, forbid direct discharging, add the shortage of resource, at present large multiple enterprises begins to recycle this part spent acid, and recovery and treatment method mainly contains neutralisation, method of enrichment.
Neutralisation is to carry out neutralization reaction with Wingdale, lime or carbide slag etc. with spent acid, produces gypsum that can be used as material of construction etc.The cost that neutralization method need to consume the recycling spent acid such as a large amount of lime, carbide slag is high, is about 1200 yuan/tons, and general enterprises is difficult to bear, and neutralization reaction can produce a large amount of wastes.
Method of enrichment is that spent acid is concentrated, and improves the concentration of spent acid, reaches the standard that can recycle.Comparing neutralisation does not need to consume a large amount of lime, carbide slag etc., does not need to discharge a large amount of wastes yet.But at present the concentration technique majority of spent acid is to utilize the direct method of enrichment of a kind of thermal source, and thermal source comprises Sweet natural gas, steam or coal-fired hot gas etc., concentrated for high temperature, highly corrosive acid, and, energy consumption high to equipment requirements and process cost are also high.The patent No. is the Chinese invention patent of CN200510019017.2, the industrial method that waste acid concentration is recycled in a kind of titanium white production is disclosed, adopt the spent acid flue gas to concentrate and concentrated two steps of spent acid steam, flue gas and steam coordinated operation, overcome existing waste acid concentration recovery method steam consumption quantity large, power consumption is high, and working cost is high; Thickening efficiency is low; Many and the complex structure of operational outfit; The deficiencies such as technological design complexity.But this patent is in whole concentration process, and the gas phase temperature of spent acid all is controlled at more than 80 ℃, and liquidus temperature adopts the high energy consumption pattern also more than 70 ℃, utilizes thermal source that spent acid is concentrated, and needs to consume a large amount of energy and comes again reclaim(ed) sulfuric acid of concentrating waste acid.
And in sulfuric acid method titanium pigment is produced, realize that metatitanic acid desulfurization and conversion need high-temperature calcination, and the equipment of calcining is rotary kiln, the tail temperature of calcining rotary kiln generally is by alkali lye spray-absorption SO at 300 ℃ ~ 450 ℃
2After the environmental protection treatment, directly be discharged into atmosphere, this part heat is that the waste heat of rotary kiln calcining tail gas is not utilized effectively.
In sum, how to reduce the waste acid concentration cost, utilizing less energy-consumption, cheaply mode effective recycling spent acid is the difficult problem that enterprise faces, and is that the industry wishes to solve unsolved technical barrier always.
Summary of the invention
The object of the invention is to overcome the defective that exists in the prior art, design a kind of calcining using waste heat from tail gas in the titanium white production and method of complex acid thickening-purification technology titanium pigment waste acid utilized, the method concentrating waste acid does not need to consume a large amount of energy, and production cost is low, and the rate of recovery of spent acid is high.
For achieving the above object, technical scheme of the present invention is a kind of method of utilizing complex acid thickening-purification technology titanium pigment waste acid of design, and concrete steps are as follows:
A, recovery titanium: with the spent acid that produces in the production process of titanium pigment, utilize the waste heat of rotary kiln calcining tail gas, be 25% ~ 32% with the preliminary concentrate of spent acid to mass concentration, then reclaim the titanium operation, namely utilize the sedimentation principle, settlement separate Waste Sulfuric Acid and the titanium that goes out to contain ferrous sulfate of Sean, titanium returns the titanium dioxide washing room, and salt processing calcining and aftertreatment obtained titanium dioxide after rinsing was clean; Waste Sulfuric Acid enters next step complex acid.
B, complex acid: spent acid and the vitriol oil that will reclaim behind the titanium in the nitration mixture groove according to the quality proportioning are: 1.2 ~ 4:1, mix, and obtain nitration mixture;
C, crystallization: in the nitration mixture groove, nitration mixture is progressively carried out gradient cooling, crystallization, slaking;
D, filtration: be down to 60 ~ 65 ℃ when the nitration mixture temperature, nitration mixture is squeezed into pressure filter, carry out solid-liquid separation, obtain concentrated vitriol and ferrous slag.
