CN107200364B - A kind of abstraction impurity removal method to industrial scum sulphuric leachate - Google Patents
A kind of abstraction impurity removal method to industrial scum sulphuric leachate Download PDFInfo
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- CN107200364B CN107200364B CN201710322960.3A CN201710322960A CN107200364B CN 107200364 B CN107200364 B CN 107200364B CN 201710322960 A CN201710322960 A CN 201710322960A CN 107200364 B CN107200364 B CN 107200364B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0009—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of abstraction impurity removal methods to industrial scum sulphuric leachate comprising five links such as soda soap, nickel soap, extraction, washing, back extraction select P507As extractant, solvent naphtha or sulfonated kerosene are as diluent, the binding ability of certain metal and extractant can be destroyed according to the hydrochloric acid of the binding ability difference of various metal ion extraction agent and various concentration, to make metal target Ni, Fe ion isolation, by the removal of one steps of metal ions such as Co, Cu, Pb, Zn, Ca, Mg in leachate, so that industrial scum sulphuric leachate deep purifying, is made impurity content low nickel sulfate solution and solution of ferrous chloride.The abstraction impurity removal method of the present invention, technological process is simple and direct, and removal of impurity is high, and produced nickel sulfate solution meets the quality requirement of production nickel sulfate and iron oxide product with solution of ferrous chloride quality.
Description
Technical field
The invention belongs to technical field of wet metallurgy, are related to a large amount of industry of output in non-ferrous metal nickel, cobalt hydrometallurgy
A kind of scum, and in particular to abstraction impurity removal method to industrial scum sulphuric leachate.
Background technology
Output largely in cinder field stockyard store up by industrial scum, industrial scum in nickel, cobalt hydrometallurgy flow, both occupies field
Ground, but there are the hidden danger of contaminated soil, while in industrial scum the waste of resource is caused with a large amount of valuable nickel metal.
To realize recycling for resource, it is necessary to carry out the technical research work that industrial scum recycles；It will be from admittedly
Valuable metal nickel therein is extracted in state substance, the best method of iron is to leach solid matter, allow iron from Solid State Transformation
The foreign metal ions such as cobalt, magnesium at ionic species, but while leaching nickel, iron in solid matter also enter in solution, to
Nickel, the iron in solution are extracted, the foreign metal ion in solution need to be removed；The method of separation metal includes from solution
Electrolysis, ion-exchange and the precipitation method.The higher electric energy of electrolysis consumption, cathode efficiency is low, solution treatment amount is small, no
It is suitble to large-scale production；Ion-exchange generates a large amount of wash waters, is also unsuitable for mass producing, by temperature when the precipitation method extract iron
Degree and pH value influence, and between various precipitations phase co-conversion speed it is slower, limit its application industrially.
Invention content
It is an object of the invention to use extractant appropriate, the plurality of impurities metal ion extraction in leachate is removed
It goes, so that gained nickel sulfate solution and solution of ferrous chloride is reached the requirement of production nickel sulfate product and iron oxide product, carry
A kind of abstraction impurity removal method to industrial scum sulphuric leachate is supplied.
The technical solution used in the present invention is：
A kind of abstraction impurity removal method to industrial scum sulphuric leachate, it includes the following steps：
Step 1：The sulfuric acid leaching process of industrial scum：
It being reacted with industrial scum using the industrial sulphuric acid after dilution, leaching process is carried out in three steps,
A. industrial scum is reacted with the industrial sulphuric acid after dilution, reaction process control scum pulp liquid consolidates volume ratio 4:1-
6:1,70-90 DEG C of temperature, the industrial sulphuric acid [H after dilution+] a concentration of 80-90g/L, react 0.5h；
B. iron powder will be added in the slurries of step a outputs, iron powder addition is leachate Cu2+1-1.2 times of amount, reaction
0.5h；
C. Na will be added in the slurries of step b outputs2SO3, sodium sulfite addition is leachate Fe3+1-1.2 times of amount,
It is filtered after reaction 2h, obtains the higher industrial scum sulphuric leachate of impurity content, i.e. ferrous sulfate（Nickel sulfate）Solution；
Step 2：Soda soap will contain extractant P507Organic phase and liquid caustic soda saponification, saponification are carried out in saponification kettle
Rate control is 50-55%, forms soda soap organic phase；
