CN104313319B - Method for reducing nickel content of hydrochloric acid leached slag of nickel cobalt hydroxide - Google Patents
Method for reducing nickel content of hydrochloric acid leached slag of nickel cobalt hydroxide Download PDFInfo
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- CN104313319B CN104313319B CN201410551552.1A CN201410551552A CN104313319B CN 104313319 B CN104313319 B CN 104313319B CN 201410551552 A CN201410551552 A CN 201410551552A CN 104313319 B CN104313319 B CN 104313319B
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 110
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 56
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 title claims abstract description 43
- 239000002893 slag Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 143
- 238000002386 leaching Methods 0.000 claims abstract description 95
- 238000003825 pressing Methods 0.000 claims abstract description 51
- 238000005406 washing Methods 0.000 claims abstract description 49
- XTOOSYPCCZOKMC-UHFFFAOYSA-L [OH-].[OH-].[Co].[Ni++] Chemical compound [OH-].[OH-].[Co].[Ni++] XTOOSYPCCZOKMC-UHFFFAOYSA-L 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims description 66
- 238000007654 immersion Methods 0.000 claims description 53
- 238000005259 measurement Methods 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000006396 nitration reaction Methods 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- -1 hydrogen cobalt nickel oxide Chemical class 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000004537 pulping Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000460 chlorine Substances 0.000 abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 abstract description 6
- 239000002002 slurry Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 53
- 229910017052 cobalt Inorganic materials 0.000 description 7
- 239000010941 cobalt Substances 0.000 description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 7
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- KSHLPUIIJIOBOQ-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[Co++].[Ni++] Chemical compound [O--].[O--].[O--].[O--].[Co++].[Ni++] KSHLPUIIJIOBOQ-UHFFFAOYSA-N 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for reducing nickel content of hydrochloric acid leached slag of cobalt nickel hydroxide. The method comprises the following steps: leaching hydrochloric acid and nickel cobalt hydroxide at a first stage, thereby obtaining first leached slag; serially connecting a first kettle, a second kettle and a third kettle in a second leaching stage, adding hydrochloric acid and nickel cobalt hydroxide into the first kettle and the second kettle, flowing solutions in the first kettle and the second kettle into the third kettle, stirring, and filter-pressing, thereby obtaining secondary leached slag and a secondary leached liquid, wherein the H<+> concentration in the first kettle and the second kettle is 0.1-0.8mol/L, and the H<+> concentration in the third kettle is 0.1-0.8mol/L; feeding first leached slag into a second-stage leaching procedure, washing the secondary leached slag with hydrochloric acid, filter-pressing to obtain an after-washing liquid and washed secondary leached slag, and delivering the washed secondary leached slag to a slag field; and feeding the secondary leached liquid and the after-washing liquid into the first stage to be leached. According to the method, the nickel content and the chlorine overflowing of the leached slag are reduced by controlling the pH value or the H<+> concentration of the slurry in two-leaching reaction and the pH values or the H<+> concentration of the secondary leached liquid and the first leached liquid at the final reaction point. The slag rate is less than 6%, and the nickel content of the slag is less than 3%.
Description
Technical field
The invention belongs to electroplating technology field, a kind of method being related to reduce slag nickel content in hydrometallurgy, particularly to
A kind of method of the thick nickel hydroxide cobalt raw material salt acid leaching slag nickel content reducing lateritic nickel ore output.
Background technology
With the development of electroplating industry, promoted the development of nickel salt industry, and the hydroxide nickel cobalt of lateritic nickel ore output by
In wide material sources, low price, it has been increasingly becoming the first-selected raw material of nickel salt manufacturer, in nickel hydroxide cobalt raw material salt acidleach
During going out, chemically angle sees generation neutralization reaction, controls the addition of hydrochloric acid and the ph value of solution can effectively reduce leaching
The nickel content slagged tap, but only account for 40%～50% with the nickel content in the nickel hydroxide of lateritic nickel ore output, and cobalt, calcium, magnesium, manganese etc.