The ratio that spent acid mixes with the vitriol oil depends on concentration requirement and impurity-eliminating effect that complex acid is concentrated.According to Fig. 1, the solubility curve figure of ferrous sulfate in sulfuric acid will remove the ferrous impurity in the spent acid as far as possible, and sulfuric acid concentration should be controlled at more than 45%, but nitration mixture concentration is too high, and viscosity is large, is unfavorable for solid-liquid separation.Therefore, the quality proportion optimization of this technique nitration mixture is 1.2 ~ 4:1, has not only guaranteed impurity-eliminating effect but also be conducive to solid-liquid separation.
As preferably: among the described step B, the massfraction of sulfuric acid is more than 93% in the vitriol oil, and the concentration of the control vitriol oil mainly is the dosage of the control vitriol oil, guarantees that concentration behind the nitration mixture is more than 45%.
The amplitude of gradient cooling described in the step C is 2 ~ 10 ℃/h, the time 7 ~ 12h of described slaking.Because ferrous sulfate forms at the process experience crystal seed of crystallization, the crystal growth process, temperature and time is very important to the growth of crystal, the applicant finds by great many of experiments, when the cooling gradient at 2 ~ 10 ℃/h, during the time 7 ~ 12h of slaking, the crystallization effect of ferrous sulfate is better, crystal grain reaches more than 50 microns, because ferrous sulfate crystal grain is larger, to be convenient to filter, sulfuric acid content is lower in the ferrous sulfate.
Temperature when filtering among the described step D is controlled at 55 ~ 70 ℃.Effect by considering filtration and the withstand temp of canvas press cloth obtain filtration temperature.
Advantage of the present invention and beneficial effect are:
1, the present invention has changed the method for the concentrated titanium pigment waste acid of the thermals source such as traditional dependence Sweet natural gas, steam, coal-fired hot gas, utilize rotary kiln calcining using waste heat from tail gas during preliminary concentrate spent acid, spent acid spray and 300 ℃ ~ 450 ℃ calcining tail gas are carried out counterflow heat exchange, thereby transpiring moisture, concentrating waste acid, then carry out metatitanic acid by flocculating settling and reclaim, can reduce titanium content in the spent acid, can improve the yield of titanium dioxide simultaneously.Behind the preliminary concentrate spent acid, the heat that utilizes spent acid to mix with the vitriol oil heats further concentrate spent acid, reaches same concentrating and impurity removing effect.Can greatly reduce by 650 ~ 700 yuan/t of waste acid concentration cost, and less investment, concrete technical indicator sees Table 1.
Table 1 waste acid concentration to 55% technico-economical comparison (ton 100% H
2SO
4Meter)
2, the nitration mixture of the present invention after to complex acid carries out gradient cooling, slaking, improves ferrous crystallization effect, and the ferrous sulfate crystal grain that the concentrated slaking of complex acid obtains is larger.Because crystal grain is larger, filtering rate is fast, and sulfuric acid content is low in the ferrous sulfate, thereby improves strainability, improves the rate of recovery of spent acid.Table 2 and table 3 contrast, can find out, ferrous sulfate content is than the obvious reduction of spray concentration in the nitration mixture that the complex acid method is filtered, improved sour quality, the ferrous slag quality that filtration obtains also improves greatly, reduced sulfuric acid content in the ferrous slag, improved iron level, the later stage ferrous iron has been mixed to burn to recycle reduce the sulphur loss.
Table 2 spray concentration test spent acid analytical results
As seen from Table 2, the spray concentration method is because of the difference of ultimate density, and the press cake that obtains and concentrated vitriol be difference to some extent, filter cake Free Acid content improves and reduces along with concentrated concentration, iron level improves with the raising of acid concentration, and on the contrary, iron reduces with the concentration raising in the concentrated vitriol that obtains.
