CN102502890A - Synthesis method of reagent nickel thiocarbonate for deeply removing copper from nickel solution - Google Patents

Synthesis method of reagent nickel thiocarbonate for deeply removing copper from nickel solution Download PDF

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CN102502890A
CN102502890A CN2011103152074A CN201110315207A CN102502890A CN 102502890 A CN102502890 A CN 102502890A CN 2011103152074 A CN2011103152074 A CN 2011103152074A CN 201110315207 A CN201110315207 A CN 201110315207A CN 102502890 A CN102502890 A CN 102502890A
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solution
nickel
copper
thio
reaction
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赵中伟
陈星宇
陈爱良
何利华
孙培梅
李洪桂
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Central South University
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Central South University
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Abstract

The invention discloses a synthesis method of reagent nickel thiocarbonate for deeply removing copper from a nickel solution. The technical scheme is as follows: soluble sulfide CS2 and sulfur (S) are used as raw materials to firstly synthesize a thiocarbonate solution, and the thiocarbonate solution reacts with a nickel-containing solution to generate nickel thiocarbonate. The nickel thiocarbonate can efficiently removing copper from nickel electrolysis anolyte, so that the copper concentration is lower than 3 mg/L, and the ratio of copper to nickel in the copper removal slag is higher than 15:1.

