CN104313319A - 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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- CN104313319A CN104313319A CN201410551552.1A CN201410551552A CN104313319A CN 104313319 A CN104313319 A CN 104313319A CN 201410551552 A CN201410551552 A CN 201410551552A CN 104313319 A CN104313319 A CN 104313319A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000002893 slag Substances 0.000 title claims abstract description 104
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 40
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 29
- UUCGKVQSSPTLOY-UHFFFAOYSA-J cobalt(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Co+2].[Ni+2] UUCGKVQSSPTLOY-UHFFFAOYSA-J 0.000 title abstract 3
- 239000007788 liquid Substances 0.000 claims abstract description 194
- 238000002386 leaching Methods 0.000 claims abstract description 151
- XTOOSYPCCZOKMC-UHFFFAOYSA-L [OH-].[OH-].[Co].[Ni++] Chemical compound [OH-].[OH-].[Co].[Ni++] XTOOSYPCCZOKMC-UHFFFAOYSA-L 0.000 claims abstract description 59
- 238000005406 washing Methods 0.000 claims abstract description 55
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 238000007654 immersion Methods 0.000 claims description 53
- 238000001914 filtration Methods 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- -1 hydrogen cobalt nickel oxide Chemical class 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 6
- 238000004537 pulping Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 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 4
- 230000001276 controlling effect Effects 0.000 description 11
- 239000011572 manganese Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- 230000001105 regulatory effect Effects 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
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000005516 engineering process Methods 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
- 150000002815 nickel Chemical class 0.000 description 2
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- 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, relate to a kind of method reducing slag nickel content in hydrometallurgy, particularly a kind of method reducing the thick nickel hydroxide cobalt raw material Leaching in Hydrochloric Acid slag nickel content of red soil nickel ore output.
Background technology
Along with the development of electroplating industry, promote the development of nickel salt industry, and the nickel hydroxide cobalt of red soil nickel ore output is due to wide material sources, low price, become the starting material of nickel salt manufacturer first-selection gradually, in nickel hydroxide cobalt raw material Leaching in Hydrochloric Acid process, chemically angle sees generation neutralization reaction, the control add-on of hydrochloric acid and the pH value of solution effectively can reduce the nickel content of leached mud, but only account for 40% ~ 50% with the nickel content in the nickel hydroxide of red soil nickel ore output, and cobalt, calcium, magnesium, the foreign matter contents such as manganese are higher, and Mn element exists with high-valence state form in the feed, if therefore in leaching process, acid concentration control is improper, high-valence state Mn element can produce a large amount of chlorine with hydrochloric acid generation redox reaction, have a strong impact on Working environment, the utilization ratio of hydrochloric acid can be reduced simultaneously, increase production cost.Part nickel hydroxide cobalt raw material can be caused not participate in reaction if reduce concentration of slurry in leaching process, exist with the form of leached mud, reduce metal yield, improve production cost.
