CN102367173A - Method for preparing copper sulphide and sodium chloride by utilizing waste residue copper sludge - Google Patents
Method for preparing copper sulphide and sodium chloride by utilizing waste residue copper sludge Download PDFInfo
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- CN102367173A CN102367173A CN2011101827681A CN201110182768A CN102367173A CN 102367173 A CN102367173 A CN 102367173A CN 2011101827681 A CN2011101827681 A CN 2011101827681A CN 201110182768 A CN201110182768 A CN 201110182768A CN 102367173 A CN102367173 A CN 102367173A
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Abstract
The invention provides a method for preparing copper sulphide and sodium chloride by utilizing waste residue copper sludge. The method comprises the following steps: acquiring the waste residue copper sludge from the production of vat grey BG; mixing industrial water with the waste residue copper sludge till forming a paste; filtering, thereby acquiring copper sulphide and a first filtrate; reacting the first filtrate with a hydrochloric acid solution, thereby acquiring a mixed solution containing the copper chloride, sodium chloride and sodium sulfate, and meanwhile, discharging hydrogen sulfide gas; filtering the mixed solution, thereby acquiring a bit of filter cake impurities and a clear filtrate; firstly distilling the clear filtrate under normal pressure, thereby evaporating organic impurities low in boiling point; and then reacting the clear filtrate with calcium chloride, thereby removing the sodium sulfate and acquiring a third filtrate; reacting the third filtrate with a hydrogen sulfide solution, thereby generating copper sulphide sediments and hydrogen chloride; filtering the products, thereby acquiring the copper sulphide and a fourth filtrate; performing reduced pressure distillation on the fourth filtrate, thereby acquiring a supersaturated solution of the sodium chloride; and separating out sodium chloride crystals, and filtering, thereby acquiring sodium phosphate and a fifth filtrate.
Description
Technical field:
The invention belongs to dyestuff organic chemical industry industry multipurpose use of three types of wastes technical field, particularly, relating to is a kind ofly to prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, and said waste residue copper sludge is for producing the Vat Grey BG gained.
Background technology
Production processes such as the reactive brilliant bule K-NR of dyestuffs industries, alkalescence purple, Vat Grey BG, methyl catechol produce copper-containing residue; Wherein contain a large amount of organic substances, inorganic salt etc.; The general calcination process that adopts; At high temperature contain copper compound in the waste residue and be oxidized to cuprously, reclaim with the copper sulfate form after reaching sulfuric acid acidation then.Oxidative decomposition at high temperature takes place in the organism in the waste residue simultaneously, generates gases such as sulfurous gas, nitrogen oxide, carbonic acid gas, hydrochloric acid, water.
Vat grey BC is to be raw material with phthalic anhydride, ammoniacal liquor, Resorcinol and midbody RK, through reaction such as condensation, ammonification, oxidation, acidylate, solid phase condensation and filter, dry, process such as spray is done and making.By how acid anhydride and ammoniacal liquor are raw material for midbody RK system, make through process such as reaction such as ammonification, hydrolysis, bob-weight nitrogen, virtueization, cyclization bromination and filtration, drying.The RK that makes supplies Vat Grey BG to produce the solid phase condensation use.The filtration procedure that midbody RK produces produces a large amount of waste residue copper sludges.
Detect the waste residue copper sludge that the above-mentioned explained hereafter Vat Grey BG of certain station-service produces, 1 ton of grey BC that redeems a vow to a god of every production produces waste residue copper sludge 989.91kg, and vat grey BC produces 300 tons per year, and then producing the waste residue copper sludge per year is 297 tons.The waste residue copper sludge component of gained is: cupric chloride 3.44%, and cupric sulfide 13.44%, sodium sulphite 3.53%, sodium-chlor 3.26%, sodium sulfate 1.67%, water are 20.4%, organic impurity 50%.