Step 3：Nickel soap, the soda soap organic phase prepared by the nickel sulfate solution and step 2 by the 50-80g/L containing Ni carry out
Reaction, reaction process adjust the volume ratio of nickel soap process organic phase and water phase, organic phase and water phase body according to the Ni contents of water phase
Product is than control in 3-5:1, liquid Ni contents are less than 0.1g/L after ensureing nickel soap, and nickel soap is carried out in extraction box, using 2-3 stage countercurrents
Nickel soap, after the completion of nickel soap process, soda soap organic phase is converted into nickel soap organic phase；
Step 4：Extraction, by the nickel soap organic phase and the finally obtained industrial scum sulfuric acid of step 1 prepared by step 3
Leachate carries out mixed phase, and the volume ratio for controlling organic phase and water phase is 3-4:1, pH of leaching solution 1.5-2.0, mixed phase time 10-
15min, using 3-4 stage countercurrents extract, so that leachate is fully reacted with organic phase, the ferrous ion and foreign metal in solution from
Son exchanged with the nickel ion in nickel soap organic phase, so that ferrous ion and foreign metal ion is combined with organic phase, and nickel from
Son reenters in water phase, realizes that nickel metal ion is detached with foreign metal, iron metal ion and foreign metal ion with it is organic
The combination of phase after dedoping step, forms the organic phase and raffinate of load iron metal ion and foreign metal ion, raffinate
Liquid is the nickel sulfate solution of qualification；
Step 5：Load organic detergent, by prepared by step 4 load ferrous ion and foreign metal ion it is organic
Mixed phase is mutually carried out with dilute sulfuric acid, organic phase is 1-1.5 with the control of water phase volume ratio:1, dilute sulfuric acid pH value 0.5-1.0, mixed phase time
For 10-15min, is washed using 1-2 grades, the foreign metal ion in load organic phases is made to enter in water phase, and iron ion continues
It is supported in organic phase；
Step 6：Back extraction, using [H+] as back washing agent, rate-determining steps five obtain negative for a concentration of 8-8.5mol/L hydrochloric acid
The stream for being loaded with machine and water phase compares for 1-1.5:1, it is stripped using 3-4 stage countercurrents, mixed phase time 10-15min makes the Asia in organic phase
Iron ion reenters in water phase, and organic phase is regenerated, and organic circulation uses after back extraction, the strip liquor of gained is after back extraction
Qualified solution of ferrous chloride.
As a further improvement on the present invention, organic phase is made of extractant and diluent in the step 2, wherein extracting
Agent is taken to account for the 25%-30% of organic phase volume, diluent accounts for the 70%-75% of organic phase volume, and diluent is solvent naphtha
Or sulfonated kerosene.
The beneficial effects of the invention are as follows：The present invention cleans to industrial scum sulphuric leachate using extraction, technological process
Simple and direct, removal of impurity is high, and produce nickel sulfate solution, solution of ferrous chloride quality satisfaction produce nickel sulfate, iron oxide product
Quality requirement.
Industry scum of the invention passes through sulfuric acid, iron powder, Na first2SO3Obtain the higher industrial scum sulfuric acid leaching of impurity content
Go out liquid, i.e. ferrous sulfate（Nickel sulfate）Solution；Containing plurality of impurities metals such as Ni, Co, Cu, Pb, Zn, Ca, Mg in leachate, leach
The composition of liquid is shown in Table 1.Then foreign metal is detached with nickel, iron by the method for abstraction impurity removal, by after soda soap it is organic into
Row nickel soap, efficiently solves raffinate（Nickel sulfate solution）The problem of middle Na high, nickel soap are organic with industrial scum sulphuric leachate
Reaction obtains to which the organic phase of the low nickel sulfate solution of impurity content and load iron metal ion and foreign metal ion be made
To nickel sulfate solution Co, Cu, Pb, Zn be respectively less than 0.003g/L, Ca, Mg are respectively less than 0.01g/L, and Na meets less than 0.2 g/L
Produce the requirement of nickel sulfate product.The organic phase for loading iron metal ion and foreign metal ion is anti-through dilute sulfuric acid washing, hydrochloric acid
Extract to obtain solution of ferrous chloride, Ni, Co, Cu, Pb, Zn, Ca, Mg are respectively less than 0.003g/L and disclosure satisfy that production in solution of ferrous chloride
The requirement of iron oxide product, to realize recycling for resource.
The industrial scum sulphuric leachate composition table g/L of table 1
The content of each metal ion is as shown in table 2 in nickel sulfate after removal of impurities.
2 nickel sulfate solution analysis result g/L of table
The content of each metal ion is as shown in table 3 in removal of impurities afterchlorinate ferrous iron.
