CN107058740A - A kind of titanium white method for treating waste liquid - Google Patents

A kind of titanium white method for treating waste liquid Download PDF

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Publication number
CN107058740A
CN107058740A CN201710073960.4A CN201710073960A CN107058740A CN 107058740 A CN107058740 A CN 107058740A CN 201710073960 A CN201710073960 A CN 201710073960A CN 107058740 A CN107058740 A CN 107058740A
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CN
China
Prior art keywords
waste liquid
titanium white
filtrate
titanium
crystal
Prior art date
Application number
CN201710073960.4A
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Chinese (zh)
Inventor
朱晓波
李望
汤森
张乾
邢宝林
张玉德
张传祥
谌伦建
陈俊涛
唐庆杰
马名杰
曹建亮
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河南理工大学
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Priority to CN201710073960.4A priority Critical patent/CN107058740A/en
Publication of CN107058740A publication Critical patent/CN107058740A/en

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00Obtaining aluminium
    • C22B21/0015Obtaining aluminium by wet processes
    • C22B21/0023Obtaining aluminium by wet processes from waste materials
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/10Obtaining titanium, zirconium or hafnium
    • C22B34/12Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1236Obtaining 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
    • C22B34/1259Obtaining 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 treatment or purification of titanium containing solutions or liquors or slurries
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/22Obtaining vanadium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention relates to a kind of titanium white method for treating waste liquid.This method is that addition potassium hydroxide mixing regulation pH value is 0 ~ 0.5 into titanium white waste liquid, 60 ~ 120min is stirred under the conditions of temperature is 90 ~ 100 DEG C, then 0 ~ 10 DEG C is cooled to rapidly gradually crystallizes out alum crystal, terminate rear separation of solid and liquid and obtain 12 hydrazine aluminum sulfate potassium and filtrate that purity is more than 99.5%, it is 2.2 ~ 2.8 to add potassium hydroxide and potassium chlorate regulation pH value into filtrate again, 90 ~ 150min is stirred under the conditions of temperature is 90 ~ 100 DEG C, autunezite crystal is gradually crystallized out in filtrate, terminate rear separation of solid and liquid to obtain three water autunezite crystal of the purity more than 99% and contain scandium, vanadium, your the dilute filtrate of titanium, your dilute filtrate obtains rare precious metal after isolating and purifying.The present invention have it is simple to operate, alkali consumption is small, and cost is low, and iron, aluminium and rare precious metal are recyclable, the characteristics of product purity is high.