Summary of the invention
The object of this invention is to provide a kind of method reducing nickel hydroxide cobalt salt acid leaching slag nickel content, the nickel content of leached mud can be reduced, 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 method reducing nickel hydroxide cobalt salt acid leaching slag nickel content, is characterized in that, specifically carry out according to the following steps:
Step 1: add hydrochloric acid and nickel hydroxide cobalt in one section of leaching kettle, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stop reinforced, heating, the temperature controlling solution in one section of leaching kettle is 60 ~ 90 DEG C, reacts after 1 ~ 1.5 hour, measures the pH value of liquid in one section of leaching kettle: if the pH value of this liquid is 3.5 ~ 4.0, press filtration, obtains an immersion liquid and a leaching slag; If the pH value of this liquid is beyond the scope of 3.5 ~ 4.0, then according to the pH value of actual measurement, interpolation nickel hydroxide cobalt or hydrochloric acid regulate, and make the pH value of liquid in one section of leaching kettle be 3.5 ~ 4.0, press filtration, obtain an immersion liquid and a leaching slag;
Meanwhile, adopt a still of series connection, No. two stills and No. three stills to carry out two sections of leachings, in a still and No. two stills, add hydrochloric acid and nickel hydroxide cobalt, control H in these two stills
+concentration is 0.1 ~ 0.8mol/L, and make the solution in a still flow into No. two stills, the solution in No. two stills flows into No. three stills, stirs in No. three stills, and to measure in No. three stills H in liquid
+concentration:
If the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, then carry out press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration > 0.8mol/L, then add nickel hydroxide cobalt in a still and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration < 0.1mol/L, then add hydrochloric acid in No. one and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
Step 2: the leaching slag in nickel hydroxide cobalt, hydrochloric acid and step 1 is sent in two sections of stills and No. two stills leached, controls H in these two stills
+concentration is 0.1 ~ 0.8mol/L, and make the solution in a still flow into No. two stills by upflow tube, the solution in No. two stills flows into No. three stills again, stirs in No. three stills, and measures the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration:
If the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, then carry out press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration > 0.8mol/L, then add nickel hydroxide cobalt in a still and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration < 0.1mol/L, then add hydrochloric acid in No. one and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
Soak slag by hydrochloric acid pulping and washing two, liquid-solid ratio during washing is 3 ~ 4 ︰ 1, and temperature is 70 DEG C ~ 90 DEG C, 2 ~ 3 hours reaction times; The H of washings in washing process
+concentration is 0.1 ~ 0.8mol/L; Press filtration, liquid and two leaching slags after washing after must washing, after washing, two leaching slags pay slag field outward;
Step 4: by liquid after the washing in two immersion liquid in step 1, two immersion liquid in step 2 and step 3, send in one section of leaching kettle, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 60 ~ 90 DEG C, reacts after 1 ~ 1.5 hour, measures the pH value of liquid in one section of leaching kettle: if the pH value of this liquid is 3.5 ~ 4.0, open filter pressing pump and carry out press filtration, obtain an immersion liquid and a leaching slag; If the pH value of this liquid is beyond the scope of 3.5 ~ 4.0, then according to the pH value of actual measurement, interpolation nickel hydroxide cobalt or hydrochloric acid regulate, and guarantee that the pH value of reacting liquid in rear one section of leaching kettle is 3.5 ~ 4.0, then carry out press filtration, obtain an immersion liquid and a leaching slag;
Step 5: repeating step 2, step 3 and step 4, processes nickel hydroxide cobalt.
The inventive method soaks pH value or the H of slurries in reaction process still by control two
+concentration, the pH value of the immersion liquid of control reaction end two, an immersion liquid simultaneously or H
+concentration reduces the spilling of leached mud nickel content and chlorine.In leaching process, slag rate is below 6%, and slag nickel content is less than 3%; Effectively can improve site work environment, improve metal yield, reduce production cost.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Be that nickel content in the nickel hydroxide cobalt of raw material output only accounts for 40% ~ 50% with red soil nickel ore, and the foreign matter contents such as cobalt, calcium, magnesium, manganese are higher, as shown in table 1; And Mn element exists with high-valence state form in the feed, if therefore in leaching process, acid concentration control is improper, high-valence state Mn element can produce a large amount of chlorine with hydrochloric acid generation redox reaction, has a strong impact on Working environment, the utilization ratio of hydrochloric acid can be reduced simultaneously, increase production cost.Part nickel hydroxide cobalt raw material can be caused not participate in reaction if reduce concentration of slurry in leaching process, exist with the form of leached mud, reduce metal yield, improve production cost.