3 solution of ferrous chloride analysis result g/L of table
The present invention is divided into soda soap, extraction to the process of industrial scum sulphuric leachate abstraction impurity removal, loads organic detergent, anti-
The four processes such as extraction select P507As extractant, solvent naphtha or sulfonated kerosene are made as being diluted to by extractant and diluent
It is different according to the binding ability of various metal ion extraction agent for organic phase, by controlling organic phase compared with water phase, make molten
Metal ion in liquid is combined with organic phase, and the combination of certain metal and extractant can be destroyed further according to the hydrochloric acid of various concentration
Ability, to make metal target Ni, Fe ion isolation, by Co, Cu, Pb, Zn, Ca, Mg etc. in industrial scum sulphuric leachate
One step of metal ion removes so that industrial scum sulphuric leachate deep purifying, be made the low nickel sulfate solution of impurity content and
Solution of ferrous chloride.So that industrial scum sulphuric leachate deep purifying.
Description of the drawings
The process flow chart of Fig. 1 present invention.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
Embodiment 1
A kind of abstraction impurity removal method to industrial scum sulphuric leachate, it includes the following steps：
Step 1：Liquid prepares before extraction, scum pulp liquid-solid ratio 4 in industrial scum sulfuric acid leaching reaction process:1 temperature 76
DEG C, sulfuric acid concentration 80.5g/L reacts 0.5h；Then plus iron powder, iron powder addition are leachate Cu2+1 times of amount, reaction
0.5h, then plus sodium sulfite, addition are Fe in leachate3+1.1 times of amount react 2h, obtain the higher work of impurity content
Industry scum sulphuric leachate, industry scum leachate composition used are as shown in table 4.
The industrial scum sulphuric leachate composition table g/L of table 4
Step 2：Soda soap, using P507For extractant, the configuration proportion for extracting organic phase is：25%P507+ 75% solvent naphtha
（Volume ratio）, organic after preparing be added to 30% liquid caustic soda and carry out saponification, and saponification rate 50% forms soda soap organic phase.
Step 3：Nickel soap, by the nickel sulfate solution of Ni contents 55g/L and soda soap organic phase according to organic phase and water phase body
Product is than control 3:1 mixing, 3 stage countercurrent nickel soaps, the organic of formation is nickel soap organic phase.
Step 4：Extraction, nickel soap organic phase carry out mixed phase, nickel with the finally obtained industrial scum sulphuric leachate of step 1
Soap organic phase is 3 with aqueous phase stream ratio:1, liquid pH value is 2.0 before extracting, the mixed phase time：10min is formed by after 3 grades of counter-current extraction
Water phase is that raffinate is qualified nickel sulfate solution, and composition is shown in Table 5, and organic phase is load iron metal ion and foreign metal ion
Organic phase.
5 raffinate analysis result g/L of table
Step 5：Washing, washs the organic phase that step 4 obtains, and washing sulfuric acid pH value is 1.0, in washing process
It is 1 that the stream of organic phase and water phase, which compares,:1, so that the foreign metal ion in load organic phases is entered in water phase, and ferrous ion continues
It is supported in organic phase.
Step 6：Back extraction, the load that step 5 is obtained as back washing agent using the hydrochloric acid of a concentration of 8mol/L it is organic into
Row is stripped, and it is 1 that organic and water phase stream is loaded in stripping process to compare:1,3 grades of series, mixed phase time 15min is organic after regeneration to follow
Ring utilizes, and the solution of ferrous chloride that water phase is qualified is formed by after back extraction, and composition is shown in Table 6.
6 solution of ferrous chloride analysis result g/L of table
Embodiment 2
A kind of abstraction impurity removal method to industrial scum sulphuric leachate, it includes the following steps：
Step 1：Liquid prepares before extraction, scum pulp liquid-solid ratio 4.5 during Leach reaction:1 80 DEG C of temperature, sulfuric acid concentration
For 83g/L, 0.5h is reacted；Then plus iron powder, iron powder addition are leachate Cu2+1.2 times of amount react 0.5h, then plus sub-
Sodium sulphate, addition are leachate Fe3+1 times of amount reacts 2h, obtains the higher industrial scum sulphuric leachate of impurity content, institute
It is as shown in table 7 with industrial scum leachate composition.
The industrial scum sulphuric leachate composition table g/L of table 7
Step 2：Soda soap, using P507For extractant, the configuration proportion for extracting organic phase is：25%P507+ 75% solvent naphtha
（Volume ratio）, organic after preparing be added to 30% liquid caustic soda and carry out saponification, saponification rate 52%, be formed by it is organic for soda soap it is organic
Phase.