Impurity content is higher, and mn element is to be existed with high-valence state form, if acid concentration therefore in leaching process in the feed
It is improper to control, and high-valence state mn element can occur redox reaction to produce substantial amounts of chlorine with hydrochloric acid, has a strong impact on working environment,
The utilization rate of hydrochloric acid can be reduced simultaneously, increase production cost.If reducing concentration of slurry in leaching process can lead to part hydroxide
Reaction do not participated in by nickel cobalt raw material, presented in leached mud, reduces metal yield, improves production cost.
Content of the invention
It is an object of the invention to provide a kind of method reducing nickel hydroxide cobalt salt acid leaching slag nickel content, leaching can be reduced
The nickel content slagged tap, also can suppress the spilling of chlorine in leaching process.
For achieving the above object, the technical solution adopted in the present invention is: a kind of reduction nickel hydroxide cobalt salt acid leaching slag
The method of nickel content is it is characterised in that specifically sequentially include the following steps:
Step 1: add hydrochloric acid and hydroxide nickel cobalt in one section of leaching kettle, when the ph value of solution in one section of leaching kettle is
When 3.5～4.0, stop charging, heating, control the temperature of solution in one section of leaching kettle to be 60～90 DEG C, react 1～1.5 hour
Afterwards, measure the ph value of liquid in one section of leaching kettle: if the ph value of this liquid is 3.5～4.0, filter pressing, obtain an immersion and phase analysis；
If the ph value of this liquid, beyond 3.5～4.0 scope, according to the ph value of actual measurement, adds hydroxide nickel cobalt or salt
Acid is adjusted, and the ph value making liquid in one section of leaching kettle is 3.5～4.0, and filter pressing obtains an immersion and phase analysis；
Meanwhile, carry out two-stage nitration leaching using a kettle of series connection, No. two kettles and No. three kettles, add into a kettle and No. two kettles
Enter hydrochloric acid and hydroxide nickel cobalt, control h in this two kettles+Concentration is 0.1～0.8mol/l, makes the solution in a kettle flow into two
Number kettle, the solution in No. two kettles flows into No. three kettles, is stirred, and measures h in liquid in No. three kettles in No. three kettles+Concentration:
If the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, then carry out filter pressing, obtain two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＞ 0.8mol/l, then add nickel hydroxide into a kettle and No. two kettles
Cobalt, and make the solution in a kettle and No. two kettles flow into No. three kettles, adjust the h in liquid in No. three kettles+Concentration be 0.1～
0.8mol/l, filter pressing, obtain two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＜ 0.1mol/l, then add hydrochloric acid into No. one and No. two kettles, and make one
Solution in number kettle and No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, pressure
Filter, obtains two phase analysis and two immersion；
Step 2: the phase analysis in hydroxide nickel cobalt, hydrochloric acid and step 1 are sent into a kettle and No. two kettles that two-stage nitration leaches
Interior, control h in this two kettles+Concentration is 0.1～0.8mol/l, makes the solution in a kettle flow into No. two kettles by overflow pipe,
Solution in No. two kettles flows into No. three kettles again, is stirred in No. three kettles, and measures the acidity of liquid in No. three kettles, i.e. this liquid
Middle h+Concentration:
If the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, then carry out filter pressing, obtain two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＞ 0.8mol/l, then add nickel hydroxide into a kettle and No. two kettles
Cobalt, and make the solution in a kettle and No. two kettles flow into No. three kettles, adjust the h in liquid in No. three kettles+Concentration, until No. three kettles
H in interior liquid+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＜ 0.1mol/l, then add hydrochloric acid into No. one and No. two kettles, and make one
Solution in number kettle and No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until in liquid in No. three kettles
H+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
With hydrochloric acid pulping and washing two phase analysis, liquid-solid ratio during washing is 3～4 1, and temperature is 70 DEG C～90 DEG C, the response time
2～3 hours；The h of cleaning mixture in washing process+Concentration is 0.1～0.8mol/l；Filter pressing, liquid and two leachings after washing after obtaining washing
Slag, pays slag field outside two phase analysis after washing；
Step 4: liquid after the washing in two immersion in step 1, two immersion in step 2 and step 3 sends into one section
In leaching kettle, dissolved hydrogen cobalt nickel oxide, when the ph value of solution in one section of leaching kettle is for 3.5～4.0, stops charging, open steam
Heating, controls the temperature of solution in one section of leaching kettle to be 60～90 DEG C, after reacting 1～1.5 hour, liquid in one section of leaching kettle of measurement
The ph value of body: if the ph value of this liquid is 3.5～4.0, opens filter pressing pump and carry out filter pressing, obtain an immersion and phase analysis；If this liquid
The ph value of body beyond 3.5～4.0 scope, then according to the actual ph value measuring, is added hydroxide nickel cobalt or hydrochloric acid is carried out
Adjust it is ensured that the ph value reacting liquid in rear one section of leaching kettle is 3.5～4.0, then carry out filter pressing, obtain an immersion and a leaching
Slag；
Step 5: repeat step 2, step 3 and step 4, hydroxide nickel cobalt is processed.