Summary of the invention
Through detecting, the component that certain factory produces the waste residue copper sludge that produces in the Vat Grey BG process per year is following: cupric chloride 3.44%, cupric sulfide 13.44%, sodium sulphite 3.53%, sodium-chlor 3.26%, sodium sulfate 1.67%, water 20.4%, organic impurity 50%.This waste residue copper sludge derives from the filter residue of the filtration procedure of midbody RK production, and 1 ton of vat grey BC of every production produces waste residue copper sludge 989.91kg.
The invention provides a kind of method for preparing cupric sulfide and sodium-chlor with the waste residue copper sludge; Said waste residue copper sludge is for producing the Vat Grey BG gained; The pollution of dye industry waste residue copper sludge is effectively administered and utilized to this method; Also produce various copper bearing compound products, created considerable economic value, have well-off social benefit and abundant economic benefit simultaneously.
In order to reach above-mentioned purpose, technical scheme of the present invention is: a kind ofly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, said waste residue copper sludge is for producing the Vat Grey BG gained; The component of said waste residue copper sludge is following: cupric chloride 3.44%, cupric sulfide 13.44%, sodium sulphite 3.53%; Sodium-chlor 3.26%, sodium sulfate 1.67%, water 20.4%; Organic impurity 50% is characterized in that, this method comprises the steps:
Step (1), weighing waste residue copper sludge with waste residue copper sludge furnishing soup compound, through filtering, obtain cupric sulfide filter cake and filtrating one with service water; The cupric sulfide filter cake is after washing, and drying obtains copper sulphide product;
The molar content of sodium sulphite in step (2), the calculating filtrating one; Ratio according to sodium sulphite and the molar weight of the pure substance of hydrogenchloride is 1: 1.6-2.4; The filtrating one of step (1) gained is dropped into corrosion resistant reactor reaction with hydrochloric acid soln; Obtain containing the mixing solutions of cupric chloride, sodium-chlor and sodium sulfate, discharge hydrogen sulfide simultaneously;
Step (3), the mixing solutions that contains cupric chloride, sodium-chlor and sodium sulfate of step (2) gained is filtered, obtain extremely a spot of filter cake impurity and clarifying filtrating;
Step (4), the first air distillation of the clarifying filtrating of step (3) gained is steamed low-boiling organic impurities, mainly contain sodium sulfate, sodium-chlor and three kinds of materials of cupric chloride in the surplus solution that obtains;
Step (5), calculate the molar content of the sodium sulfate in the surplus solution, and add calcium chloride, make sulfate ion and calcium ion be combined into calcium sulfate and precipitate, and generate sodium-chlor, after the filtration, obtain calcium sulfate precipitation and filtrate three;
Main sodium chloride-containing and copper chloride in step (6), the filtrating three, the molar content of calculating copper chloride, and according to the excessive hydrogen sulfide solution of this molar content adding; Make the reaction of copper chloride and hydrogen sulfide generate copper sulfide and hydrogen chloride; This reaction is redox reaction, and the copper sulfide precipitation of generation is insoluble to hydrochloric acid solution, thereby; Reaction can be carried out, and obtains copper sulphide product and filtrating four after filtration;
Step (7), filtrating four are the supersaturated solution of sodium-chlor through underpressure distillation, and the sodium-chlor crystallization is separated out, and filter, and obtain sodium-chlor and filtrating five, and filtrating five is mixed with the filtrating one of next round step (1) gained and reused.
The hydrogen sulfide that step (2) is discharged feeds in the alkali lye or through reclaiming and makes hydrosulphuric acid.
Buried or the burning of the filter cake impurity that step (3) obtains.
According to the inventionly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, its chemical equation is:
Na
2S+2HCl＝＝＝＝2NaCl+H
2S
CuCl
2+H
2S＝＝＝＝CuS+2HCl
Beneficial effect of the present invention is: saidly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, simple to operate, facility investment is few, has effectively administered the pollution of dye industry waste residue copper sludge, realizes turning waste into wealth, and has created considerable economic value.