Description

A kind of from nickel solution the compound method of the reagent thiocarbonic acid SOH nickel of degree of depth copper removal
Technical field
The present invention relates to copper nickel hydrometallurgy field, especially for the reagent compound method of degree of depth copper removal from copper nickel mixing solutions.
Background technology
In the copper-nickel process,, it is carried out the degree of depth separate very difficulty because the chemical property of copper nickel is quite similar.Although SX can more effectively separate copper nickel with IX, only be applicable to and handle short run solution, can't carry out large-scale industrial production.Discover that copper nickel all has certain thiophilicity, but Comparatively speaking copper then has more close sulphur.The copper nickel stripping technique of exploitation mostly is based on this characteristic at present, as separation agent, reaches the optionally purpose of high efficiency separation copper from mixing solutions with various sulfide.But most sulfide is not that sulphur very easily discharges and be prone to produce toxic gas and cause producing and be difficult to carry out, and is exactly too stablely to be difficult for discharging sulfonium ion and to cause the copper removal weak effect.The investigator continually develops the Tong Shiji that removes that is applicable to from solution containing nickel copper removal that makes new advances for this reason, this wherein " active nickel sulfide " the most effective.Active nickel sulfide is to utilize the higher characteristics of reactive behavior of instability, sulphur of freshly prepd deposition chemical structure, and copper is removed.But the synthesis condition of active nickel sulfide is too harsh, and the active utmost point is hard to keep, thereby causes it can not be applied to industrial production.Also the someone utilizes other sulfocompound to carry out copper removal in addition, but all can't satisfy the copper removal production requirement fully.
For a long time, degree of depth copper removal is perplexing domestic and international metallurgical boundary always from solution containing nickel.To this difficult problem, China classifies this research as key research projects twice in " eight or five " and the ninth five-year plan, and has once attempted the whole bag of tricks, is not well solved always.This mainly is not remove Tong Shiji efficiently because find always.Solve in view of problem difficulty is big, difficult; Jinchuan company face was once more when the science and technology bid was carried out in the whole nation in 2004; The 2mg/L that copper content in the solution behind the copper removal is required during by tackling of key scientific and technical problems then is loosened to 3mg/L, removes that copper nickel mass ratio then is reduced to 15 by 20 in the copper ashes.
And want copper removal from solution containing nickel efficiently, key to be the synthesizing efficient decoppering agent.So the efficient decoppering agent that the urgent need exploitation makes new advances is to be adapted to suitability for industrialized production.The thought of the reactive behavior of sulphur has important value in " active nickel sulfide " method regulatory molecule structure.
Active nickel sulfide is formed very simple, has only two kinds of atoms of nickel and sulphur.No matter crystal formation how, the atomic properties of nickel and sulphur atom has determined that regulatable scope is little.If can carry out the chemical constitution transformation to it, through introducing new structure the sulfonium ion in the structure is modified or replaced, just can enlarge active setting range, might obtain efficiently removing Tong Shiji.In order to make the synthetic decoppering agent have efficient copper removal effect, it should have following characteristics:
Therefore based on following some design new remove Tong Shiji:
(1) meliority of sulfocompound separating copper, newly-designed negatively charged ion should contain elementary sulfur, and this elementary sulfur can be under proper working conditions with solution in impurity copper form firm Chemical bond and copper removed.
(2) do not introduce harmful ion in the use, so decoppering agent should be a nickel salt.
(3) the new negatively charged ion in the decoppering agent should have bigger ionic radius with the coulomb interaction power between minimizing and nickel ion, increases zwitterion effect steric hindrance.And negatively charged ion itself can be removed with the copper mortise, the solution noresidue; Perhaps anionic nature is unstable, and decomposition generates the sulfide of copper but also do not introduce harmful ion in the copper removal process.
Based on such consideration, we design, and to have synthesized thiocarbonic acid SOH nickel be decoppering agent, can be efficiently from the single nickel salt anolyte from copper removal, satisfy production requirement.
Summary of the invention
The purpose of this invention is to provide a kind of new being used for from the compound method of the reagent thiocarbonic acid SOH nickel of nickel solution degree of depth copper removal.