The inventive method is passed through to control the ph value of serosity or h in two leaching course of reaction kettles+Concentration, controls reaction end simultaneously
Two immersion, the ph value of an immersion or h+Concentration is reducing the spilling of leached mud nickel content and chlorine.In leaching process, slag rate is 6%
Hereinafter, slag nickel content is less than 3%；Site work environment can be effectively improved, improve metal yield, reduce production cost.
Brief description
Fig. 1 is the process chart of the inventive method.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Nickel content in lateritic nickel ore for the hydroxide nickel cobalt of raw material output only accounts for 40%～50%, and cobalt, calcium, magnesium, manganese
Higher Deng impurity content, as shown in table 1；And mn element is to be existed with high-valence state form in the feed, is therefore leaching
If acid concentration control is improper in journey, high-valence state mn element can occur redox reaction to produce substantial amounts of chlorine with hydrochloric acid, seriously
Impact working environment, can reduce the utilization rate of hydrochloric acid simultaneously, increase production cost.If reducing concentration of slurry in leaching process can lead
Cause part nickel hydroxide cobalt raw material not participate in reaction, presented in leached mud, reduce metal yield, improve and produce into
This.
The composition (/ %) of the thick hydroxide nickel cobalt of table 1
In order to overcome problem present in existing process, the invention provides a kind of technological process reduction as shown in Figure 1
The method of nickel hydroxide cobalt salt acid leaching slag nickel content, specifically sequentially includes the following steps:
Step 1: it is slowly added to hydroxide nickel cobalt while injecting hydrochloric acid in one section of leaching kettle, dissolved hydrogen cobalt nickel oxide,
When the ph value of solution in one section of leaching kettle is for 3.5～4.0, stop charging, open steam heating, control solution in one section of leaching kettle
Temperature be 60～90 DEG C, reaction 1～1.5 hour after, measurement one section of leaching kettle in liquid ph value: if the ph value of this liquid is
3.5～4.0, open filter pressing pump and carry out filter pressing, obtain an immersion and phase analysis；If the ph value of this liquid is beyond 3.5～4.0 model
Enclose, then the ph value according to actual measurement, add hydroxide nickel cobalt or hydrochloric acid is adjusted it is ensured that reacting in rear one section of leaching kettle
The ph value of liquid is 3.5～4.0, then carries out filter pressing, obtains an immersion and phase analysis；
Meanwhile, carry out two-stage nitration leaching using a kettle of series connection, No. two kettles and No. three kettles, note into a kettle and No. two kettles
Enter to be slowly added to hydroxide nickel cobalt while hydrochloric acid, control h in this two kettles+Concentration is 0.1～0.8mol/l, by adding hydrogen
The h of liquid in cobalt nickel oxide and a hydrochloric acid number kettle of regulation and No. two kettles+Concentration is 0.1～0.8mol/l, makes molten in a kettle
Liquid flows into No. two kettles by overflow pipe, and the solution in No. two kettles flows into No. three kettles again, stirs when the liquid level of liquid in No. three kettles rises to
After mixing leaf location, open the agitator in No. three kettles, be stirred, now, the acidity of liquid in No. three kettles of measurement, that is,
H in this liquid+Concentration:
If the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, then carry out filter pressing, obtain two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＞ 0.8mol/l, then add nickel hydroxide into a kettle and No. two kettles
Cobalt, and make the solution in a kettle and No. two kettles flow into No. three kettles, adjust the h in liquid in No. three kettles+Concentration, until No. three kettles