Embodiment
Embodiment 1:
A kind ofly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, said waste residue copper sludge is for producing the Vat Grey BG gained, and the component of said waste residue copper sludge is following: cupric chloride 3.44%; Cupric sulfide 13.44%, sodium sulphite 3.53%, sodium-chlor 3.26%; Sodium sulfate 1.67%; Water 20.4%, organic impurity 50%, this method comprises the steps:
Step (1), weighing 500kg waste residue copper sludge with waste residue copper sludge furnishing soup compound, through filtering, obtain cupric sulfide filter cake and filtrating one with service water; The cupric sulfide filter cake is after washing, and drying obtains the 67.2kg copper sulphide product;
The molar content of sodium sulphite in step (2), the calculating filtrating one; Ratio according to sodium sulphite and the molar weight of the pure substance of hydrogenchloride is 1: 2.0; The filtrating one of step (1) gained is dropped into corrosion resistant reactor reaction with hydrochloric acid soln; Obtain containing the mixing solutions of cupric chloride, sodium-chlor and sodium sulfate, discharge hydrogen sulfide simultaneously;
Step (3), the mixing solutions that contains cupric chloride, sodium-chlor and sodium sulfate of step (2) gained is filtered, obtain extremely a spot of filter cake impurity and clarifying filtrating;
Step (4), the first air distillation of the clarifying filtrating of step (3) gained is steamed low-boiling organic impurities; Mainly contain sodium sulfate, sodium-chlor and three kinds of materials of cupric chloride in the surplus solution that obtains; Contain the about 17.2kg of cupric chloride, the about 42.78kg of sodium-chlor, the about 8.35kg of sodium sulfate;
Step (5), calculate the molar content of the sodium sulfate in the surplus solution, and add calcium chloride, make sulfate ion and calcium ion be combined into calcium sulfate and precipitate, and generate sodium-chlor, after the filtration, obtain calcium sulfate precipitation and filtrate three;
Main sodium chloride-containing and copper chloride in step (6), the filtrating three, the molar content of calculating copper chloride, and according to the excessive hydrogen sulfide solution of this molar content adding; Make the reaction of copper chloride and hydrogen sulfide generate copper sulfide and hydrogen chloride; This reaction is redox reaction, and the copper sulfide precipitation of generation is insoluble to hydrochloric acid solution, thereby; Reaction can be carried out, and obtains about 9.7kg copper sulphide product and filtrating four after filtration;
Step (7), filtrating four are the supersaturated solution of sodium-chlor through underpressure distillation, and the sodium-chlor crystallization is separated out, and filter, and obtain sodium-chlor and filtrating five, filtrating five mixes with the filtrating one of next round step (1) gained and after reuse.
Embodiment 2:
A kind ofly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, said waste residue copper sludge is for producing the Vat Grey BG gained, and the component of said waste residue copper sludge is following: cupric chloride 3.44%; Cupric sulfide 13.44%, sodium sulphite 3.53%, sodium-chlor 3.26%; Sodium sulfate 1.67%; Water 20.4%, organic impurity 50%, this method comprises the steps:
Step (1), weighing 500kg waste residue copper sludge with waste residue copper sludge furnishing soup compound, through filtering, obtain cupric sulfide filter cake and filtrating one with service water; The cupric sulfide filter cake is after washing, and drying obtains the 67.2kg copper sulphide product;
The molar content of sodium sulphite in step (2), the calculating filtrating one; Ratio according to sodium sulphite and the molar weight of the pure substance of hydrogenchloride is 1: 2.4; The filtrating one of step (1) gained is dropped into corrosion resistant reactor reaction with hydrochloric acid soln; Obtain containing the mixing solutions of cupric chloride, sodium-chlor and sodium sulfate, discharge hydrogen sulfide simultaneously;
Step (3), the mixing solutions that contains cupric chloride, sodium-chlor and sodium sulfate of step (2) gained is filtered, obtain extremely a spot of filter cake impurity and clarifying filtrating;
Step (4), the first air distillation of the clarifying filtrating of step (3) gained is steamed low-boiling organic impurities; Mainly contain sodium sulfate, sodium-chlor and three kinds of materials of cupric chloride in the surplus solution that obtains; Contain the about 17.2kg of cupric chloride, the about 42.78kg of sodium-chlor, the about 8.35kg of sodium sulfate;
Step (5), calculate the molar content of the sodium sulfate in the surplus solution, and add calcium chloride, make sulfate ion and calcium ion be combined into calcium sulfate and precipitate, and generate sodium-chlor, after the filtration, obtain calcium sulfate precipitation and filtrate three;
Main sodium chloride-containing and copper chloride in step (6), the filtrating three, the molar content of calculating copper chloride, and according to the excessive hydrogen sulfide solution of this molar content adding; Make the reaction of copper chloride and hydrogen sulfide generate copper sulfide and hydrogen chloride; This reaction is redox reaction, and the copper sulfide precipitation of generation is insoluble to hydrochloric acid solution, thereby; Reaction can be carried out, and obtains 9.7kg copper sulphide product and filtrating four after filtration;
Step (7), filtrating four are the supersaturated solution of sodium-chlor through underpressure distillation, and the sodium-chlor crystallization is separated out, and filter, and obtain sodium-chlor and filtrating five, filtrating five mixes with the filtrating one of next round step (1) gained and after reuse.