Table 3 single groove complex acid operation scheme and spent acid analytical results
As seen from Table 3, in the complex acid method, different cooling methods and rate of temperature fall also have no impact to press cake and the concentrated vitriol that obtains, and rate of temperature fall is slower, and the free acid content in the filter cake is lower, and the time is shorter, and filter cake Free Acid content is higher.With respect to the result of spray concentration in the table 2 as seen, iron level is lower in the concentrated concentrated vitriol that obtains of complex acid, and filter cake Free Acid content is lower, illustrates that the quality of concentrated vitriol and yield are improved.
Description of drawings
Fig. 1 is the solubility curve figure of ferrous sulfate in sulfuric acid.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only are used for technical scheme of the present invention more clearly is described, and can not limit protection scope of the present invention with this.
With the spent acid in the production process of titanium pigment, its main component is counted: H in mass ratio
2SO
421%, FeSO
48.5%, MgSO
42%, metatitanic acid 0.5%, process countercurrent spray rotary kiln calcining tail gas utilizes the waste heat concentrate to 25% of calcining tail gas, by behind the spent acid flocculating settling recovery metatitanic acid, obtains limpid spent acid again; Spent acid is joined in the spent acid configured slot, add the sulfuric acid massfraction again and be 98% the vitriol oil, the spent acid of every 3.5t adds the 1t vitriol oil, and the two mixes, and obtains nitration mixture.Then carry out gradient cooling, slaking, the amplitude of gradient cooling is 8 ℃/h, and the time of slaking is 10h; After temperature was down to below 60 ℃, whole nitration mixture were squeezed into pressure filter and are carried out solid-liquid separation, separated obtaining liquid phase thing sulfuric acid.Massfraction is 43.9%, iron level 0.68% in the sulfuric acid, the ferrous sulfate particle crystal grain that separates is 75 microns, ferrous Free Sulfuric Acid content is 16.5%, the rate of recovery of spent acid reaches 87%, rolling over the cost recovery of (100%) per ton spent acid is 125 yuan, and sulfuric acid is for titanium dioxide acidolysis or phosphorous chemical industry extraction and sulfonic acid absorption etc.Solid formation is ferrous sulfate monohydrate, and wherein TFe approximately 18.5%, is used for sand acid and mixes burning and prepare sulfuric acid again.
Embodiment 2
With the spent acid in the production process of titanium pigment, its mass ratio is: H
2SO
421%, FeSO
48.5%, MgSO
42%, metatitanic acid 0.5%, process countercurrent spray rotary kiln calcining tail gas utilizes the waste heat concentrate to 28% of calcining tail gas, by behind the spent acid flocculating settling recovery metatitanic acid, obtains limpid spent acid again.Spent acid is joined in the spent acid configured slot, add the sulfuric acid massfraction again and be 96% the vitriol oil, every 2.3t spent acid adds the 1t vitriol oil, and the two mixes, and obtains nitration mixture.Then carry out gradient cooling, slaking, the amplitude of gradient cooling is 5 ℃/h, and the time of slaking is 8h.After temperature was down to below 62 ℃, whole nitration mixture were squeezed into pressure filter and are carried out solid-liquid separation, separated obtaining liquid phase thing sulfuric acid.Massfraction is 50.3%, iron level 0.59% in the sulfuric acid, the ferrous sulfate particle crystal grain that separates is 94 microns, ferrous Free Sulfuric Acid content is 13.8%, the rate of recovery of spent acid reaches 91%, rolling over the cost recovery of (100%) per ton spent acid is 110 yuan, and sulfuric acid is for titanium dioxide acidolysis or phosphorous chemical industry extraction and sulfonic acid absorption etc.Solid formation is ferrous sulfate monohydrate, and wherein TFe approximately 20.1%, is used for sand acid and mixes burning and prepare sulfuric acid again.