H in interior liquid+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＜ 0.1mol/l, then add hydrochloric acid into No. one and No. two kettles, and make one
Solution in number kettle and No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until in liquid in No. three kettles
H+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
Step 2: the phase analysis in hydroxide nickel cobalt, hydrochloric acid and step 1 are sent into a kettle and No. two kettles that two-stage nitration leaches
Interior, control h in this two kettles+Concentration is 0.1～0.8mol/l, adjusts a kettle and two by adding hydroxide nickel cobalt and hydrochloric acid
The h of liquid in number kettle+Concentration is 0.1～0.8mol/l, makes the solution in a kettle flow into No. two kettles, No. two kettles by overflow pipe
Interior solution flows into No. three kettles again, after the liquid level of liquid in No. three kettles rises to paddle location, opens in No. three kettles
Agitator, be stirred, now, measurement No. three kettles in liquid acidity, i.e. h in this liquid+Concentration:
If the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, then carry out filter pressing, obtain two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＞ 0.8mol/l, then add nickel hydroxide into a kettle and No. two kettles
Cobalt, and make the solution in a kettle flow into No. two kettles, the solution in No. two kettles flows into No. three kettles, adjusts in liquid in No. three kettles
h+Concentration, until the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＜ 0.1mol/l, then add hydrochloric acid into No. one and No. two kettles, and make one
Solution in number kettle and No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until in liquid in No. three kettles
H+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
With hydrochloric acid pulping and washing two phase analysis, liquid-solid ratio during washing is 3～4 1, and temperature is 70 DEG C～90 DEG C, the response time
2～3 hours；Washing process controls plus the quantity of slag or hydrochloric acid amount it is ensured that the h of cleaning mixture+Concentration is 0.1～0.8mol/l；
Filter pressing, after obtaining washing, liquid and two phase analysis after washing, pay slag field outside two phase analysis after washing；
Step 4: liquid after the washing in two immersion in step 1, two immersion in step 2 and step 3 sends into one section
In leaching kettle, dissolved hydrogen cobalt nickel oxide, when the ph value of solution in one section of leaching kettle is for 3.5～4.0, stops charging, open steam
Heating, controls the temperature of solution in one section of leaching kettle to be 60～90 DEG C, after reacting 1～1.5 hour, liquid in one section of leaching kettle of measurement
The ph value of body: if the ph value of this liquid is 3.5～4.0, opens filter pressing pump and carry out filter pressing, obtain an immersion and phase analysis；If this liquid
The ph value of body beyond 3.5～4.0 scope, then according to the actual ph value measuring, is added hydroxide nickel cobalt or hydrochloric acid is carried out
Adjust it is ensured that the ph value reacting liquid in rear one section of leaching kettle is 3.5～4.0, then carry out filter pressing, obtain an immersion and a leaching
Slag；
Step 5: repeat step 2, step 3 and step 4, hydroxide nickel cobalt is processed.
The inventive method effectively reduces, by the ph value controlling leaching process, the hydroxide producing with lateritic nickel ore transition
The method of nickel cobalt salt acid leaching slag nickel content, due to being divided into two sections of leachings in leaching process, and has first wash operation, and two
H in section leaching and washing process+It is controlled to 0.8mol/l, leaching process completely, reduces leached mud nickel content.Two leached
H in journey+It is controlled to 0.1～0.8mol/l, do not have concentrated hydrochloric acid to participate in reaction it is suppressed that high-valence state mn element is occurred with hydrochloric acid
Redox reaction produces substantial amounts of chlorine.
