CN105271157A - Method for comprehensively treating titanium white waste acid and phosphate floatation tailings - Google Patents
Method for comprehensively treating titanium white waste acid and phosphate floatation tailings Download PDFInfo
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- CN105271157A CN105271157A CN201510705393.0A CN201510705393A CN105271157A CN 105271157 A CN105271157 A CN 105271157A CN 201510705393 A CN201510705393 A CN 201510705393A CN 105271157 A CN105271157 A CN 105271157A
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- titanium white
- waste acid
- white waste
- flotation tailings
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Abstract
The invention discloses a method for comprehensively treating titanium white waste acid and phosphate floatation tailings. The method comprises the following steps: (1) mashing the floatation tailings by adopting mother liquor, then adding the titanium white waste acid, controlling the reaction temperature, time and pH value, and then separating solid and liquid; (2) concentrating clear liquid after the solid-liquid separation until the specific weight is 1.40 to 1.5 g/ml, adding a flocculating agent to carrying out the sedimentation, and carrying out the liquid-solid separation for thick slurry; (3) cooling the clear liquid after the solid-liquid separation and crystallizing, and separating to obtain a ferrous magnesium sulfate product, and returning the mother liquor to the step (1). According to the method, not only can elements such as iron, magnesium, sulfur, phosphorus, titanium and the like of the titanium white waste acid and the phosphate floatation tailings be effectively utilized, but also the influence on the peripheral environment and land resource can be alleviated, the treatment cost of the tailings and titanium white waste acid is greatly reduced, a purpose of treating the waste by waste is achieved, and the economic benefit is remarkable; the precipitated solid waste can be used for producing cement retarder and high-quality flame retardant titanium phosphate, no waste and byproduct are discharged during the entire process, the production cost is extremely low, the operation is simple, and an important significance for recycling the resource and realizing the environment-friendly production can be realized.
Description
Technical field
The present invention relates to a kind of titanium white waste acid field of comprehensive utilization, specifically relate to the treatment process of a kind of titanium white waste acid and phosphate ore flotation tailings.
Background technology
Titanium White Production By Sulfuric Acid Process has the advantages such as production cost is low, technology maturation, is a kind of method generally adopted in existing titanium white production mode.Production By Sulfuric Acid Process technique often produces 1t titanium dioxide, need the sulfuric acid consuming more than 4t, produce the spent acid that 6 ~ 8t sulfuric acid concentration is 20 ~ 25% simultaneously, so many spent acid, spent acid except about 20% return for titanium dioxide hydrolysis procedure dilution water and leaching water except, how all the other spent acid of 80% of digestion process, be the key of sulfuric acid method titanium pigment Business survival and development, this limits the sound development of sulfuric acid method titanium pigment to a certain extent.To the process of spent acid, relatively more conventional is be back to titanium dioxide acid hydrolysis workshop section after concentrating at present, but during titanium white waste acid reuse ratio height, impurity is as enrichments in titanium dioxide such as vanadium, chromium, manganese, so to the optimum mode of the process of titanium white waste acid, be titanium white waste acid is applied to other to use sour industry.
Titanium white waste acid concentrating degree is higher, and the repeating utilization factor of spent acid is higher, but concentrated expense sharply rises, far above the expense of the fresh vitriol oil, therefore the concentration general control of concentrated rear spent acid is 50 ~ 65%, now eliminates the impurity such as the vitriol in a large amount of spent acid, is convenient to recycle.More than 55% is reached as the tail gas by gas washing in SA production in CN200910272373 concentrates titanium white waste acid mass percent; In CN201010511576, titanium white waste acid and vitriol oil mixture obtain 58 ~ 69% sulfuric acid; Long Mang group has researched and developed " sulphur-phosphorus-titanium co-production method titanium dioxide new cleanproduction process " leading in the world, it utilizes complex acid explained hereafter titanium white gelled acid, gelled acid is back to titanium dioxide acidolysis and phosphorous chemical industry phosphorus ore extraction workshop section, but needs the phosphorus chemical product of supporting larger production capacity.
Though above method has recycled spent acid, because of the restriction of cost and supporting industry, Some Enterprises can only be adapted to.Part spent acid is had to need process for most of enterprise, therefore neutralisation process titanium white waste acid can only be adopted, it adopts lime or carbide slag etc. to react with spent acid and produces titanium gypsum, with cost is higher, titanium gypsum moisture content is high, the shortcoming of gypsum market saturation during neutralizing treatment exists, substantially titanium gypsum adopts and stacks processing mode, occupy a large amount of land resources, have impact on surrounding enviroment.