Description

A kind of titanium white method for treating waste liquid
Technical field
The invention belongs to titanium white waste liquid comprehensive treatment technique field, and in particular to a kind of titanium white method for treating waste liquid.
Background technology
Titanium white waste liquid is the acid waste water for preparing the generation of titanium dioxide process.The method that China prepares production titanium dioxide is mainly Sulfuric acid process, result in one ton of titanium dioxide of every production, it will produce 50~100m3Titanium white waste liquid, not only acid strong, it contains greatly The iron ion and aluminium ion of amount, the rare precious metal ion such as also a small amount of titanium, scandium, vanadium, therefore, processing titanium white waste liquid is not only to ring There is protective effect in border, also can be as the secondary resource for reclaiming valuable metal, with important economical and environmentally friendly meaning.
At present, the processing of titanium white waste liquid focuses mostly in the recovery and utilization of acid, the extracting and developing of rare precious metal and iron and returns Receive, and acid-base neutralization prepares white gypsum etc..Such as yellow coral have studied reclaims titanium white waste liquid using the method for evaporation and UF membrane In sulfuric acid, also have the highly acid of research and utilization titanium white waste liquid, as leaching agent leach extract red mud in scandium (Huang Shan, Li Zheng The improvement of mountain titanium white waste liquids, recovery and comprehensive utilizating research [J] developments of resources and market, 2007,23 (9): 778- 781;Tao Yang, Wang Zhijian, Xiao Jing wait extract technology research [J] mining and metallurgys that scandium is carried in red muds and titanium white waste liquid, 2015, 24(5): 37-40;Liu Jibo, Tao Yang, Wu Xitao waits synthetical recoveries to handle waste red mud residues and titanium white waste liquid Method patents of invention, the A of CN 103614563).This process efficiently utilizes the acidity of titanium white waste liquid, but to therein The recovery of the essential elements such as iron, aluminium is not referred to, while the liquid after turnover is still difficult and recycles.For titanium white waste liquid (Xu's copper text emulsion liquid membranes extract Microamounts of Scandium in sulfate process titanium dioxide waste liquid for the extraction that middle precious and rare metals recovery focuses mostly in scandium Study [J] rare metals, 1994,18 (4):245-248), due in titanium white waste liquid scandium concentration it is relatively low, the impurity such as iron, aluminium Ion concentration is very high, causes to reclaim scandium process separation difficulty, the purity of scandium product is low.Using addition calcic alkaline matter regulation pH Value, can preparing white gypsum, (research [J] that Xu's copper text emulsion liquid membranes extract Microamounts of Scandium in sulfate process titanium dioxide waste liquid is rare Metal, 1994,18 (4):245-248), this process alkali consumption is high, and the purity of white gypsum is low, wherein containing substantial amounts of iron, aluminium Deng impurity.In addition, also scholar's research using titanium white waste liquid production iron oxide yellow pigments and iron oxide, (fourth is outstanding, He Xiyang, Liu Xiao Swallow prepares iron oxide yellow pigments research [J] chemical research and application, 2008,20 (7) using hydrochloric acid method titanium white waste liquid: 932- 934;Fourth outstanding person hydrochloric acid methods production titanium white waste liquid high purity Fe2O3Experimental study [J] chemical research and application, 2007, 14(4):39-41), this process operation is complicated, it is necessary to which multi-step impurity removal operation, alkali consumption greatly, is only applicable to hydrochloric acid method titanium white and given up Liquid, and the main source of titanium white waste liquid is titanium dioxide sulfuric acid preparation technology.
Therefore, there is complex operation in the processing procedure of current titanium white waste liquid, and alkali consumption is big, and cost is high, processing recovery pair As single, the product impurity of generation is high and purity is low, it is impossible to large defect such as recycle.
The content of the invention
The purpose of the present invention exactly provides a kind of titanium white waste liquid for the weak point in the presence of above-mentioned prior art Processing method, this method meets that titanium white liquid waste processing is simple to operate, and alkali consumption is small, and cost is low, and iron, aluminium and rare precious metal can be returned Receive, product alum, autunezite and your dilute filtrate purity are high, can be with the requirement of large recycling.
The purpose of the present invention can be realized by following technique measures:
The step of titanium white method for treating waste liquid of the present invention, is as follows:Potassium hydroxide mixing regulation pH value is added into titanium white waste liquid is 0 ~ 0.5,60 ~ 120min is stirred under the conditions of temperature is 90 ~ 100 DEG C, is then cooled to rapidly in 0 ~ 10 DEG C, titanium white waste liquid gradually Alum crystal is crystallized out, terminates rear separation of solid and liquid and obtains alum crystal and filtrate that purity is more than 99.5%;Again Into filtrate add potassium hydroxide and potassium chlorate regulation pH value be 2.2 ~ 2.8, temperature be 90 ~ 100 DEG C under the conditions of stirring 90 ~ Autunezite crystal is gradually crystallized out in 150min, filtrate, terminates rear separation of solid and liquid and obtains the yellow potassium iron that purity is more than 99% Alum crystal and your dilute filtrate, your dilute filtrate can obtain the rare precious metal that purity is more than 99% after isolating and purifying.
Institute's titanium white waste liquid is the waste liquid of gained after ilmenite prepares titanium dioxide through sulfuric acid pressure leaching hydrolysis in the present invention, is given up Liquid hydrogen ion concentration is more than 1 mol/L, and iron concentration is more than 4 g/L, and aluminium ion concentration is more than 1 g/L.
Heretofore described alum crystal is 12 hydrazine aluminum sulfate potassium, and wherein the rate of recovery of aluminium is more than 95%.
Heretofore described autunezite crystal is three water autunezite, and wherein the rate of recovery of iron is more than 95%.
Your dilute filtrate of gained is the solution containing scandium, titanium and vanadium in the present invention, and scandium concentration is more than 10 mg/L, and vanadium concentration is big In 50 mg/L, titanium concentration is more than 500 mg/L.
It is heretofore described to isolate and purify as ion exchange, solvent extraction and charcoal absorption integrated processes.
Gained rare precious metal is respectively vanadic anhydride, scandium oxide and the titanium dioxide that purity is more than 99% in the present invention Titanium products.
The potassium hydroxide and the mass ratio of potassium chlorate added again into filtrate in the present invention is 2~5:1.
Beneficial effects of the present invention are as follows:
The present invention prepares product sulphur using method processing titanium white devil liquor recovery aluminium therein, iron and the rare precious metal of two sections of crystallizations Sour aluminium potassium and autunezite purity are high, and cost is low, and the pH value of your dilute filtrate is in 2.5 or so, wherein iron, aluminium impurity content after processing It is low, it is very beneficial for the rare precious metals such as scandium, titanium, vanadium and is separated and recovered using ion exchange or solvent-extracted method.Titanium white Waste liquid by add potassium hydroxide adjust pH value to 0 ~ 0.5, abundant dissolving is stirred under the high temperature conditions, with temperature by Gradually reduce, crystal is gradually formed and grown up, the 12 hydrazine aluminum sulfate potassium crystal that purity is more than 99.5%, aluminium recovery can be generated More than 95%, and iron, titanium, scandium plasma can be remained in the solution, realize the recovery of aluminium in titanium white waste liquid.Alum is crystallized Filtrate afterwards, then add potassium hydroxide and potassium chlorate and adjust pH value to 2.2 ~ 2.8, the stirred crystallization under the conditions of 90 ~ 100 DEG C, with The progress of stirring, crystal is gradually formed and grown up, the autunezite solution that purity is more than 99% can be generated, iron recovery is more than 95%, and scandium, titanium and vanadium rare precious metal ion can be residued in solution, now the pH value of solution is exactly dilute between 2.2 ~ 2.8 The optimal pH scope that precious metal separation is extracted, can be reclaimed using ion exchange, solvent extraction method and charcoal absorption method Scandium, titanium and vanadium.The present invention is used as crystallization medicament and carries out titanium white liquid waste processing recovery aluminium, iron by adding potassium hydroxide and potassium chlorate And rare precious metal, the Selective Separation of valuable element is realized, reagent consumption is reduced, alum, autunezite and dilute expensive Impurity content is few in filtrate, and product purity is high, and alum purity is more than 99.5%, and autunezite purity is more than 99%, and titanium white gives up The rate of recovery of aluminium and iron is all higher than scandium in 95%, your dilute filtrate, titanium, vanadium purity height in liquid, and impurity content is few, and solution ph is suitable The separating-purifying of rare precious metal.
Therefore, the present invention is simple to operate with titanium white liquid waste processing, and alkali consumption is small, and cost is low, and iron, aluminium and rare precious metal are equal Recyclable, product alum, autunezite and your dilute filtrate purity are high, the characteristics of can be with large recycling.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
The present invention is below with reference to embodiment(Accompanying drawing)It is further described:
It is now that the technical parameter Unify legislation involved by the specific embodiment of the invention is as follows to avoid repeated description:Institute's titanium white Waste liquid is the waste liquid of gained after ilmenite prepares titanium dioxide through sulfuric acid pressure leaching hydrolysis, and waste liquid hydrogen ion concentration is more than 1 mol/ L, iron concentration is more than 4 g/L, and aluminium ion concentration is more than 1 g/L, described to isolate and purify as ion exchange, solvent extraction and work Property charcoal absorption integrated processes, your the dilute filtrate is that scandium concentration is more than 10 mg/L, and vanadium concentration is more than 50 mg/L, and titanium concentration is more than 500 mg/L acid solution, the rare precious metal is vanadic anhydride, scandium oxide and titanium dioxide product, specific embodiment In repeat no more.
Embodiment 1
It is 0 ~ 0.5 that potassium hydroxide mixing regulation pH value is added into titanium white waste liquid, and 100 are stirred under the conditions of temperature is 90 ~ 100 DEG C ~ 120min, is then cooled to rapidly in 0 ~ 10 DEG C, titanium white waste liquid and gradually crystallizes out alum crystal, terminate rear solid-liquid Separation obtains 12 hydrazine aluminum sulfate potassium crystal and the filtrate that purity is more than 99.8%, and the rate of recovery of aluminium is more than 98%;Again to filtrate In with 2~5:1 mass ratio addition potassium hydroxide and potassium chlorate regulation pH value is 2.6 ~ 2.8, is 90 ~ 100 DEG C of conditions in temperature Autunezite crystal is gradually crystallized out in 130 ~ 150min of lower stirring, filtrate, terminates rear separation of solid and liquid acquisition purity and is more than 99.5% three water autunezite crystal and your dilute filtrate, the rate of recovery of iron are more than 97%, and your dilute filtrate can be obtained after isolating and purifying Obtain the rare precious metal that purity is more than 99.3%.
Embodiment 2
Into titanium white waste liquid add potassium hydroxide mixing regulation pH value be 0 ~ 0.5, temperature be 90 ~ 100 DEG C under the conditions of stirring 80 ~ 100min, is then cooled to rapidly in 0 ~ 10 DEG C, titanium white waste liquid and gradually crystallizes out alum crystal, terminates rear solid-liquid point From 12 hydrazine aluminum sulfate potassium crystal and filtrate that purity is more than 99.6% is obtained, the rate of recovery of aluminium is more than 96%;Again into filtrate With 2~5:1 mass ratio addition potassium hydroxide and potassium chlorate regulation pH value is 2.4 ~ 2.6, under the conditions of temperature is 90 ~ 100 DEG C Stir in 110 ~ 130min, filtrate and gradually crystallize out autunezite crystal, terminate rear separation of solid and liquid acquisition purity and be more than 99.2% three water autunezite crystal and your dilute filtrate, the rate of recovery of iron are more than 96%, and your dilute filtrate can be obtained after isolating and purifying Obtain the rare precious metal that purity is more than 99.2%.
Embodiment 3
Into titanium white waste liquid add potassium hydroxide mixing regulation pH value be 0 ~ 0.5, temperature be 90 ~ 100 DEG C under the conditions of stirring 60 ~ 80min, is then cooled to rapidly in 0 ~ 10 DEG C, titanium white waste liquid and gradually crystallizes out alum crystal, terminates rear solid-liquid point From 12 hydrazine aluminum sulfate potassium crystal and filtrate that purity is more than 99.5% is obtained, the rate of recovery of aluminium is more than 95%;Again into filtrate With 2~5:1 mass ratio addition potassium hydroxide and potassium chlorate regulation pH value is 2.2 ~ 2.4, under the conditions of temperature is 90 ~ 100 DEG C Stir in 90 ~ 110min, filtrate and gradually crystallize out autunezite crystal, terminate rear separation of solid and liquid and obtain purity more than 99% Three water autunezite crystal and your dilute filtrate, the rate of recovery of iron is more than 95%, and your dilute filtrate can obtain purity after isolating and purifying Rare precious metal more than 99%.
The present invention is simple to operate with titanium white liquid waste processing, and alkali consumption is small, and cost is low, and iron, aluminium and rare precious metal can be returned Receive, product alum, autunezite and your dilute filtrate purity are high, the characteristics of can be with large recycling.