Embodiment 1
It is slowly added to hydroxide nickel cobalt, dissolved hydrogen cobalt nickel oxide, when one section while injecting hydrochloric acid in one section of leaching kettle
When the ph value of solution is for 3.5～4.0 in leaching kettle, stop charging, open steam heating, control the temperature of solution in one section of leaching kettle
For 60 DEG C, after reacting 1.5 hours, in one section of leaching kettle of measurement, the ph of liquid is 3.8, carries out filter pressing, obtains an immersion and phase analysis；
Meanwhile, carry out two-stage nitration leaching using a kettle of series connection, No. two kettles and No. three kettles, the injection hydrochloric acid into a kettle and No. two kettles
It is slowly added hydroxide nickel cobalt, control h in a kettle and No. two kettles+Concentration is 0.1mol/l, makes the solution in a kettle
No. two kettles are flowed into by overflow pipe, the solution in No. two kettles flows into No. three kettles again, when the liquid level of liquid in No. three kettles rises to stirring
After leaf location, open the agitator in No. three kettles, be stirred, now, the acidity of liquid, this liquid in No. three kettles of measurement
H in body+Concentration be 0.1～0.8mol/l, filter pressing, obtain two phase analysis and two immersion；Hydrochloric acid, hydroxide nickel cobalt and phase analysis are sent
Enter in a kettle and No. two kettles of two-stage nitration leaching, control h in this two kettles+Concentration is 0.1～0.8mol/l, makes in a kettle
Solution flows into No. two kettles by overflow pipe, and the solution in No. two kettles flows into No. three kettles again, when the liquid level of liquid in No. three kettles rises to
After paddle location, open the agitator in No. three kettles, be stirred, now, the acidity of liquid in No. three kettles of measurement,
I.e. h in this liquid+Concentration ＞ 0.8mol/l, then into a kettle and No. two kettles add hydroxide nickel cobalt, and make a kettle and
Solution in No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until the h in liquid in No. three kettles+Concentration
For 0.1～0.8mol/l, filter pressing, obtain two phase analysis and two immersion；With hydrochloric acid pulping and washing two phase analysis, liquid-solid ratio during washing is 3
1, temperature is 70 DEG C, 3 hours response time；Control the h of cleaning mixture in washing process+Concentration is 0.1～0.8mol/l；Pressure
Filter, after obtaining washing, liquid and two phase analysis after washing, pay slag field outside two phase analysis after washing；Liquid after two immersion and washing is sent into one section of leaching
Kettle, dissolved hydrogen cobalt nickel oxide, when the ph value of solution in one section of leaching kettle is for 3.5～4.0, stop charging, open steam heating, control
In one section of leaching kettle of system, the temperature of solution is 60 DEG C, after reacting 1.5 hours, records ph value ＜ 3.5 of liquid in one section of leaching kettle,
Add hydroxide nickel cobalt to be adjusted, the ph value making this liquid is 3.5～4.0, and filter pressing obtains an immersion and phase analysis；On repeating
State process, hydroxide nickel cobalt is processed.
After testing, through washing obtain wash after two phase analysis nickel content be 2.84%, slag rate be 5.2%.