Also have pertinent literature and patent report at present to the process of titanium white waste acid, as CN201280044488 adopts titanium dioxide waste acid by sulfuric acid process, after being concentrated, 26 ~ 40% react with magnesium oxide, magnesium hydroxide, magnesiumcarbonate, prepare magnesium sulfate; CN201410370859 reacts with light-burning magnesium powder and prepares technical grade magnesium sulfate after adopting the removal of impurities of titanium white waste acid concentrate; Magnesium sulfate is prepared after hydrogen peroxide oxidation deironing; CN201010110363 titanium white waste acid and magnesia prepare ferromagnesium sulfate, for the preparation of efficient water-purifying agent; With titanium white waste acid and magnesia extracting sulfuric acid ferromagnesium [inorganic chemicals industry handbook 1996], spent acid directly and magnesia react, and then condensing crystal prepares ferromagnesium sulfate.
The dilution gradually of current phosphate rock resource, the use of the phosphorus ore of middle-low grade, substantially be become higher-grade phosphorus ore to use by flotation beneficiation enrichment, but it can produce a large amount of flotation tailingss, often produce 1 ton of high-grade phosphorus ore, by-product about 0.45 ton of mine tailing, mine tailing does not process and will take a large amount of land resources, for the process of mine tailing in CN200810058958, the vitriol oil, strong phosphoric acid and flotation tailings is adopted to prepare phosphor magnesium fertilizer by calcium superphosphate mode; In CN201210036491, mine tailing is calcined then digestion process, obtain phosphorus concentrate and rich magnesium leach liquor, light magnesium oxide prepared by leach liquor;
In sum, although above method effectively disposal and utilization titanium white waste acid or flotation tailings, all exist some shortcomings as: energy consumption is high, production cost is high, supporting production capacity is large.From the angle of the recycle of resource, comprehensive utilizating research and the exploitation of carrying out titanium white waste acid and phosphate ore flotation tailings have great importance, but yet there are no relevant report.
Summary of the invention
The object of the invention is to: overcome the deficiencies in the prior art, a kind of method of comprehensive treating process titanium white waste acid and phosphate ore flotation tailings is provided.
The technical solution used in the present invention is as follows:
A method for comprehensive treating process titanium white waste acid and phosphate ore flotation tailings, comprises the following steps:
(1) adopt mother liquor to pull an oar flotation tailings, then add titanium white waste acid, control pH1.0 ~ 1.5 of reaction, temperature 50 ~ 60 DEG C, reaction times 2h, then solid-liquid separation;
(2) clear liquid of step (1) solid-liquid separation is concentrated into proportion 1.40-1.50g/ml, then adds flocculation agent and carry out flocculating settling, keep system temperature at 80 DEG C ~ 90 DEG C, thick slurry carries out solid-liquid separation;
(3) by the clear liquid of step (2) solid-liquid separation cooling crystallizing at room temperature, centrifugation obtains ferrous sulfate magnesium products, and mother liquor returns step (1).
P in flotation tailings in described step (1)
2o
5content accounts for 3% ~ 6% of total mass;
Described step (1) flotation tailings quality and mother liquor mass ratio are 1:4 ~ 1:5;
In described step (1), the add-on of titanium white waste acid is 3 ~ 5 times of flotation tailings quality;
The solid phase main ingredient that in described step (1), solid phase is separated is the mixture of terra alba, a small amount of silicon and a small amount of undecomposed phosphorus ore, can be used for producing cement setting retarder;
The main component of step (1) and the middle mother liquor of step (3) is magnesium sulfate and ferrous sulfate, and magnesium sulfate content counts 85g/l with MgO, and ferrous sulfate content is with Fe
2o
3count 10g/l, mother liquor proportion is about 1.3g/ml, and mother liquor composition fluctuates than fluctuation with the iron magnesium of sulfuric acid concentration in titanium white waste acid and ferrous sulfate content, phosphate ore flotation tailings quality, cooling final temperature and product.
In described step (2), flocculation agent is selected from anionic polyacrylamide, and compound concentration is 500ppm, and working concentration is 50ppm;
The solid phase that in described step (2), solid phase is separated can be used for producing titanium phosphate fire retardant.
