CN102367179A - Method for preparing copper sulfide, cupric chloride and sodium chloride from waste residue copper sludge - Google Patents
Method for preparing copper sulfide, cupric chloride and sodium chloride from waste residue copper sludge Download PDFInfo
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- CN102367179A CN102367179A CN2011101827925A CN201110182792A CN102367179A CN 102367179 A CN102367179 A CN 102367179A CN 2011101827925 A CN2011101827925 A CN 2011101827925A CN 201110182792 A CN201110182792 A CN 201110182792A CN 102367179 A CN102367179 A CN 102367179A
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Abstract
The invention provides a method for preparing copper sulfide, cupric chloride and sodium chloride from waste residue copper sludge. According to the invention, waste residue copper sludge is prepared into a slurry by using industrial water, and the slurry is filtered, such that copper sulfide and a filtrate A are obtained; the filtrate A is subject to a reaction with a hydrochloric acid solution, such that a mixed solution containing cupric chloride, sodium chloride and sodium sulfate is obtained, and hydrogen sulfide gas is discharged; the mixed solution is filtered, such that an extremely small amount of filter cake impurities and a clarified filtrate are obtained; organic impurities with low boiling points are removed from the clarified filtrate through normal-pressure distillation; the filtrate is then subject to a reaction with an appropriate amount of calcium chloride, such that a calcium sulfate precipitate is produced, and sodium chloride is also produced; the solution is filtered, such that calcium sulfate and a filtrate B are obtained; the filtrate B mainly comprises sodium chloride and cupric chloride. According to the dissolubility difference of the two, the solution is crystallized under different temperatures, such that sodium chloride and cupric chloride are respectively 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 cupric chloride 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 BG 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 BG 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 producing Vat Grey BG gained waste residue copper sludge; The method of cupric chloride and sodium-chlor; 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 cupric sulfide with the waste residue copper sludge, the method for cupric chloride and sodium-chlor; 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), the said waste residue copper sludge of weighing with said 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;
Step (5): calculate the content of the sodium sulfate in the surplus solution, and add an amount of calcium chloride according to the content of sodium sulfate, make sulfate ion combine with calcium ion to generate calcium sulfate and precipitate, also generate sodium-chlor simultaneously, process filters calcium sulfate and filtrating two;
Main sodium chloride-containing and cupric chloride in step (6), the filtrating two, the content of sodium-chlor and cupric chloride in the calculating filtrating two; During according to 80 ℃, the solubleness of sodium-chlor is 38g, and the solubleness of cupric chloride is 104g; With 80 ℃ of following underpressure distillation of surplus solution; Make the concentration of sodium-chlor reach supersaturation, and the concentration of cupric chloride does not reach its saturation concentration, at this moment; The sodium-chlor crystallization is separated out, warp filters, and obtains sodium-chlor and filtrating three; The volume of water adjustment filtrating three, and be cooled to 0 ℃, at this moment; The solubleness of sodium-chlor is 35.7g, and the solubleness of cupric chloride is 68.6g, makes the concentration of cupric chloride reach supersaturation; And the concentration of sodium-chlor does not reach its saturation concentration, and at this moment, copper chloride crystal is separated out, warp filters; Obtain cupric chloride and filtrating four, filtrating four merges the back recycling with next round filtrating two.
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 cupric chloride and sodium-chlor, its chemical equation is:
CuS+2HCl＝＝＝＝CuCl
2+H
2S
Na
2S+2HCl＝＝＝＝2NaCl+H
2S
Na
2SO
4+CaCl
2＝＝＝＝CaSO
4↓+2NaCl
Beneficial effect of the present invention is: saidly prepare cupric sulfide with the waste residue copper sludge, and the method for cupric chloride 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 cupric chloride 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; Buried or the burning of filter cake impurity; 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;
Step (5): the content that calculates the sodium sulfate in the surplus solution is approximately 8.35kg; And add an amount of calcium chloride according to the content of sodium sulfate; Make sulfate ion combine with calcium ion to generate calcium sulfate and precipitate, also generate sodium-chlor simultaneously, through filtering calcium sulfate and filtrating two;
Main sodium chloride-containing and cupric chloride in step (6), the filtrating two, the content of sodium-chlor and cupric chloride in the calculating filtrating two, the about 17.2kg of cupric chloride, the about 49.66kg of sodium-chlor; During according to 80 ℃, the solubleness of sodium-chlor is 38g, and the solubleness of cupric chloride is 104g; With 80 ℃ of following underpressure distillation 17L of surplus solution; Make the concentration of sodium-chlor reach supersaturation, and the concentration of cupric chloride does not reach its saturation concentration, at this moment; The sodium-chlor crystallization is separated out, warp filters, and obtains about 43.2kg sodium-chlor and filtrating three; To filtrate three is adjusted to 18L, is cooled to 0 ℃, at this moment; The solubleness of sodium-chlor is 35.7g, and the solubleness of cupric chloride is 68.6g, and the concentration of cupric chloride reaches supersaturation; And the concentration of sodium-chlor does not reach its saturation concentration, and at this moment, copper chloride crystal is separated out, warp filters; Obtain about 5kg cupric chloride and filtrating four, filtrating four merges the back recycling with next round filtrating two.