Claims (8)

1. a kind of titanium white method for treating waste liquid, it is characterised in that:The process method step is as follows:Hydrogen is added into titanium white waste liquid Potassium oxide mixing regulation pH value is 0 ~ 0.5, stirs 60 ~ 120min under the conditions of temperature is 90 ~ 100 DEG C, 0 is then cooled to rapidly ~ 10 DEG C, alum crystal is gradually crystallized out in titanium white waste liquid, terminates rear separation of solid and liquid and obtain purity to be more than 99.5% Alum crystal and filtrate;It is 2.2 ~ 2.8 to add potassium hydroxide and potassium chlorate regulation pH value into filtrate again, is 90 in temperature Stirred under the conditions of ~ 100 DEG C in 90 ~ 150min, filtrate and gradually crystallize out autunezite crystal, terminated rear separation of solid and liquid and obtain Purity is more than 99% autunezite crystal and your dilute filtrate, and it is dilute more than 99% that your dilute filtrate can obtain purity after isolating and purifying Noble metal.
2. titanium white method for treating waste liquid according to claim 1, it is characterised in that:The titanium white waste liquid is ilmenite through sulphur Sour pressure leaching hydrolysis prepares the waste liquid of gained after titanium dioxide, and waste liquid hydrogen ion concentration is more than 1 mol/L, and iron concentration is more than 4 g/L, aluminium ion concentration is more than 1 g/L.
3. titanium white method for treating waste liquid according to claim 1, it is characterised in that:The alum crystal is Shi Ershui Alum is closed, the wherein rate of recovery of aluminium is more than 95%.
4. titanium white method for treating waste liquid according to claim 1, it is characterised in that:The autunezite crystal is that three water are yellow The rate of recovery of krausite, wherein iron is more than 95%.
5. titanium white method for treating waste liquid according to claim 1, it is characterised in that:Your the dilute filtrate is to contain scandium, titanium With the solution of vanadium, scandium concentration is more than 10 mg/L, and vanadium concentration is more than 50 mg/L, and titanium concentration is more than 500 mg/L.
6. titanium white method for treating waste liquid according to claim 1, it is characterised in that:It is described isolate and purify for ion exchange, Solvent extraction and charcoal absorption integrated processes.
7. titanium white method for treating waste liquid according to claim 1, it is characterised in that:The rare precious metal is respectively that purity is big In 99% vanadic anhydride, scandium oxide and titanium dioxide product.
8. titanium white method for treating waste liquid according to claim 1, it is characterised in that:The hydrogen-oxygen added again into filtrate The mass ratio for changing potassium and potassium chlorate is 2~5:1.
CN201710073960.4A 2017-02-10 2017-02-10 A kind of titanium white method for treating waste liquid CN107058740A (en)

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Cited By (1)

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Application publication date: 20170818