Embodiment 3
Step (1), weighing 500kg waste residue copper sludge with waste residue copper sludge furnishing soup compound, through filtering, obtain cupric sulfide filter cake and filtrating one with service water; The cupric sulfide filter cake is after washing, and drying obtains the 67.2kg copper sulphide product;
The molar content of sodium sulphite in step (2), the calculating filtrating one; Ratio according to sodium sulphite and the molar weight of the pure substance of hydrogenchloride is 1: 1.6; The filtrating one of step (1) gained is dropped into corrosion resistant reactor reaction with hydrochloric acid soln; Obtain containing the mixing solutions of cupric chloride, sodium-chlor and sodium sulfate, discharge hydrogen sulfide simultaneously;
Step (3), the mixing solutions that contains cupric chloride, sodium-chlor and sodium sulfate of step (2) gained is filtered, obtain extremely a spot of filter cake impurity and clarifying filtrating;
Step (4), the first air distillation of the clarifying filtrating of step (3) gained is steamed low-boiling organic impurities; Mainly contain sodium sulfate, sodium-chlor and three kinds of materials of cupric chloride in the surplus solution that obtains; Contain the about 17.2kg of cupric chloride in the filtrating; The about 37.5kg of sodium-chlor, the about 8.35kg of sodium sulfate;
Step (5), calculate the molar content of the sodium sulfate in the surplus solution, and add calcium chloride, make sulfate ion and calcium ion be combined into calcium sulfate and precipitate, and generate sodium-chlor, after the filtration, obtain calcium sulfate precipitation and filtrate three;
Main sodium chloride-containing and copper chloride in step (6), the filtrating three, the molar content of calculating copper chloride, and according to the excessive hydrogen sulfide solution of this molar content adding; Make the reaction of copper chloride and hydrogen sulfide generate copper sulfide and hydrogen chloride; This reaction is redox reaction, and the copper sulfide precipitation of generation is insoluble to hydrochloric acid solution, thereby; Reaction can be carried out, and obtains 9.7kg copper sulphide product and filtrating four after filtration;
Step (7), filtrating four are the supersaturated solution of sodium-chlor through underpressure distillation, and the sodium-chlor crystallization is separated out, and filter, and obtain sodium-chlor and filtrating five, filtrating five mixes with the filtrating one of next round step (1) gained and after reuse.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection that the present invention is confirmed by claims of being submitted to.