A kind of from nickel solution the compound method of the reagent thiocarbonic acid SOH nickel of degree of depth copper removal, one or more in the thio-carbonate solution that any one mode of (1)-(6) prepares below adopting continue and the synthetic thiocarbonic acid SOH nickel of solution containing nickel reaction again;
(1) with dissolvable sulfide solution and CS 2Fully reacted 5～24 hours by stoichiometry, obtaining negatively charged ion is CS 3 2-Thio-carbonate solution;
(2) solution that mode (1) is obtained continues and CS 2Reacted 5～24 hours, obtaining negatively charged ion after the reaction is C nS 2n+1 2-With CS 3 2-Mixture, perhaps C nS 2n+1 2-Thio-carbonate solution, wherein n is>=2 integer;
(3) solution that mode (1) is obtained continues and sulphur thorough mixing stirring reaction 10～24 hours, and obtaining negatively charged ion after the reaction is CS 3+y 2-With CS 3 2-Mixture, perhaps CS 3+y 2-Thio-carbonate solution, wherein y is>=1 integer;
(4) only contain C with what mode (2) obtained nS 2n+1 2-Solution continue and sulphur thorough mixing stirring reaction 10～24 hours, obtaining negatively charged ion after reacting completely is C nS M+2n+1 2-Thio-carbonate solution, wherein m is>=1, n is>=2 integer;
(5) with solubility polysulfide solution and CS 2Fully reacted 5～24 hours by stoichiometry, obtaining negatively charged ion is CS 2+x 2-Thio-carbonate solution, wherein x is>=2 integer;
(6) solution that mode (5) is obtained continues and CS 2Reacted 5～24 hours, obtaining negatively charged ion after reacting completely is C nS 2n+x 2-Thio-carbonate solution, n wherein, x is>=2 integer;
Described dissolvable sulfide comprises sulfide Na 2S, K 2Among the S one or both, the solubility polysulfide comprises Na 2S x, K 2S xIn one or both, x is>=2 integer.
PH value with solution containing nickel is adjusted to 3.0～7.0 earlier; Mol ratio by nickel in thio-carbonate and the solution is that 0.5～1.0 adding thio-carbonate solution reaction generates thiocarbonic acid SOH nickel deposition then, and continues stirring reaction 10～30 minutes.
Described solution containing nickel is NiSO 4, NiCl 2, Ni (NO 3) 2The mixture of one or more in the solution also can be a nickle electrolysis anode solution.
The synthetic key of thiocarbonic acid SOH nickel is the synthetic of thiocarbonate.The synthetic effect of thiocarbonate is directly determining the copper removal effect of thiocarbonic acid SOH nickel.Dissolvable sulfide solution ability and CS 2Reaction generates corresponding thiocarbonate, and thiocarbonate can continue and CS 2Reaction generates the polymerization thiocarbonate.For decoppering agent can provide more can with copper bonded sulphur, utilize polysulfide and CS 2Reaction perhaps makes (polymerization) thiocarbonate and sulphur further react and generates corresponding polythio carbonate.These ready-formed thiocarbonates generate thiocarbonic acid SOH nickel with the solution containing nickel reaction again, are used for efficient copper removal.According to practical situation, the thiocarbonic acid SOH nickel that can synthesize various polymerization and degree of thioation carries out copper removal.
The synthetic ultimate principle of thiocarbonic acid SOH nickel is:
Use dissolvable sulfide Me 2S and CS 2During mixing, following reaction takes place in the solution:
S 2-+CS 2＝CS 3 2-
Work as CS 3 2-Continue and CS 2During contact, following reaction can take place:
CS 3 2-+ (n-1) CS 2=C nS 2n+1 2-(n is>=2 integer)
When the synthetic more high-sulfur of needs during for the decoppering agent of degree, following reaction capable of using:
CS 3 2-+ yS=CS 3+y 2-(y is>=1 integer)
C nS 2n+1 2-+ mS=C nS M+2n+1 2-(m is>=1, and n is>=2 integer)
With solubility polysulfide Me 2S xWith CS 2During mixing, following reaction takes place in the solution:
S x 2-+ CS 2=CS 2+x 2-(x is>=2 integer)
Work as CS 2+x 2-Continue and CS 2During contact, following reaction can take place:
CS 2+x 2-+ (n-1) CS 2=C nS 2n+x 2-(n is>=2, and x is>=2 integer)
More than obtain the reaction of thiocarbonate and solution containing nickel and just obtain thiocarbonic acid SOH nickel.
Synthetic thiocarbonic acid SOH nickel and solution containing nickel reaction carrying out copper removal:
Earlier solution containing nickel pH value is adjusted to 2.5～6.5; Mol ratio by copper in thio-carbonate and the solution is 1.0～1.5 adding thiocarbonic acid SOH nickel hybrid reactions then; Control reaction temperature is 25～90 ℃, and the reaction times is 5～120 minutes.
Innovative point of the present invention has been to provide a kind of new efficient decoppering agent---preparation method of thiocarbonic acid SOH nickel, so far, has no the relevant report about the preparation method of thiocarbonic acid SOH nickel.
The thiocarbonic acid SOH nickel that the inventive method prepares can be reduced to the copper concentration in the nickle electrolysis anode solution below the 3mg/L, except that copper nickel ratio in the copper ashes is higher than 15, makes copper ashes directly get into the copper production system as copper ore concentrates.Adopt this decoppering agent to carry out copper removal and can simplify technical process greatly and reduce cost, be applicable to large-scale copper removal industrial production.Synthetic and the copper removal process of thiocarbonic acid SOH nickel is easy to operate and control in addition.