Embodiment 3
With the spent acid in the production process of titanium pigment, its mass ratio is: H
2SO
421%, FeSO
48.5%, MgSO
42%, metatitanic acid TiO
20.5%, process countercurrent spray rotary kiln calcining tail gas utilizes the waste heat concentrate to 32% of calcining tail gas, by behind the spent acid flocculating settling recovery metatitanic acid, obtains limpid spent acid again.Spent acid is joined in the spent acid configured slot, add the sulfuric acid massfraction again and be 93% the vitriol oil, every 1.5t spent acid adds the 1t vitriol oil, and the two mixes, and obtains nitration mixture.Then carry out gradient cooling, slaking, the amplitude of gradient cooling is 2 ℃/h, and the time of slaking is 7h.After temperature was down to below 65 ℃, whole nitration mixture were squeezed into pressure filter and are carried out solid-liquid separation, separated obtaining liquid phase thing sulfuric acid.Massfraction is 58.2%, iron level 0.38% in the sulfuric acid, the ferrous sulfate particle crystal grain that separates is 100 microns, ferrous Free Sulfuric Acid content is 10.7%, the rate of recovery of spent acid reaches 92%, rolling over the cost recovery of (100%) per ton spent acid is 100 yuan, and sulfuric acid is for titanium dioxide acidolysis or phosphorous chemical industry extraction and sulfonic acid absorption etc.Solid formation is ferrous sulfate monohydrate, and wherein TFe approximately 20.8%, is used for sand acid and mixes burning and prepare sulfuric acid again.
The comparative example 1
With the spent acid that produces in the production process of titanium pigment, from dry upgrading tower jacking row atomisation, the thermal evaporation concentration process is finished in the heating of the warm air of coming at the bottom of Ta Nei and tower (combustion of natural gas) adverse current multiple-contact, the steam of concentration and evaporation is got rid of from cat head, through entering exhaust fan after the mist eliminator demist, get rid of into atmosphere from chimney.The sulfuric acid liquid that contains the precipitated impurities of separating out after concentrated is got rid of at the bottom of tower, and through supercooler heat exchange cooling, the entrance pressure filter carries out solid-liquid separation again, and filtrate is the vitriol oil.Its massfraction is 55.0%, iron level 0.45% in the sulfuric acid, the ferrous sulfate particle crystal grain that separates is 20 microns, ferrous Free Sulfuric Acid content is 16.8%, the rate of recovery of spent acid reaches 82%, rolling over the cost recovery of (100%) per ton spent acid is 825 yuan, and sulfuric acid is for titanium dioxide acidolysis or phosphorous chemical industry extraction and sulfonic acid absorption etc.Solid formation is ferrous sulfate monohydrate, and wherein TFe approximately 18.3%, is used for sand acid and mixes burning and prepare sulfuric acid again.
Claims (4)
1. a method of utilizing complex acid thickening-purification technology titanium pigment waste acid is characterized in that, concrete steps are as follows:
A, recovery titanium: with the spent acid that produces in the production process of titanium pigment, utilizing the waste heat of rotary kiln calcining tail gas, is 25%-32% with the preliminary concentrate of spent acid to mass concentration, then reclaims the titanium operation;
B, complex acid: spent acid and the vitriol oil that will reclaim behind the titanium in the nitration mixture groove according to the quality proportioning are: 1.2-4:1, mix, and obtain nitration mixture;
C, crystallization: in the nitration mixture groove, nitration mixture is progressively carried out gradient cooling, crystallization, slaking;
D, filtration: be down to 60-65 ℃ when the nitration mixture temperature, nitration mixture is squeezed into pressure filter, carry out solid-liquid separation, obtain concentrated vitriol and ferrous slag.
2. the method for thickening-purification technology titanium pigment waste acid as claimed in claim 1 is characterized in that, the massfraction of the sulfuric acid of the vitriol oil is more than 93% among the described step B.
3. the method for thickening-purification technology titanium pigment waste acid as claimed in claim 1 is characterized in that, the amplitude of gradient cooling described in the step C is 2-10 ℃/h, the time 7-12h of described slaking.
4. the method for thickening-purification technology titanium pigment waste acid as claimed in claim 1 is characterized in that, the temperature when filtering among the described step D is controlled at 55-70 ℃.