The composition (/ %) of the thick nickel hydroxide cobalt of table 1
In order to overcome Problems existing in existing technique, the invention provides the method for a kind of technical process reduction nickel hydroxide cobalt salt acid leaching slag nickel content as shown in Figure 1, specifically carrying out according to the following steps:
Step 1: slowly add nickel hydroxide cobalt inject hydrochloric acid in one section of leaching kettle while, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stop reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 60 ~ 90 DEG C, react after 1 ~ 1.5 hour, measure the pH value of liquid in one section of leaching kettle: if the pH value of this liquid is 3.5 ~ 4.0, open filter pressing pump and carry out press filtration, obtain an immersion liquid and a leaching slag; If the pH value of this liquid is beyond the scope of 3.5 ~ 4.0, then according to the pH value of actual measurement, interpolation nickel hydroxide cobalt or hydrochloric acid regulate, and guarantee that the pH value of reacting liquid in rear one section of leaching kettle is 3.5 ~ 4.0, then carry out press filtration, obtain an immersion liquid and a leaching slag;
Meanwhile, adopt a still of series connection, No. two stills and No. three stills to carry out two sections of leachings, slowly add nickel hydroxide cobalt inject hydrochloric acid in a still and No. two stills while, control H in these two stills
+concentration is 0.1 ~ 0.8mol/L, is regulated the H of liquid in a still and No. two stills by interpolation nickel hydroxide cobalt and hydrochloric acid
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration:
If the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, then carry out press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration > 0.8mol/L, then add nickel hydroxide cobalt in a still and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration < 0.1mol/L, then add hydrochloric acid in No. one and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
Step 2: the leaching slag in nickel hydroxide cobalt, hydrochloric acid and step 1 is sent in two sections of stills and No. two stills leached, controls H in these two stills
+concentration is 0.1 ~ 0.8mol/L, is regulated the H of liquid in a still and No. two stills by interpolation nickel hydroxide cobalt and hydrochloric acid
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration:
If the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, then carry out press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration > 0.8mol/L, then add nickel hydroxide cobalt in a still and No. two stills, and make the solution in a still flow into No. two stills, and the solution in No. two stills flows into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration < 0.1mol/L, then add hydrochloric acid in No. one and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
Soak slag by hydrochloric acid pulping and washing two, liquid-solid ratio during washing is 3 ~ 4 ︰ 1, and temperature is 70 DEG C ~ 90 DEG C, 2 ~ 3 hours reaction times; In washing process, control the amount adding the quantity of slag or hydrochloric acid, guarantee the H of washings
+concentration is 0.1 ~ 0.8mol/L; Press filtration, liquid and two leaching slags after washing after must washing, after washing, two leaching slags pay slag field outward;
Step 4: by liquid after the washing in two immersion liquid in step 1, two immersion liquid in step 2 and step 3, send in one section of leaching kettle, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 60 ~ 90 DEG C, reacts after 1 ~ 1.5 hour, measures the pH value of liquid in one section of leaching kettle: if the pH value of this liquid is 3.5 ~ 4.0, open filter pressing pump and carry out press filtration, obtain an immersion liquid and a leaching slag; If the pH value of this liquid is beyond the scope of 3.5 ~ 4.0, then according to the pH value of actual measurement, interpolation nickel hydroxide cobalt or hydrochloric acid regulate, and guarantee that the pH value of reacting liquid in rear one section of leaching kettle is 3.5 ~ 4.0, then carry out press filtration, obtain an immersion liquid and a leaching slag;
Step 5: repeating step 2, step 3 and step 4, processes nickel hydroxide cobalt.