Embodiment 2:
A kind of waste residue copper sludge prepares cupric sulfide, the method for cupric chloride 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%, 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 137.0kg 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;
Step (5): the content that calculates the sodium sulfate in the surplus solution is approximately 8.35kg; And add an amount of calcium chloride according to the content of sodium sulfate; Make sulfate ion combine with calcium ion to generate calcium sulfate and precipitate, also generate sodium-chlor simultaneously, through filtering calcium sulfate and filtrating two;
Main sodium chloride-containing and cupric chloride in step (6), the filtrating two, the content of sodium-chlor and cupric chloride in the calculating filtrating two, the about 17.2kg of cupric chloride, the about 49.66kg of sodium-chlor; During according to 80 ℃, the solubleness of sodium-chlor is 38g, and the solubleness of cupric chloride is 104g; With 80 ℃ of following underpressure distillation 17L of surplus solution; Make the concentration of sodium-chlor reach supersaturation, and the concentration of cupric chloride does not reach its saturation concentration, at this moment; The sodium-chlor crystallization is separated out, warp filters, and obtains about 43.2kg sodium-chlor and filtrating three; To filtrate three is adjusted to 18L, is cooled to 0 ℃, at this moment; The solubleness of sodium-chlor is 35.7g, and the solubleness of cupric chloride is 68.6g, and the concentration of cupric chloride reaches supersaturation; And the concentration of sodium-chlor does not reach its saturation concentration, and at this moment, copper chloride crystal is separated out, warp filters; Obtain about 5kg cupric chloride and filtrating four, filtrating four merges the back recycling with next round filtrating two.
Embodiment 3
A kind of waste residue copper sludge prepares cupric sulfide, the method for cupric chloride 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%, 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 113.1kg 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;
Step (5): the content that calculates the sodium sulfate in the surplus solution is approximately 8.35kg; And add an amount of calcium chloride according to the content of sodium sulfate; Make sulfate ion combine with calcium ion to generate calcium sulfate and precipitate, also generate sodium-chlor simultaneously, through filtering calcium sulfate and filtrating two;
Main sodium chloride-containing and cupric chloride in step (6), the filtrating two, the content of sodium-chlor and cupric chloride in the calculating filtrating two, the about 17.2kg of cupric chloride, the about 44.67kg of sodium-chlor; During according to 80 ℃, the solubleness of sodium-chlor is 38g, and the solubleness of cupric chloride is 104g; With 80 ℃ of following underpressure distillation 17L of surplus solution; Make the concentration of sodium-chlor reach supersaturation, and the concentration of cupric chloride does not reach its saturation concentration, at this moment; The sodium-chlor crystallization is separated out, warp filters, and obtains about 38.2kg sodium-chlor and filtrating three; To filtrate three is adjusted to 18L, is cooled to 0 ℃, at this moment; The solubleness of sodium-chlor is 35.7g, and the solubleness of cupric chloride is 68.6g, and the concentration of cupric chloride reaches supersaturation; And the concentration of sodium-chlor does not reach its saturation concentration, and at this moment, copper chloride crystal is separated out, warp filters; Obtain about 5kg cupric chloride and filtrating four, filtrating four merges the back recycling with next round filtrating two.
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 cupric chloride 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%, this method comprises the steps:
Step (1), the said waste residue copper sludge of weighing with said 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;
Step (5): calculate the content of the sodium sulfate in the surplus solution, and add an amount of calcium chloride according to the content of sodium sulfate, make sulfate ion combine with calcium ion to generate calcium sulfate and precipitate, also generate sodium-chlor simultaneously, process filters calcium sulfate and filtrating two;
Main sodium chloride-containing and cupric chloride in step (6), the filtrating two, the content of sodium-chlor and cupric chloride in the calculating filtrating two; During according to 80 ℃, the solubleness of sodium-chlor is 38g, and the solubleness of cupric chloride is 104g; With 80 ℃ of following underpressure distillation of surplus solution; Make the concentration of sodium-chlor reach supersaturation, and the concentration of cupric chloride does not reach its saturation concentration, at this moment; The sodium-chlor crystallization is separated out, warp filters, and obtains sodium-chlor and filtrating three; The volume of water adjustment filtrating three, and be cooled to 0 ℃, at this moment; The solubleness of sodium-chlor is 35.7g, and the solubleness of cupric chloride is 68.6g, makes the concentration of cupric chloride reach supersaturation; And the concentration of sodium-chlor does not reach its saturation concentration, and at this moment, copper chloride crystal is separated out, warp filters; Obtain cupric chloride and filtrating four, filtrating four merges the back recycling with next round filtrating two.
2. as claimed in claim 1ly prepare cupric sulfide with the waste residue copper sludge, the method for cupric chloride 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 cupric chloride 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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| CN2011101827925A CN102367179A (en) | 2011-07-01 | 2011-07-01 | Method for preparing copper sulfide, cupric chloride and sodium chloride from waste residue copper sludge |
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| CN2011101827925A CN102367179A (en) | 2011-07-01 | 2011-07-01 | Method for preparing copper sulfide, cupric chloride and sodium chloride from waste residue copper sludge |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102688874A (en) * | 2012-04-24 | 2012-09-26 | 中南大学 | Mechanical dry sulfurization processing method for heavy metal waste residue |
| CN113460965A (en) * | 2021-07-02 | 2021-10-01 | 深圳星河环境股份有限公司 | Method for treating acid copper chloride etching waste liquid and fully recycling acid copper chloride etching waste liquid by using thermal precipitation method |
Citations (2)
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| 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 CN2011101827925A patent/CN102367179A/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 |
|---|---|---|---|---|
| CN102688874A (en) * | 2012-04-24 | 2012-09-26 | 中南大学 | Mechanical dry sulfurization processing method for heavy metal waste residue |
| CN113460965A (en) * | 2021-07-02 | 2021-10-01 | 深圳星河环境股份有限公司 | Method for treating acid copper chloride etching waste liquid and fully recycling acid copper chloride etching waste liquid by using thermal precipitation method |
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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 |