If titanium white waste acid just adopts phosphate ore flotation tailings to neutralize, although in effectively reducing and cost, but wherein the element such as magnesium, iron, sulphur, phosphorus, titanium of phosphate ore flotation tailings not effectively utilize, cause great waste, also take certain land resources.The ferrous sulfate that titanium white waste acid contains is conventional iron supplementary, but it to there is fertilizer efficiency short, Fe
2+easy oxidation by air is the Fe be not easily absorbed by plants
3+etc. shortcoming.The magnesium of phosphate ore flotation tailings to rely on one of natural supplementary fertilizer, namely both combine is ferromagnesium sulfate, it is the stable ferrous iron existed with the form of double salt, magnesium sulfate, as ferrous stablizer, makes ferrous iron long-term stability constant, therefore the compound use of iron and magnesium, sulphur, it is the best medicament preventing and treating yellowtop, especially to fruit tree, mulberry tree, Lawn Yellowing best results, therefore titanium white waste acid and flotation tailings produce ferromagnesium sulfate multi-component composite fertilizer, are one processing modes extremely effectively.
The P of general phosphate ore flotation tailings
2o
5>=6%, for more low-grade phosphate ore flotation tailings, its utility value is just very low, adopts method described in background technology just to lose more than gain.The spent acid that the art of this patent is used and mine tailing composition as follows: the main component (mass percent) of titanium white waste acid: H
2sO
4: 20% ~ 25%, TiO
2: 0.4% ~ 0.6%, Fe
2o
3: 5.7% ~ 7.1%, MgO:0.7% ~ 1.0%, the main component (mass percentage content) of phosphate ore flotation tailings: P
2o
5: 3% ~ 6%, CaO:28% ~ 36%, MgO:17% ~ 21%, Fe
2o
3: 0.3% ~ 0.7%.Phosphate ore flotation tailings is containing a large amount of carbonate and a small amount of fluorapatite (Ca
5f (PO
4)
3), and containing the sulfuric acid of 20% in titanium white waste acid, both are organically combined, reach the object of waste recycling, the resource of spent acid and mine tailing obtains fully effectively utilizing, and the neutralizing treatment and the mine tailing that reduce titanium white waste acid routine stack expense, economize the land resource, keep surrounding enviroment.Concrete chemical equation is as follows:
H
2SO
4+CaCO
3+H
2O=CaSO
4 ·2H
2O+CO
2
H
2SO
4+MgCO3=MgSO
4+H
2O+CO
2
2H
3PO
4+Ti(SO4)
2=Ti(HPO4)
2 ·H
2O+2H
2SO4
Contriver found through experiments, because phosphorite tailings contains a small amount of phosphorus, the reaction of the sulfuric acid in itself and spent acid generates phosphoric acid, titanium in phosphoric acid and spent acid generates the titanium phosphate of colloidal, and it exists and stops in the liquid phase, at concentration process curding out, the crystallization of the serious ferromagnesium sulfate of meeting, by settlement separate removing, can obtain the fire retardant titanium phosphate of high-quality, effective element must make full use of.
The temperature of titanium white waste acid to be reacted with phosphate ore flotation tailings at 50 ~ 60 DEG C and is belonged to thermopositive reaction, and the solubleness of ferrous sulfate and magnesium sulfate is higher, can not cause detrimentally affect to reaction, and spent acid and phosphate ore flotation tailings cost almost nil, therefore production cost is extremely low.