Claims (3)
1. one kind prepares the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, and said waste residue copper sludge is for producing the Vat Grey BG gained, and the component of said waste residue copper sludge is following: cupric chloride 3.44%; Cupric sulfide 13.44%, sodium sulphite 3.53%, sodium-chlor 3.26%; Sodium sulfate 1.67%, water 20.4%, organic impurity 50%; It is characterized in that this method comprises the steps:
Step (1), weighing waste residue copper sludge with waste residue copper sludge furnishing soup compound, through filtering, obtain cupric sulfide filter cake and filtrating one with service water; The cupric sulfide filter cake is after washing, and drying obtains copper sulphide product;
The molar content of sodium sulphite in step (2), the calculating filtrating one; Ratio according to sodium sulphite and the molar weight of the pure substance of hydrogenchloride is 1: 1.6-2.4; The filtrating one of step (1) gained is dropped into corrosion resistant reactor reaction with hydrochloric acid soln; Obtain containing the mixing solutions of cupric chloride, sodium-chlor and sodium sulfate, discharge hydrogen sulfide simultaneously;
Step (3), the mixing solutions that contains cupric chloride, sodium-chlor and sodium sulfate of step (2) gained is filtered, obtain extremely a spot of filter cake impurity and clarifying filtrating;
Step (4), the first air distillation of the clarifying filtrating of step (3) gained is steamed low-boiling organic impurities, mainly contain sodium sulfate, sodium-chlor and three kinds of materials of cupric chloride in the surplus solution that obtains;
Step (5), calculate the molar content of the sodium sulfate in the surplus solution, and add calcium chloride, make sulfate ion and calcium ion be combined into calcium sulfate and precipitate, and generate sodium-chlor, after the filtration, obtain calcium sulfate precipitation and filtrate three;
Main sodium chloride-containing and copper chloride in step (6), the filtrating three, the molar content of calculating copper chloride, and according to the excessive hydrogen sulfide solution of this molar content adding; Make the reaction of copper chloride and hydrogen sulfide generate copper sulfide and hydrogen chloride; This reaction is redox reaction, and the copper sulfide precipitation of generation is insoluble to hydrochloric acid solution, thereby; Reaction can be carried out, and obtains copper sulphide product and filtrating four after filtration;
Step (7), filtrating four are the supersaturated solution of sodium-chlor through underpressure distillation, and the sodium-chlor crystallization is separated out, and filter, and obtain sodium-chlor and filtrating five, and filtrating five is mixed with the filtrating one of next round step (1) gained and reused.
2. as claimed in claim 1ly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, said waste residue copper sludge is characterized in that for producing the Vat Grey BG gained hydrogen sulfide that step (2) is discharged feeds in the alkali lye or through reclaiming and makes hydrosulphuric acid.
3. as claimed in claim 1ly prepare the method for cupric sulfide and sodium-chlor with the waste residue copper sludge, said waste residue copper sludge is characterized in that for producing the Vat Grey BG gained, and the filter cake impurity that step (3) obtains is buried or burn.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101827681A CN102367173A (en) | 2011-07-01 | 2011-07-01 | Method for preparing copper sulphide and sodium chloride by utilizing waste residue copper sludge |
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| CN2011101827681A CN102367173A (en) | 2011-07-01 | 2011-07-01 | Method for preparing copper sulphide and sodium chloride by utilizing waste residue copper sludge |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392902A (en) * | 2000-09-18 | 2003-01-22 | 英科有限公司 | Recovery of nickel and cobalt values from sulfidic flotation concentrate by chloride assisted oxidative pressure leaching in sulfuric acid |
| CN101503761A (en) * | 2009-03-24 | 2009-08-12 | 中南大学 | Method for separating and recycling valuable metal from pressure leached high sulphur slag |
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2011
- 2011-07-01 CN CN2011101827681A patent/CN102367173A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392902A (en) * | 2000-09-18 | 2003-01-22 | 英科有限公司 | Recovery of nickel and cobalt values from sulfidic flotation concentrate by chloride assisted oxidative pressure leaching in sulfuric acid |
| US20030033906A1 (en) * | 2000-09-18 | 2003-02-20 | Inco Limited | Hydrometallurgical process for the recovery of nickel and cobalt values from a sulfidic flotation concentrate |
| CN101503761A (en) * | 2009-03-24 | 2009-08-12 | 中南大学 | Method for separating and recycling valuable metal from pressure leached high sulphur slag |
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Address after: 523000, room five, building 508, Jinhai building, Dongcheng District Tong Road, Dongguan, Guangdong Applicant after: Wang Jiaxing Address before: Wushi Village Primary School in Dongguan city of Dongcheng District province Guangdong road 523000 Lane 1 No. 6 main mountain Applicant before: Wang Jiaxing |
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Application publication date: 20120307 |