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| CN104118893A (en) * | 2014-07-31 | 2014-10-29 | 四川龙蟒钛业股份有限公司 | Method for producing industrial-grade magnesium sulfate by using titanium white waste acid |
| CN104129816A (en) * | 2014-07-31 | 2014-11-05 | 四川龙蟒钛业股份有限公司 | Method for removing iron from titanium dioxide concentrated acid solution |
| CN104140082A (en) * | 2014-07-31 | 2014-11-12 | 四川龙蟒钛业股份有限公司 | Method for recycling titanium dioxide waste acid |
| CN104555949A (en) * | 2014-12-28 | 2015-04-29 | 贵州兰鑫石墨机电设备制造有限公司 | Titanium white waste acid concentration process |
| CN106564863A (en) * | 2016-11-15 | 2017-04-19 | 四川龙蟒钛业股份有限公司 | Hydrogen peroxide addition level control equipment for concentrated waste acid iron removal process |
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| CN110776004A (en) * | 2019-12-04 | 2020-02-11 | 龙佰四川钛业有限公司 | Method for recovering soluble titanium dioxide in titanium dioxide waste acid |
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| CN104118893A (en) * | 2014-07-31 | 2014-10-29 | 四川龙蟒钛业股份有限公司 | Method for producing industrial-grade magnesium sulfate by using titanium white waste acid |
| CN104129816A (en) * | 2014-07-31 | 2014-11-05 | 四川龙蟒钛业股份有限公司 | Method for removing iron from titanium dioxide concentrated acid solution |
| CN104140082A (en) * | 2014-07-31 | 2014-11-12 | 四川龙蟒钛业股份有限公司 | Method for recycling titanium dioxide waste acid |
| CN104118893B (en) * | 2014-07-31 | 2015-11-18 | 四川龙蟒钛业股份有限公司 | One utilizes titanium white waste acid manufacture level magnesium sulfate method |
| CN104129816B (en) * | 2014-07-31 | 2016-03-30 | 襄阳龙蟒钛业有限公司 | The method of a kind of titanium white gelled acid deironing |
| CN104140082B (en) * | 2014-07-31 | 2016-08-24 | 四川龙蟒钛业股份有限公司 | A kind of recoverying and utilizing method of titanium white waste acid |
| CN104555949A (en) * | 2014-12-28 | 2015-04-29 | 贵州兰鑫石墨机电设备制造有限公司 | Titanium white waste acid concentration process |
| CN106564863A (en) * | 2016-11-15 | 2017-04-19 | 四川龙蟒钛业股份有限公司 | Hydrogen peroxide addition level control equipment for concentrated waste acid iron removal process |
| CN109941968A (en) * | 2019-04-24 | 2019-06-28 | 成都先进金属材料产业技术研究院有限公司 | Utilize the method for sodium dihydrogen phosphate processing waste sulfuric acid solution |
| CN109987591A (en) * | 2019-04-29 | 2019-07-09 | 成都先进金属材料产业技术研究院有限公司 | Utilize the method for chlorination Copper treatment titanium dioxide waste acid by sulfuric acid process |
| CN110697792A (en) * | 2019-10-31 | 2020-01-17 | 襄阳龙蟒钛业有限公司 | Method for preparing yellow ferrous iron with controllable particle size by using waste acid from titanium dioxide production |
| CN110776004A (en) * | 2019-12-04 | 2020-02-11 | 龙佰四川钛业有限公司 | Method for recovering soluble titanium dioxide in titanium dioxide waste acid |
| CN110776004B (en) * | 2019-12-04 | 2022-02-01 | 龙佰四川钛业有限公司 | Method for recovering soluble titanium dioxide in titanium dioxide waste acid |
| CN111924808A (en) * | 2020-09-09 | 2020-11-13 | 胡光雄 | Equipment for concentrating high-temperature flue gas waste acid in titanium dioxide production by sulfuric acid method and use method |
| CN111924808B (en) * | 2020-09-09 | 2023-05-02 | 胡光雄 | Equipment for concentrating high-temperature flue gas waste acid in sulfuric acid process titanium dioxide production and application method |
| CN113772633A (en) * | 2021-09-09 | 2021-12-10 | 东华工程科技股份有限公司 | Mixed acid system and method for removing ferrous sulfate in titanium white waste acid |
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Application publication date: 20130403 |