The inventive method effectively reduces with the method for the nickel hydroxide cobalt salt acid leaching slag nickel content of red soil nickel ore production transition by the pH value controlling leaching process, owing to being divided into two sections of leachings in leaching process, and have first wash operation, and two sections are leached and H in washing process
+control as 0.8mol/L, leaching process is complete, reduces leached mud nickel content.H in two leaching process
+control is 0.1 ~ 0.8mol/L, does not have concentrated hydrochloric acid to participate in reaction, inhibits high-valence state Mn element and hydrochloric acid generation redox reaction to produce a large amount of chlorine.
embodiment 1
Nickel hydroxide cobalt is slowly added inject hydrochloric acid in one section of leaching kettle while, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stop reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 60 DEG C, react after 1.5 hours, the pH measuring liquid in one section of leaching kettle is 3.8, carries out press filtration, obtains an immersion liquid and a leaching slag; Meanwhile, adopt a still of series connection, No. two stills and No. three stills to carry out two sections of leachings, slowly add nickel hydroxide cobalt inject hydrochloric acid in a still and No. two stills while, control H in a still and No. two stills
+concentration is 0.1mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, H in this liquid
+concentration be 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid; Hydrochloric acid, nickel hydroxide cobalt and a leaching slag are sent in two sections of stills and No. two stills leached, controls H in these two stills
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration > 0.8mol/L, then in a still and No. two stills, add nickel hydroxide cobalt, and make the solution in a still and No. two stills flow into No. three stills, regulate the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid; Soak slag by hydrochloric acid pulping and washing two, liquid-solid ratio during washing is 3 ︰ 1, and temperature is 70 DEG C, 3 hours reaction times; The H of washings is controlled in washing process
+concentration is 0.1 ~ 0.8mol/L; Press filtration, liquid and two leaching slags after washing after must washing, after washing, two leaching slags pay slag field outward; Liquid after two immersion liquid and washing is sent into one section of leaching kettle, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 60 DEG C, reacts after 1.5 hours, records the pH value < 3.5 of liquid in one section of leaching kettle, add nickel hydroxide cobalt to regulate, make the pH value of this liquid be 3.5 ~ 4.0, press filtration, obtain an immersion liquid and a leaching slag; Repeat said process, nickel hydroxide cobalt is processed.
After testing, through washing obtain wash after two leaching slags nickel contents be 2.84%, slag rate is 5.2%.
embodiment 2
Nickel hydroxide cobalt is slowly added inject hydrochloric acid in one section of leaching kettle while, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 90 DEG C, reacts after 1 hour, measures the pH value < 3.5 of liquid in one section of leaching kettle, add nickel hydroxide cobalt to regulate, make the pH value of liquid in one section of leaching kettle be 3.5 ~ 4.0, press filtration, obtain an immersion liquid and a leaching slag; Meanwhile, adopt a still of series connection, No. two stills and No. three stills to carry out two sections of leachings, slowly add nickel hydroxide cobalt inject hydrochloric acid in a still and No. two stills while, control H in these two stills
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration be between 0.5mol/L, then carry out press filtration, obtain two leaching slags and two immersion liquid; Hydrochloric acid, nickel hydroxide cobalt and a leaching slag are sent in two sections of stills and No. two stills leached, controls H in these two stills
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration < 0.1mol/L between, then in a still and No. two stills, add hydrochloric acid, and make the solution in a still and No. two stills flow into No. three stills, regulate the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, carries out press filtration, obtains two leaching slags and two immersion liquid; Soak slag by hydrochloric acid pulping and washing two, liquid-solid ratio during washing is 4 ︰ 1, and temperature is 90 DEG C, 2 hours reaction times; The H of washings is controlled in washing process
+concentration is 0.1 ~ 0.8mol/L; Press filtration, liquid and two leaching slags after washing after must washing, after washing, two leaching slags pay slag field outward; Liquid after two immersion liquid and washing is sent in one section of leaching kettle, dissolved hydrogen cobalt nickel oxide, when the pH value of solution is 3.5 ~ 4.0 in one section of leaching kettle, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 90 DEG C, react after 1 hour, measure the pH value > 4.0 of liquid in one section of leaching kettle, interpolation hydrochloric acid carries out regulating makes the pH value of liquid in one section of leaching kettle be 3.5 ~ 4.0, then carry out press filtration, obtain an immersion liquid and a leaching slag; Repeat said process to process nickel hydroxide cobalt.