beneficial effect
The present invention has not only effectively processed titanium white waste acid and phosphate ore flotation tailings, optimize sulphur-phosphorus-titanium industry chain further, take full advantage of the iron of titanium white waste acid and phosphate ore flotation tailings, magnesium, sulphur, phosphorus, the elements such as titanium, decrease the impact on surrounding enviroment and land resources, greatly reduce the production cost of phosphorous chemical industry and titanizing work, reach the object of waste recycling, remarkable in economical benefits, the solid phase refuse of separating out is for the production of cement setting retarder and high-quality fire retardant titanium phosphate, whole process is without useless pair discharge, invest little, production cost is low, easy and simple to handle, resource regeneration and green production are had great importance, therefore its popularizing application prospect is wide.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Acidolysis rate:
Certain component substances amount before certain component content * raw materials quality=reaction in raw material-----------------------(1)
After after reaction, certain component content * of residue reacts rear mass of residue=reaction, certain component substances amount-----(2)
((1)-(2))/(1) * 100 or 100*(1-(2)/(1)) be namely the acidolysis rate of this useful component, its unit is %
embodiment 1
By 4000g mother liquor (FeSO
48.78%, MgSO
411.22%) with 1000g flotation tailings (P
2o
54.1%) join in the container of 10L, under rapid mixing conditions, add 4000g spent acid (H
2sO
423.62%), control temperature of reaction 50 DEG C, joining day 30min, slaking 90min, after reaction, pH is 1.5, and filtering separation obtains filter cake washing post-drying and obtains 1030g acid hydrolysis residue.Again by filtrate evaporation concentration to proportion 1.45g/ml, add flocculation agent anionic polyacrylamide, system concentration 50ppm, keep system temperature at 80 DEG C, thick plasm scouring is dried and is obtained titanium phosphate 77g, and clear liquid is cooled to room temperature, centrifugation, obtains ferromagnesium sulfate 2220g.
The acidolysis rate 95.44% of mine tailing magnesium in the present embodiment, the acidolysis rate 57.91% of mine tailing phosphorus.
embodiment 2
By 6000g mother liquor (FeSO48.78%, MgSO411.22%) and 1000g flotation tailings (P
2o
53.1%) join in the container of 12L, under rapid mixing conditions, add 4164g spent acid (H
2sO
423.62%), control temperature of reaction temperature 58 DEG C, joining day 30min, slaking 90min, after reaction, pH is 1.0, and filtering separation obtains filter cake washing post-drying and obtains 1030g acid hydrolysis residue.Again by filtrate evaporation concentration to proportion 1.40g/ml, add flocculation agent anionic polyacrylamide, system concentration 50ppm, keep system temperature at 85 DEG C, thick plasm scouring is dried and is obtained titanium phosphate 62g, and clear liquid is cooled to room temperature, centrifugation, obtains ferromagnesium sulfate 2160g.
The acidolysis rate 97.35% of mine tailing magnesium in the present embodiment, the acidolysis rate 61.42% of mine tailing phosphorus
embodiment 3
By 4000g mother liquor (FeSO48.78%, MgSO411.22%) and 1000g flotation tailings (P
2o
55.8%) join in the container of 10L, under rapid mixing conditions, add 4067g spent acid (H
2sO
423.62%), control temperature of reaction temperature 53 DEG C, joining day 30min, slaking 90min, after reaction, pH is 1.5, and filtering separation obtains filter cake washing post-drying and obtains 1030g acid hydrolysis residue.Again by filtrate evaporation concentration to proportion 1.50g/ml, add flocculation agent anionic polyacrylamide, system concentration 50ppm, keep system temperature at 90 DEG C, thick plasm scouring is dried and is obtained titanium phosphate 112g, and clear liquid is cooled to room temperature, and centrifugation obtains ferromagnesium sulfate 2480g.
The acidolysis rate 95.76% of mine tailing magnesium in the present embodiment, the acidolysis rate 59.17% of phosphorus.
Claims (7)
1. a method for comprehensive treating process titanium white waste acid and phosphate ore flotation tailings, is characterized in that, comprises the following steps:
(1) adopt mother liquor to pull an oar flotation tailings, then add titanium white waste acid, control pH1.0 ~ 1.5 of reaction, temperature 50 ~ 60 DEG C, reaction times 2h, then solid-liquid separation;
(2) clear liquid of step (1) solid-liquid separation is concentrated into proportion 1.40-1.50g/ml, then adds flocculation agent and carry out flocculating settling, keep system temperature at 80 DEG C ~ 90 DEG C, thick slurry carries out solid-liquid separation;
(3) by the clear liquid of step (2) solid-liquid separation cooling crystallizing at room temperature, centrifugation obtains ferrous sulfate magnesium products, and mother liquor returns step (1).
2. the method for a kind of comprehensive treating process titanium white waste acid according to claim 1 and phosphate ore flotation tailings, is characterized in that, P in flotation tailings in described step (1)
2o
5content accounts for 3% ~ 6% of total mass.
3. the method for a kind of comprehensive treating process titanium white waste acid according to claim 1 and phosphate ore flotation tailings, is characterized in that, described step (1) flotation tailings quality and mother liquor mass ratio are 1:4 ~ 1:5.