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
Na with 78Kg 2S is dissolved in earlier in the 1000L water, adds the CS of 60L again 2Solution after reaction is carried out 10 hours, obtains Na 2CS 3Solution; Again with 1.2m 3Nickeliferous 59g/L, pH are 4.0 nickel sulfate solution mixing, after reaction is carried out 20 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 128m 3The nickel sulfate solution of cupric 0.5g/L reacts after 30 minutes copper concentration and reduces to 0.0025g/L, removes that copper nickel ratio is 20.5 in the copper ashes.
Embodiment 2
Na with 78Kg 2S is dissolved in earlier in the 1000L water, adds the CS of 120L again 2Solution after reaction is carried out 24 hours, obtains Na 2C 2S 5Solution; Again with 2.0m 3Nickeliferous 62g/L, pH are 6.0 nickel chloride solution mixing, after reaction is carried out 10 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 128m 3The nickel sulfate solution of cupric 0.5g/L reacts after 5 minutes copper concentration and reduces to 0.002g/L, removes that copper nickel ratio is 18.6 in the copper ashes.
Embodiment 3
K with 142Kg 2S 2Be dissolved in earlier in the 1000L water, add the CS of 65L again 2Solution after reaction is carried out 20 hours, obtains K 2CS 4With K 2C 2S 6Mixing solutions; Again with 1.8m 3Nickeliferous 60g/L, pH are 5.2 nickel nitrate solution mixing, after reaction is carried out 30 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 128m 3The nickel sulfate solution of cupric 0.5g/L reacts after 120 minutes copper concentration and reduces to 0.0018g/L, removes that copper nickel ratio is 20.4 in the copper ashes.
Embodiment 4
Na with 39Kg 2S is dissolved in earlier in the 500L water, adds the CS of 30L again 2Solution after reaction is carried out 15 hours, obtains Na 2CS 3Solution; With 16Kg sulphur stirring reaction 24 hours, obtain Na again 2CS 4Solution; Again with 1.0m 3Nickeliferous 62g/L, pH are 7.0 nickel sulfate solution mixing, after reaction is carried out 25 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 64m 3The nickel sulfate solution of cupric 0.5g/L reacts after 60 minutes copper concentration and reduces to 0.0023g/L, removes that copper nickel ratio is 25.1 in the copper ashes.
Embodiment 5
Na with 55Kg 2S 2Be dissolved in earlier in the 500L water, add the CS of 30L again 2Solution after reaction is carried out 24 hours, obtains Na 2CS 4Solution; Again with 0.5m 3Nickeliferous 60g/L, pH are 6.5 nickel sulfate solution mixing, after reaction is carried out 10 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 64m 3The nickel sulfate solution of cupric 0.5g/L reacts after 20 minutes copper concentration and reduces to 0.0019g/L, removes that copper nickel ratio is 22.4 in the copper ashes.
Embodiment 6
K with 88Kg 2S is dissolved in earlier in the 800L water, adds the CS of 55L again 2Solution after reaction is carried out 20 hours, obtains K 2CS 3And K 2C 2S 5Mixing solutions; Again with 0.85m 3Nickeliferous 62g/L, pH are 5.1 nickel chloride solution mixing, after reaction is carried out 10 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 102.4m 3The nickel sulfate solution of cupric 0.5g/L reacts after 15 minutes copper concentration and reduces to 0.0026g/L, removes that copper nickel ratio is 27.2 in the copper ashes.
Embodiment 7
Na with 46.8Kg 2S is dissolved in earlier in the 600L water, adds the CS of 48L again 2Solution after reaction is carried out 24 hours, obtains Na 2CS 3Solution; With 10g sulphur stirring reaction 5 hours, obtain Na again 2CS 3And Na 2CS 4Mixing solutions; Again with 0.9m 3Nickeliferous 55g/L, pH are 3.0 nickle electrolysis anode solution mixing, after reaction is carried out 18 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 76.8m 3The nickel sulfate solution of cupric 0.5g/L reacts after 22 minutes copper concentration and reduces to 0.0022g/L, removes that copper nickel ratio is 31.3 in the copper ashes.
Embodiment 8
K with 33Kg 2S is dissolved in earlier in the 300L water, adds the CS of 54L again 2Solution after reaction is carried out 20 hours, obtains K 2C 3S 7Solution; Again with 0.5m 3Nickeliferous 58g/L, pH are 4.5 nickel chloride solution mixing, after reaction is carried out 15 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 38.4m 3The nickel sulfate solution of cupric 0.5g/L reacts after 18 minutes copper concentration and reduces to 0.0012g/L, removes that copper nickel ratio is 19.5 in the copper ashes.
Embodiment 9
Na with 54.6Kg 2S is dissolved in earlier in the 700L water, adds the CS of 84L again 2Solution after reaction is carried out 23 hours, obtains Na 2C 2S 5Solution; With 22.4g sulphur stirring reaction 20 hours, obtain Na again 2C 2S 6Solution; Again with 0.75m 3Nickeliferous 62g/L, pH are 4.3 nickel nitrate solution mixing, after reaction is carried out 10 minutes, filter and obtain thiocarbonic acid SOH nickel deposition; To prepare thiocarbonic acid SOH nickel precipitation process 89.6m 3The nickel sulfate solution of cupric 0.5g/L reacts after 30 minutes copper concentration and reduces to 0.0015g/L, removes that copper nickel ratio is 18.8 in the copper ashes.