Step 3：Nickel soap, by the nickel sulfate solution of Ni contents 62g/L and soda soap organic phase according to organic phase and water phase volume
Than controlling 3:1 mixing, 2 stage countercurrent nickel soaps, it is nickel soap organic phase to be formed by organic.
Step 4：Extraction, nickel soap organic phase carry out mixed phase, nickel with the finally obtained industrial scum sulphuric leachate of step 1
Soap organic phase is 1.5 with aqueous phase stream ratio, the mixed phase time：12min, it is conjunction that be formed by water phase after 3 grades of counter-current extraction, which be raffinate,
Lattice nickel sulfate solution, composition are shown in Table 8, and organic phase is to load the organic phase of iron metal ion and foreign metal ion.
8 raffinate analysis result g/L of table
Step 5：Washing, washs the organic phase that step 4 obtains, and washing sulfuric acid pH value is 1.0, in washing process
It is 1.5 that the stream of organic phase and water phase, which compares,:1, so that the foreign metal ion in load organic phases is entered in water phase, and ferrous ion after
It is continuous to be supported in organic phase.
Step 6：Back extraction, the load obtained to step 5 as back washing agent using the hydrochloric acid of a concentration of 8.2mol/L are organic
It is stripped, it is 1 that organic and water phase stream is loaded in stripping process to compare:1,4 grades of series, mixed phase time 13min is organic after regeneration
It recycles, the solution of ferrous chloride that water phase is qualified is formed by after back extraction, composition is shown in Table 9.
9 solution of ferrous chloride analysis result g/L of table
Embodiment 3
A kind of abstraction impurity removal method to industrial scum sulphuric leachate, it includes the following steps：
Step 1：Liquid prepares before extraction, scum pulp liquid-solid ratio 5 during Leach reaction:1 85 DEG C of temperature, sulfuric acid concentration are
85g/L reacts 0.5h；Then plus iron powder, iron powder addition are leachate Cu2+1.1 times of amount react 0.5h, then add sulfurous
Sour sodium, addition are leachate Fe3+1.1 times of amount react 2h, obtain the higher industrial scum sulphuric leachate of impurity content,
Industry scum leachate composition used is as shown in table 10.
The industrial scum sulphuric leachate composition table g/L of table 10
Step 2：Soda soap, using P507For extractant, the configuration proportion for extracting organic phase is：30%P507+ 70% solvent naphtha
（Volume ratio）, organic after preparing be added to 30% liquid caustic soda and carry out saponification, saponification rate 50%, be formed by it is organic for soda soap it is organic
Phase.
Step 3：Nickel soap, by the nickel sulfate solution of Ni contents 58g/L and soda soap organic phase according to organic phase and water phase volume
Than controlling 3:1 mixing, 3 stage countercurrent nickel soaps, it is nickel soap organic phase to be formed by organic.
Step 4：Extraction, nickel soap organic phase carry out mixed phase, nickel with the finally obtained industrial scum sulphuric leachate of step 1
Soap organic phase is 4 with aqueous phase stream ratio:1, liquid pH value is 2.0 before extracting, the mixed phase time：10min, 4 grades of adverse current series, is formed by water
It is mutually qualified nickel sulfate solution, composition is shown in Table 11, and organic phase is to load the organic phase of iron metal ion and foreign metal ion.
11 raffinate analysis result g/L of table
Step 5：Washing, washs the organic phase that step 4 obtains, and washing sulfuric acid pH value is 0.5, in washing process
It is 1 that the stream of organic phase and water phase, which compares,:1, so that the foreign metal ion in load organic phases is entered in water phase, and ferrous ion continues
It is supported in organic phase.
Step 6：Back extraction, the load obtained to step 5 as back washing agent using the hydrochloric acid of a concentration of 8.5mol/L are organic
It is stripped, it is 1.5 that organic and water phase stream is loaded in stripping process to compare:1,4 grades of series, mixed phase time 10min has after regeneration
Machine recycles, and the solution of ferrous chloride that water phase is qualified is formed by after back extraction, and composition is shown in Table 12.