The nickel content recording two leaching slags after washing is 1.65%, and slag rate is 4.5%.
embodiment 3
Nickel hydroxide cobalt is slowly added inject hydrochloric acid in one section of leaching kettle while, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 75 DEG C, reacts after 1.2 hours, records the pH value > 4.0 of liquid in one section of leaching kettle, add hydrochloric acid to regulate, make the pH value of liquid in one section of leaching kettle be 3.5 ~ 4.0, press filtration, obtain an immersion liquid and a leaching slag; Meanwhile, adopt a still of series connection, No. two stills and No. three stills to carry out two sections of leachings, slowly add nickel hydroxide cobalt inject hydrochloric acid in a still and No. two stills while, control H in these two stills
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, measure the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration < 0.1mol/L, then in No. one and No. two stills, add hydrochloric acid, and make the solution in a still and No. two stills flow into No. three stills, regulate the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid; Hydrochloric acid, nickel hydroxide cobalt and a leaching slag are sent in two sections of stills and No. two stills leached, in a still and No. two stills, injects hydrochloric acid, one soak slag and nickel hydroxide cobalt, control H in these two stills
+concentration is 0.1 ~ 0.8mol/L, the solution in a still is made to flow into No. two stills by upflow tube, solution in No. two stills flows into No. three stills again, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir, now, record the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration < 0.1mol/L, then in No. one and No. two stills, add hydrochloric acid, and make the solution in a still and No. two stills flow into No. three stills, regulate the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid; Soak slag by hydrochloric acid pulping and washing two, liquid-solid ratio during washing is 3.5 ︰ 1, and temperature is 80 DEG C, 2.5 hours reaction times; The H of washings is controlled in washing process
+concentration is 0.1 ~ 0.8mol/L; Press filtration, liquid and two leaching slags after washing after must washing, after washing, two leaching slags pay slag field outward; Liquid after two immersion liquid and washing is sent in one section of leaching kettle, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stop reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 75 DEG C, react after 1.2 hours, the pH value recording liquid in one section of leaching kettle is 3.7, carries out press filtration, obtains an immersion liquid and a leaching slag; Repeat said process to process nickel hydroxide cobalt.
Recording two leaching slag nickel contents after washing is 2.13%, and slag rate is 4.75%.
Claims (3)
1. reduce a method for nickel hydroxide cobalt salt acid leaching slag nickel content, it is characterized in that, specifically carry out according to the following steps:
Step 1: add hydrochloric acid and nickel hydroxide cobalt in one section of leaching kettle, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stop reinforced, heating, the temperature controlling solution in one section of leaching kettle is 60 ~ 90 DEG C, reacts after 1 ~ 1.5 hour, measures the pH value of liquid in one section of leaching kettle: if the pH value of this liquid is 3.5 ~ 4.0, press filtration, obtains an immersion liquid and a leaching slag; If the pH value of this liquid is beyond the scope of 3.5 ~ 4.0, then according to the pH value of actual measurement, interpolation nickel hydroxide cobalt or hydrochloric acid regulate, and make the pH value of liquid in one section of leaching kettle be 3.5 ~ 4.0, press filtration, obtain an immersion liquid and a leaching slag;
Meanwhile, adopt a still of series connection, No. two stills and No. three stills to carry out two sections of leachings, in a still and No. two stills, add hydrochloric acid and nickel hydroxide cobalt, control H in these two stills
+concentration is 0.1 ~ 0.8mol/L, and make the solution in a still flow into No. two stills, the solution in No. two stills flows into No. three stills, stirs in No. three stills, and to measure in No. three stills H in liquid
+concentration:
If the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, then carry out press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration > 0.8mol/L, then add nickel hydroxide cobalt in a still and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration < 0.1mol/L, then add hydrochloric acid in No. one and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