Embodiment 2
It is slowly added to hydroxide nickel cobalt, dissolved hydrogen cobalt nickel oxide, when one section while injecting hydrochloric acid in one section of leaching kettle
When the ph value of solution is for 3.5～4.0 in leaching kettle, stop charging, open steam heating, control the temperature of solution in one section of leaching kettle
For 90 DEG C, after reacting 1 hour, ph value ＜ 3.5 of liquid in one section of leaching kettle of measurement, add hydroxide nickel cobalt and be adjusted, make
In one section of leaching kettle, the ph value of liquid is 3.5～4.0, filter pressing, obtains an immersion and phase analysis；Meanwhile, using series connection a kettle,
No. two kettles and No. three kettles carry out two-stage nitration leaching, are slowly added to nickel hydroxide while injecting hydrochloric acid into a kettle and No. two kettles
Cobalt, controls h in this two kettles+Concentration is 0.1～0.8mol/l, makes the solution in a kettle flow into No. two kettles by overflow pipe,
Solution in No. two kettles flows into No. three kettles again, after the liquid level of liquid in No. three kettles rises to paddle location, opens three
Agitator in number kettle, is stirred, now, the acidity of liquid, i.e. h in this liquid in No. three kettles of measurement+Concentration be
Between 0.5mol/l, then carry out filter pressing, obtain two phase analysis and two immersion；Hydrochloric acid, hydroxide nickel cobalt and phase analysis are sent into two-stage nitration leaching
In the kettle and No. two kettles going out, control h in this two kettles+Concentration is 0.1～0.8mol/l, so that the solution in a kettle is passed through
Overflow pipe flows into No. two kettles, and the solution in No. two kettles flows into No. three kettles again, when the liquid level of liquid in No. three kettles rises to paddle institute
Behind the position at place, open the agitator in No. three kettles, be stirred, now, the acidity of liquid, i.e. this liquid in No. three kettles of measurement
Middle h+Concentration ＜ 0.1mol/l between, then add hydrochloric acid into a kettle and No. two kettles, and make in a kettle and No. two kettles
Solution flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until the h in liquid in No. three kettles+Concentration be 0.1～
0.8mol/l, carries out filter pressing, obtains two phase analysis and two immersion；With hydrochloric acid pulping and washing two phase analysis, liquid-solid ratio during washing is 41,
Temperature is 90 DEG C, 2 hours response time；Control the h of cleaning mixture in washing process+Concentration is 0.1～0.8mol/l；Filter pressing,
After must washing, liquid and two phase analysis after washing, pay slag field outside two phase analysis after washing；Liquid after two immersion and washing is sent into one section of leaching kettle
Interior, dissolved hydrogen cobalt nickel oxide, when the ph value of solution in one section of leaching kettle is for 3.5～4.0, stop charging, open steam heating, control
In one section of leaching kettle of system, the temperature of solution is 90 DEG C, and after reacting 1 hour, in one section of leaching kettle of measurement, ph value ＞ 4.0 of liquid, adds
It is 3.5～4.0 that salt adding acid is adjusted making the ph value of liquid in one section of leaching kettle, then carries out filter pressing, obtains an immersion and a leaching
Slag；Repeat said process hydroxide nickel cobalt is processed.
The nickel content recording two phase analysis after washing is 1.65%, and slag rate is 4.5%.
Embodiment 3
It is slowly added to hydroxide nickel cobalt, dissolved hydrogen cobalt nickel oxide, when one section while injecting hydrochloric acid in one section of leaching kettle
When the ph value of solution is for 3.5～4.0 in leaching kettle, stop charging, open steam heating, control the temperature of solution in one section of leaching kettle
For 75 DEG C, after reacting 1.2 hours, record ph value ＞ 4.0 of liquid in one section of leaching kettle, add hydrochloric acid and be adjusted, make one section
In leaching kettle, the ph value of liquid is 3.5～4.0, filter pressing, obtains an immersion and phase analysis；Meanwhile, using series connection a kettle, No. two
Kettle and No. three kettles carry out two-stage nitration leaching, are slowly added to hydroxide nickel cobalt, control into a kettle and No. two kettles while injecting hydrochloric acid
Make h in this two kettles+Concentration is 0.1～0.8mol/l, makes the solution in a kettle flow into No. two kettles, No. two kettles by overflow pipe
Interior solution flows into No. three kettles again, after the liquid level of liquid in No. three kettles rises to paddle location, opens in No. three kettles