12 solution of ferrous chloride analysis result g/L of table
Claims (3)
1. a kind of abstraction impurity removal method to industrial scum sulphuric leachate, it is characterised in that：It includes the following steps：
Step 1：The sulfuric acid leaching process of industrial scum：
A. the industrial sulphuric acid of industrial scum and a concentration of 80-90g/L are pressed into solid-liquid volume ratio 1:4-6 carries out scum pulp, control
70-90 DEG C of temperature reacts 0.5h, obtains slurries；
B. iron powder will be added in the slurries of step a outputs, iron powder addition is leachate Cu2+1-1.2 times of amount reacts 0.5h,
Obtain slurries；
C. sodium sulfite Na will be added in the slurries of step b outputs2SO3, sodium sulfite addition is leachate Fe3+The 1-1.2 of amount
Times, it is filtered after reacting 1-2h, obtains the higher industrial scum sulphuric leachate of impurity content, i.e. sulfur acid ferrous iron, sulfuric acid
The solution of nickel；
Step 2：Soda soap will contain extractant P507Organic phase reacted with liquid caustic soda, saponification, saponification are carried out in saponification kettle
Rate control is 50-55%, forms soda soap organic phase；
Step 3：Nickel soap, the soda soap organic phase prepared by the nickel sulfate solution and step 2 by the 50-80g/L containing Ni carry out anti-
It answers, reaction process adjusts the volume ratio of nickel soap process organic phase and water phase, organic phase and water phase volume according to the Ni contents of water phase
Than controlling in 3-5:1, liquid Ni contents are less than 0.1g/L after ensureing nickel soap, and using 2-3 stage countercurrent nickel soaps, nickel soap process is completed
Afterwards, soda soap organic phase is converted into nickel soap organic phase；
Step 4：Extraction, by the nickel soap organic phase and the finally obtained industrial scum sulfuric acid leaching of step 1 prepared by step 3
Liquid carries out mixed phase, and the stream for controlling organic phase and water phase compares for 3-4:1, pH of leaching solution 1.5-2.0, mixed phase time 10-15min,
It is extracted using 3-4 stage countercurrents, so that leachate is fully reacted with organic phase, the ferrous ion and foreign metal ion in solution and nickel
Nickel ion in soap organic phase exchanges, and nickel ion enters in water phase, and foreign metal and ferrous metal enter load organic phases
In；The organic phase and raffinate of load iron metal ion and foreign metal ion are formed, raffinate is that qualified nickel sulfate is molten
Liquid；
Step 5：Load organic phases wash, by step 4 obtain load ferrous ion and foreign metal ion organic phase with
Dilute sulfuric acid carries out mixed phase, and organic phase is 1-1.5 with the control of water phase volume ratio:1, dilute sulfuric acid pH value 0.5-1.0, mixed phase time is
10-15min is washed using 1-2 grades, the foreign metal ion in load organic phases is made to enter in water phase, and ferrous ion continues
It is supported in organic phase；
Step 6：Back extraction, using [H+] as back washing agent, the load that rate-determining steps five obtain has for a concentration of 8-8.5mol/L hydrochloric acid
The stream of machine phase and water phase compares for 1-1.5:1, it is stripped using 3-4 stage countercurrents, mixed phase time 10-15min makes the Asia in organic phase
Iron ion reenters in water phase, and organic phase is regenerated, and organic circulation uses after back extraction, and the strip liquor of gained is qualified
Solution of ferrous chloride.
2. according to a kind of abstraction impurity removal method to industrial scum sulphuric leachate described in claim 1, it is characterised in that：
Contain extractant P described in step 2507Organic phase be made of extractant and diluent, wherein extractant accounts for described organic
The 25%-30% of phase volume, diluent account for the 70%- 75% of organic phase volume.
3. according to a kind of abstraction impurity removal method to industrial scum sulphuric leachate described in claim 2, it is characterised in that：
The diluent is solvent naphtha or sulfonated kerosene.
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| CN109022822A (en) * | 2018-07-06 | 2018-12-18 | 金川集团股份有限公司 | A kind of method of nickel, cadmium impurity in processing cobalt sulfate solution |
| CN109279667A (en) * | 2018-10-09 | 2019-01-29 | 金川集团股份有限公司 | A method of LITHIUM BATTERY nickel sulfate is produced by raw material of nickel oxide |
| CN111349786A (en) * | 2018-12-24 | 2020-06-30 | 格林美（江苏）钴业股份有限公司 | Method for recovering slag washing liquid in cobalt electrodeposition process |
| CN109777954B (en) * | 2019-03-13 | 2021-01-05 | 荆门市格林美新材料有限公司 | Method for extracting ions in mineral liquid |
| CN110066080B (en) * | 2019-04-03 | 2022-04-15 | 广东兴发环境科技有限公司 | Sludge recycling process in aluminum profile processing |
| CN110092423B (en) * | 2019-04-23 | 2021-06-29 | 金川集团股份有限公司 | Method for producing nickel sulfate solution by quickly dissolving nickel oxide and deacidifying and removing impurities with nickel soap |
| CN110669932B (en) * | 2019-09-25 | 2021-04-20 | 中南大学 | Method for comprehensively utilizing copper electrolyte purification resources |
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