CN102367175A - Method for preparing copper sulphide, copper hydroxide and sodium chloride from waste copper sludge - Google Patents
Method for preparing copper sulphide, copper hydroxide and sodium chloride from waste copper sludge Download PDFInfo
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- CN102367175A CN102367175A CN2011101827662A CN201110182766A CN102367175A CN 102367175 A CN102367175 A CN 102367175A CN 2011101827662 A CN2011101827662 A CN 2011101827662A CN 201110182766 A CN201110182766 A CN 201110182766A CN 102367175 A CN102367175 A CN 102367175A
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Abstract
The invention provides a method for preparing copper sulphide, copper hydroxide and sodium chloride from waste copper sludge. The waste copper sludge is obtained by production of vat grey BG. The method comprises the following steps that the waste copper sludge and industrial water are mixed into pulp; the pulp is filtered so that copper sulphide and filtrate I are obtained; the filtrate I and a hydrochloric acid solution undergo a reaction to produce a mixed solution containing copper chloride, sodium chloride and sodium sulfate and simultaneously, hydrogen sulfide gas is discharged; the mixed solution is filtered so that clarified filtrate and a minute quantity of filter cake impurities are obtained; the clarified filtrate is subjected to normal pressure distillation so that organic matter impurities having low boiling points are removed; the clarified filtrate treated by the previous step undergoes a reaction with calcium chloride so that sodium sulfate is removed and filtrate III is obtained; the filtrate III and an excessive sodium bisulfite solution undergo a reaction to produce copper hydroxide precipitates, sodium chloride and sulfur dioxide gas and through filtration, copper hydroxide and filtrate IV are obtained; the filtrate IV is subjected to reduced pressure distillation to form a sodium chloride supersaturated solution; sodium chloride is crystallized and precipitated in the sodium chloride supersaturated solution; and through filtration, sodium chloride and filtrate V are obtained.
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 cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, 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 BG is produced 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 and a kind ofly prepare cupric sulfide with the waste residue copper sludge; The method of verditer and sodium-chlor; Said waste residue copper sludge is for producing the Vat Grey BG gained, and the pollution of dye industry waste residue copper sludge is effectively administered and utilized to this method, also produces various copper bearing compound products; Create considerable economic value, had 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 cupric sulfide with the waste residue copper sludge, and the method for verditer and sodium-chlor, 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 cupric chloride in step (6), the filtrating three; Calculate the molar content of cupric chloride; And according to the excessive sodium sulfite solution of this molar content adding; Make the reaction of cupric chloride and sodium sulfite anhy 96 generate verditer deposition and sodium-chlor and sulfur dioxide gas, through filtering verditer product and filtrating four;
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 cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, its chemical equation is:
Na
2S+2HCl＝＝＝＝2NaCl+H
2S
CuCl
2+2NaHSO
3＝＝2NaCl+Cu(OH)
2↓+2SO
2
Beneficial effect of the present invention is: saidly prepare cupric sulfide with the waste residue copper sludge, and the method for verditer and sodium-chlor, 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 cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, 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%, 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; Contain the about 17.2kg of cupric chloride in the filtrating, the about 42.78kg of sodium-chlor, the about 8.35kg of sodium sulfate;
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 cupric chloride in step (6), the filtrating three; Calculate the molar content of cupric chloride; And according to the excessive sodium sulfite solution of this molar content adding; Make the reaction of cupric chloride and sodium sulfite anhy 96 generate verditer deposition and sodium-chlor and sulfur dioxide gas, through filtering 9.9kg verditer product and filtrating four;
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.
Embodiment 2:
A kind ofly prepare cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, 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%, 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; Contain the about 17.2kg of cupric chloride in the filtrating, the about 42.78kg of sodium-chlor, the about 8.35kg of sodium sulfate;
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 cupric chloride in step (6), the filtrating three; Calculate the molar content of cupric chloride; And according to the excessive sodium sulfite solution of this molar content adding; Make the reaction of cupric chloride and sodium sulfite anhy 96 generate verditer deposition and sodium-chlor and sulfur dioxide gas, through filtering 9.9kg verditer product and filtrating four;
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.
Embodiment 3
A kind ofly prepare cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, 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%, 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: 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; 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 (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 cupric chloride in step (6), the filtrating three; Calculate the molar content of cupric chloride; And according to the excessive sodium sulfite solution of this molar content adding; Make the reaction of cupric chloride and sodium sulfite anhy 96 generate verditer deposition and sodium-chlor and sulfur dioxide gas, through filtering 9.9kg verditer product and filtrating four;
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.
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 cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, and 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 cupric chloride in step (6), the filtrating three; Calculate the molar content of cupric chloride; And according to the excessive sodium sulfite solution of this molar content adding; Make the reaction of cupric chloride and sodium sulfite anhy 96 generate verditer deposition and sodium-chlor and sulfur dioxide gas, through filtering verditer product and filtrating four;
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 cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, 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 cupric sulfide with the waste residue copper sludge, the method for verditer and sodium-chlor, said waste residue copper sludge is characterized in that for producing the Vat Grey BG gained, the filter cake impurity that step (3) obtains is buried or burn.
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|---|---|---|---|
| CN2011101827662A CN102367175A (en) | 2011-07-01 | 2011-07-01 | Method for preparing copper sulphide, copper hydroxide and sodium chloride from waste copper sludge |
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|---|---|---|---|
| CN2011101827662A CN102367175A (en) | 2011-07-01 | 2011-07-01 | Method for preparing copper sulphide, copper hydroxide and sodium chloride from waste copper sludge |
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| CN102367175A true CN102367175A (en) | 2012-03-07 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110817928A (en) * | 2019-11-28 | 2020-02-21 | 中新国际联合研究院 | Method for preparing high-purity hydrated copper chloride by using copper-containing sludge |
| CN115140776A (en) * | 2022-08-03 | 2022-10-04 | 贵州金瑞新材料有限责任公司 | Novel process for producing manganese sulfate by using manganese waste liquid |
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 |
-
2011
- 2011-07-01 CN CN2011101827662A patent/CN102367175A/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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110817928A (en) * | 2019-11-28 | 2020-02-21 | 中新国际联合研究院 | Method for preparing high-purity hydrated copper chloride by using copper-containing sludge |
| CN115140776A (en) * | 2022-08-03 | 2022-10-04 | 贵州金瑞新材料有限责任公司 | Novel process for producing manganese sulfate by using manganese waste liquid |
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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 |