Agitator, be stirred, now, measurement No. three kettles in liquid acidity, i.e. h in this liquid+Concentration ＜ 0.1mol/l, then
Add hydrochloric acid into No. one and No. two kettles, and make the solution in a kettle and No. two kettles flow into No. three kettles, adjust liquid in No. three kettles
H in body+Concentration, until the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, and filter pressing obtains two phase analysis and two immersion；
Hydrochloric acid, hydroxide nickel cobalt and phase analysis are sent in the kettle and No. two kettles that two-stage nitration leaches, notes into a kettle and No. two kettles
Enter hydrochloric acid, phase analysis and hydroxide nickel cobalt, control h in this two kettles+Concentration is 0.1～0.8mol/l, makes molten in a kettle
Liquid flows into No. two kettles by overflow pipe, and the solution in No. two kettles flows into No. three kettles again, stirs when the liquid level of liquid in No. three kettles rises to
After mixing leaf location, open the agitator in No. three kettles, be stirred, now, record the acidity of liquid in No. three kettles, that is,
H in this liquid+Concentration ＜ 0.1mol/l, then add hydrochloric acid into No. one and No. two kettles, and make in a kettle and No. two kettles
Solution flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until the h in liquid in No. three kettles+Concentration be 0.1～
0.8mol/l, filter pressing, obtain two phase analysis and two immersion；With hydrochloric acid pulping and washing two phase analysis, liquid-solid ratio during washing is 3.5 1, temperature
Spend for 80 DEG C, 2.5 hours response time；Control the h of cleaning mixture in washing process+Concentration is 0.1～0.8mol/l；Filter pressing,
After must washing, liquid and two phase analysis after washing, pay slag field outside two phase analysis after washing；Liquid after two immersion and washing is sent into one section of leaching kettle
Interior, dissolved hydrogen cobalt nickel oxide, when the ph value of solution in one section of leaching kettle is for 3.5～4.0, stop charging, open steam heating, control
In one section of leaching kettle of system, the temperature of solution is 75 DEG C, and after reacting 1.2 hours, the ph value recording liquid in one section of leaching kettle is 3.7,
Carry out filter pressing, obtain an immersion and phase analysis；Repeat said process hydroxide nickel cobalt is processed.
Recording two phase analysis nickel contents after washing is 2.13%, and slag rate is 4.75%.
Claims (2)
1. a kind of method reducing nickel hydroxide cobalt salt acid leaching slag nickel content is it is characterised in that specifically sequentially include the following steps:
Step 1: add hydrochloric acid and hydroxide nickel cobalt in one section of leaching kettle, when solution in one section of leaching kettle ph value for 3.5～
When 4.0, stopping charging, heating, control the temperature of solution in one section of leaching kettle to be 60～90 DEG C, after reacting 1～1.5 hour, survey
The ph value of liquid in one section of leaching kettle of amount: if the ph value of this liquid is 3.5～4.0, filter pressing, obtain an immersion and phase analysis；If should
The ph value of liquid beyond 3.5～4.0 scope, then according to the actual ph value measuring, is added hydroxide nickel cobalt or hydrochloric acid is entered
Row is adjusted, and the ph value making liquid in one section of leaching kettle is 3.5～4.0, and filter pressing obtains an immersion and phase analysis；
Meanwhile, carry out two-stage nitration leaching using a kettle of series connection, No. two kettles and No. three kettles, add salt into a kettle and No. two kettles
Acid and hydroxide nickel cobalt, and adjust the h of liquid in a kettle and No. two kettles by adding hydroxide nickel cobalt and hydrochloric acid+Concentration is
0.1～0.8mol/l, makes the solution in a kettle flow into No. two kettles, the solution in No. two kettles flows into No. three kettles, enters in No. three kettles
Row stirring, now, h in liquid in No. three kettles of measurement+Concentration:
If the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, then carry out filter pressing, obtain two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＞ 0.8mol/l, then add hydroxide nickel cobalt into a kettle and No. two kettles, and make
Solution in a number kettle and No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, pressure
Filter, obtains two phase analysis and two immersion；
If the h in liquid in No. three kettles+Concentration ＜ 0.1mol/l, then into No. one and No. two kettles add hydrochloric acid, and make a kettle and