Claims (3)

1. the compound method of the reagent thiocarbonic acid SOH nickel of a degree of depth copper removal from nickel solution; It is characterized in that: one or more in the thio-carbonate solution that any one mode of (1)-(6) prepares below adopting, continue and the synthetic thiocarbonic acid SOH nickel of solution containing nickel reaction again;
(1) with dissolvable sulfide solution and CS 2Fully reacted 5～24 hours by stoichiometry, obtaining negatively charged ion is CS 3 2-Thio-carbonate solution;
(2) solution that mode (1) is obtained continues and CS 2Reacted 5～24 hours, obtaining negatively charged ion after the reaction is C nS 2n+1 2-With CS 3 2-Mixture, perhaps C nS 2n+1 2-Thio-carbonate solution, wherein n is>=2 integer;
(3) solution that mode (1) is obtained continues and sulphur thorough mixing stirring reaction 10～24 hours, and obtaining negatively charged ion after the reaction is CS 3+y 2-With CS 3 2-Mixture, perhaps CS 3+y 2-Thio-carbonate solution, wherein y is>=1 integer;
(4) only contain C with what mode (2) obtained nS 2n+1 2-Solution continue and sulphur thorough mixing stirring reaction 10～24 hours, obtaining negatively charged ion after reacting completely is C nS M+2n+1 2-Thio-carbonate solution, wherein m is>=1, n is>=2 integer;
(5) with solubility polysulfide solution and CS 2Fully reacted 5～24 hours by stoichiometry, obtaining negatively charged ion is CS 2+x 2-Thio-carbonate solution, wherein x is>=2 integer;
(6) solution that mode (5) is obtained continues and CS 2Reacted 5～24 hours, obtaining negatively charged ion after reacting completely is C nS 2n+x 2-Thio-carbonate solution, n wherein, x is>=2 integer;
Described dissolvable sulfide comprises sulfide Na 2S, K 2Among the S one or both, the solubility polysulfide comprises Na 2S x, K 2S xIn one or both, x is>=2 integer.
2. according to the compound method described in the claim 1, it is characterized in that: the pH value with solution containing nickel is adjusted to 3.0～7.0 earlier; Mol ratio by nickel in thio-carbonate and the solution is that 0.5～1.0 adding thio-carbonate solution reaction generates thiocarbonic acid SOH nickel deposition then, and continues stirring reaction 10～30 minutes.
3. according to the compound method described in the claim 1, it is characterized in that: described solution containing nickel is NiSO 4, NiCl 2, Ni (NO 3) 2The mixture of one or more in the solution, or nickle electrolysis anode solution.
CN2011103152074A 2011-10-17 2011-10-17 Synthesis method of reagent nickel thiocarbonate for deeply removing copper from nickel solution Pending CN102502890A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102719671A (en) * 2012-07-06 2012-10-10 中南大学 Method and device for deeply removing copper of nickel thiocarbonate from nickel-containing solution
CN102864307A (en) * 2012-09-20 2013-01-09 中南大学 Deep decoppering method by nickel thiocarbonate/nickel-containing solution two-section reflux reaction

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102719671A (en) * 2012-07-06 2012-10-10 中南大学 Method and device for deeply removing copper of nickel thiocarbonate from nickel-containing solution
CN102719671B (en) * 2012-07-06 2015-02-04 中南大学 Method and device for deeply removing copper of nickel thiocarbonate from nickel-containing solution
CN102864307A (en) * 2012-09-20 2013-01-09 中南大学 Deep decoppering method by nickel thiocarbonate/nickel-containing solution two-section reflux reaction

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Application publication date: 20120620