4. the method for a kind of comprehensive treating process titanium white waste acid according to claim 1 and phosphate ore flotation tailings, is characterized in that, in described step (1), the add-on of titanium white waste acid is 3 ~ 5 times of flotation tailings quality.
5. the method for a kind of comprehensive treating process titanium white waste acid according to claim 1 and phosphate ore flotation tailings, is characterized in that, the solid phase that in described step (1), solid phase is separated can be used for producing cement setting retarder.
6. the method for a kind of comprehensive treating process titanium white waste acid according to claim 1 and phosphate ore flotation tailings, is characterized in that, in described step (2), flocculation agent is anionic polyacrylamide.
7. the method for a kind of comprehensive treating process titanium white waste acid according to claim 1 and phosphate ore flotation tailings, is characterized in that, the solid phase that in described step (2), solid phase is separated can be used for producing titanium phosphate fire retardant.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106379946A (en) * | 2016-08-25 | 2017-02-08 | 襄阳龙蟒钛业有限公司 | Method for production of ferromagnesium sulfate from titanium white waste acid and phosphate ore flotation tailings |
| CN106830098A (en) * | 2017-03-14 | 2017-06-13 | 襄阳龙蟒钛业有限公司 | A kind of production method of ferromagnesium sulfate |
| CN107055495A (en) * | 2017-04-25 | 2017-08-18 | 贵州芭田生态工程有限公司 | A kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging |
| CN107055494A (en) * | 2017-04-13 | 2017-08-18 | 云南胜威化工有限公司 | The method that a kind of spent acid in utilization sulfuric acid method titanium pigment production technology selects phosphorus ore |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774650A (en) * | 2010-02-08 | 2010-07-14 | 枣庄天元精细化工有限公司 | Method for producing high-efficiency purifying agent magnesium ferrous sulfate from titanium dioxide waste acid by using sulphuric acid method |
| CN102328984A (en) * | 2011-08-11 | 2012-01-25 | 四川龙蟒钛业股份有限公司 | Processing method of waste water in phosphorus chemical industry |
-
2015
- 2015-10-27 CN CN201510705393.0A patent/CN105271157B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774650A (en) * | 2010-02-08 | 2010-07-14 | 枣庄天元精细化工有限公司 | Method for producing high-efficiency purifying agent magnesium ferrous sulfate from titanium dioxide waste acid by using sulphuric acid method |
| CN102328984A (en) * | 2011-08-11 | 2012-01-25 | 四川龙蟒钛业股份有限公司 | Processing method of waste water in phosphorus chemical industry |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106379946A (en) * | 2016-08-25 | 2017-02-08 | 襄阳龙蟒钛业有限公司 | Method for production of ferromagnesium sulfate from titanium white waste acid and phosphate ore flotation tailings |
| CN106830098A (en) * | 2017-03-14 | 2017-06-13 | 襄阳龙蟒钛业有限公司 | A kind of production method of ferromagnesium sulfate |
| CN107055494A (en) * | 2017-04-13 | 2017-08-18 | 云南胜威化工有限公司 | The method that a kind of spent acid in utilization sulfuric acid method titanium pigment production technology selects phosphorus ore |
| CN107055495A (en) * | 2017-04-25 | 2017-08-18 | 贵州芭田生态工程有限公司 | A kind of acid phosphorus-containing wastewater is used for the method for phosphorus ore de-magging |
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Inventor after: Fan Xianguo Inventor after: Wen Jun Inventor after: Chen Kui Inventor after: Zhang Yujie Inventor after: Tang Wenjun Inventor after: Zhou Chunyong Inventor after: Deng Bosong Inventor after: Chen Xiang Inventor before: Wen Jun Inventor before: Fan Xianguo Inventor before: Deng Bosong Inventor before: Zhou Chunyong Inventor before: Tang Wenjun Inventor before: Chen Xiang |
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Effective date of registration: 20160920 Address after: 441000, Xiangyang, Hubei province Nanzhang County Town Road, No. 1 Applicant after: XIANGYANG LOMON TITANIUM INDUSTRY CO., LTD. Applicant after: East China University of Science and Technology Address before: 441000, Xiangyang, Hubei province Nanzhang County Town Road, No. 1 Applicant before: XIANGYANG LOMON TITANIUM INDUSTRY CO., LTD. |
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