Solution in No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, and filter pressing obtains two
Phase analysis and two immersion；
Step 2: the phase analysis in hydroxide nickel cobalt, hydrochloric acid and step 1 are sent in the kettle and No. two kettles that two-stage nitration leaches, control
Make h in this two kettles+Concentration is 0.1～0.8mol/l, makes the solution in a kettle flow into No. two kettles, No. two kettles by overflow pipe
Interior solution flows into No. three kettles again, is stirred in No. three kettles, and measures the acidity of liquid in No. three kettles, i.e. h in this liquid+'s
Concentration:
If the h in liquid in No. three kettles+Concentration is 0.1～0.8mol/l, then carry out filter pressing, obtain three phase analysis and three immersion；
If the h in liquid in No. three kettles+Concentration ＞ 0.8mol/l, then add hydroxide nickel cobalt into a kettle and No. two kettles, and make
Solution in a number kettle and No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until liquid in No. three kettles
In h+Concentration is 0.1～0.8mol/l, and filter pressing obtains three phase analysis and three immersion；
If the h in liquid in No. three kettles+Concentration ＜ 0.1mol/l, then into No. one and No. two kettles add hydrochloric acid, and make a kettle and
Solution in No. two kettles flows into No. three kettles, adjusts the h in liquid in No. three kettles+Concentration, until the h in liquid in No. three kettles+Concentration
For 0.1～0.8mol/l, filter pressing, obtain three phase analysis and three immersion；
Step 3: with hydrochloric acid pulping and washing two phase analysis, liquid-solid ratio during washing is 3～4 1, and temperature is 70 DEG C～90 DEG C, during reaction
Between 2～3 hours；The h of cleaning mixture in washing process+Concentration is 0.1～0.8mol/l；Filter pressing, liquid and two after washing after obtaining washing
Phase analysis, pay slag field outside two phase analysis after washing；
Step 4: liquid after the washing in two immersion in step 1, three immersion in step 2 and step 3 sends into one section of leaching
In kettle, dissolved hydrogen cobalt nickel oxide, when the ph value of solution in one section of leaching kettle is for 3.5～4.0, stop charging, open steam heating,
The temperature controlling solution in one section of leaching kettle is 60～90 DEG C, after reacting 1～1.5 hour, liquid in one section of leaching kettle of measurement
Ph value: if the ph value of this liquid is 3.5～4.0, opens filter pressing pump and carry out filter pressing, obtain an immersion and phase analysis；If this liquid
Ph value beyond 3.5～4.0 scope, then according to the actual ph value measuring, is added hydroxide nickel cobalt or hydrochloric acid is adjusted,
Guarantee that the ph value reacting liquid in rear one section of leaching kettle is 3.5～4.0, then carry out filter pressing, obtain an immersion and phase analysis；
Step 5: repeat step 2, step 3 and step 4, hydroxide nickel cobalt is processed.
2. the method reducing nickel hydroxide cobalt salt acid leaching slag nickel content according to claim 1 is it is characterised in that described
In step 1 and step 2, after the liquid level of liquid in No. three kettles rises to paddle location, open the stirring in No. three kettles
Device, is stirred.
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| CN106365212A (en) * | 2016-08-29 | 2017-02-01 | 金川集团股份有限公司 | Method for inhibiting chlorine from being generated when coarse nickel hydroxide is leached with concentrated hydrochloric acid |
| CN110468289A (en) * | 2019-09-12 | 2019-11-19 | 金川集团股份有限公司 | A kind of method that three sections of counter current acid leachings recycle after spherical shape nickel protoxide mechanical activation |
| CN110607439A (en) * | 2019-09-12 | 2019-12-24 | 金川集团股份有限公司 | Spherical nickel protoxide sectional oxidation acid leaching treatment method |
| CN111826523B (en) * | 2020-06-28 | 2022-07-15 | 广东邦普循环科技有限公司 | Method for refining nickel hydroxide cobalt |
| CN111910075A (en) * | 2020-08-12 | 2020-11-10 | 矿冶科技集团有限公司 | Method for leaching nickel and cobalt from rough nickel and cobalt hydroxide in two stages |
| CN114293028A (en) * | 2021-12-09 | 2022-04-08 | 格林美（江苏）钴业股份有限公司 | Method for washing cobalt intermediate leaching residues |
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| CN104073633A (en) * | 2014-06-12 | 2014-10-01 | 金川集团股份有限公司 | Purification method of cobalt nickel hydroxide hydrochloric acid leaching solution |
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| CN104073633A (en) * | 2014-06-12 | 2014-10-01 | 金川集团股份有限公司 | Purification method of cobalt nickel hydroxide hydrochloric acid leaching solution |
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