Step 2: the leaching slag in nickel hydroxide cobalt, hydrochloric acid and step 1 is sent in two sections of stills and No. two stills leached, controls H in these two stills
+concentration is 0.1 ~ 0.8mol/L, and make the solution in a still flow into No. two stills by upflow tube, the solution in No. two stills flows into No. three stills again, stirs in No. three stills, and measures the acidity of liquid in No. three stills, i.e. H in this liquid
+concentration:
If the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, then carry out press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration > 0.8mol/L, then add nickel hydroxide cobalt in a still and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
If the H in No. three stills in liquid
+concentration < 0.1mol/L, then add hydrochloric acid in No. one and No. two stills, and make the solution in a still and No. two stills flow into No. three stills, regulates the H in liquid in No. three stills
+concentration, until the H in No. three stills in liquid
+concentration is 0.1 ~ 0.8mol/L, press filtration, obtains two leaching slags and two immersion liquid;
Soak slag by hydrochloric acid pulping and washing two, liquid-solid ratio during washing is 3 ~ 4 ︰ 1, and temperature is 70 DEG C ~ 90 DEG C, 2 ~ 3 hours reaction times; The H of washings in washing process
+concentration is 0.1 ~ 0.8mol/L; Press filtration, liquid and two leaching slags after washing after must washing, after washing, two leaching slags pay slag field outward;
Step 4: by liquid after the washing in two immersion liquid in step 1, two immersion liquid in step 2 and step 3, send in one section of leaching kettle, dissolved hydrogen cobalt nickel oxide, when in one section of leaching kettle, the pH value of solution is 3.5 ~ 4.0, stops reinforced, open steam heating, the temperature controlling solution in one section of leaching kettle is 60 ~ 90 DEG C, reacts after 1 ~ 1.5 hour, measures the pH value of liquid in one section of leaching kettle: if the pH value of this liquid is 3.5 ~ 4.0, open filter pressing pump and carry out press filtration, obtain an immersion liquid and a leaching slag; If the pH value of this liquid is beyond the scope of 3.5 ~ 4.0, then according to the pH value of actual measurement, interpolation nickel hydroxide cobalt or hydrochloric acid regulate, and guarantee that the pH value of reacting liquid in rear one section of leaching kettle is 3.5 ~ 4.0, then carry out press filtration, obtain an immersion liquid and a leaching slag;
Step 5: repeating step 2, step 3 and step 4, processes nickel hydroxide cobalt.
2. the method for reduction nickel hydroxide cobalt salt acid leaching slag nickel content according to claim 1, it is characterized in that, in described step 1 and step 2, after in No. three stills, the liquid level of liquid rises to the position residing for paddle, open the agitator in No. three stills, stir.
3. the method for reduction nickel hydroxide cobalt salt acid leaching slag nickel content according to claim 1, is characterized in that, in described step 1 and step 2, regulates the H of liquid in a still and No. two stills by adding nickel hydroxide cobalt or hydrochloric acid
+concentration is 0.1 ~ 0.8mol/L.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111826523A (en) * | 2020-06-28 | 2020-10-27 | 广东邦普循环科技有限公司 | Method for refining nickel cobalt hydroxide |
| CN112095005A (en) * | 2020-08-12 | 2020-12-18 | 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 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352119A (en) * | 2013-06-25 | 2013-10-16 | 工信华鑫科技有限公司 | Novel leaching-extracting process for wet slag of mixed nickel cobalt hydroxide |
| 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 |
-
2014
- 2014-10-17 CN CN201410551552.1A patent/CN104313319B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103352119A (en) * | 2013-06-25 | 2013-10-16 | 工信华鑫科技有限公司 | Novel leaching-extracting process for wet slag of mixed nickel cobalt hydroxide |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111826523A (en) * | 2020-06-28 | 2020-10-27 | 广东邦普循环科技有限公司 | Method for refining nickel cobalt hydroxide |
| CN112095005A (en) * | 2020-08-12 | 2020-12-18 | 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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