CN107365910A - A kind of method of the purifying containing zinc ion and copper ion organic liquid waste - Google Patents
A kind of method of the purifying containing zinc ion and copper ion organic liquid waste Download PDFInfo
- Publication number
- CN107365910A CN107365910A CN201610319149.5A CN201610319149A CN107365910A CN 107365910 A CN107365910 A CN 107365910A CN 201610319149 A CN201610319149 A CN 201610319149A CN 107365910 A CN107365910 A CN 107365910A
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- China
- Prior art keywords
- ion
- organic liquid
- copper ion
- liquid waste
- waste
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0086—Treating solutions by physical methods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of method for purifying the organic liquid waste containing zinc ion and copper ion, including precipitation, reducing process obtain cuprous bromide, the precipitation method obtain zinc hydroxide and recovery four steps of waste water.Method provided by the invention has that method is simple, is adapted to the characteristics of industrial applications, can effectively reclaim the zinc ion and copper ion in organic liquid waste, be purified organic liquid waste.
Description
Technical field
The invention belongs to fluorine chemical field, and in particular to a kind of method of the purifying containing zinc ion and copper ion organic liquid waste.
Background technology
Have that persistence, toxicity be big, the harm such as seriously polluted containing zinc ion and copper ion waste water, enter environment after discharge,
It can not be biodegradable, it is most of to participate in food chain circulation, and finally accumulate in vivo, destroy organism normal physiological
Metabolic activity, it is detrimental to health.Therefore need before discharging to carrying out zinc ion and copper ion recovery containing zinc and copper-containing wastewater,
To solve problem of environmental pollution, and economize on resources and obtain economic value.
Hexachlorobutadiene is a kind of excellent dry etching gas, has high selectivity and accuracy, can be to less than 100nm even
Narrower width carries out dry ecthing, and environment-friendly, GWP only 290, and the atmospheric lifetime phase is less than 2 days.Produced in hexachlorobutadiene
During, due to using zinc, copper bromide inevitably to generate the organic waste containing zinc ion and copper ion as reaction raw materials
Liquid.Processing for this organic liquid waste containing zinc ion and copper ion, i.e. zinc ion and copper ion are reclaimed, and prior art does not have also
Report.
Therefore, it is necessary to in hexachlorobutadiene production process containing the organic liquid waste of zinc ion and copper ion carry out zinc ion and copper from
Son recovery.
The content of the invention
It is an object of the invention to provide a kind of processing method containing zinc ion and copper ion organic liquid waste, has method simple, suitable
The characteristics of closing industrial applications, can effectively reclaim the zinc ion and copper ion in organic liquid waste, be purified organic liquid waste.
The present invention provides following technical scheme：
A kind of method for purifying the organic liquid waste containing zinc ion and copper ion, methods described include：
(1) organic liquid waste is distilled, it is 50~90 DEG C to control vapo(u)rizing temperature, reclaims organic solvent, remaining is waste liquid；
(2) toward sodium sulfite solution is added in waste liquid, copper ion is made to be reduced into cuprous bromide, adding inorganic acid makes waste liquid
PH value is 3~3.5, and filtering waste liquid obtains filter cake and filtrate, and the filter cake is cuprous bromide；
(3) inorganic alkali solution is added in the filtrate obtained toward step (2), until the pH value of the filtrate is 7~9.5, made
Zinc ion generates zinc hydroxide, is filtrated to get filter cake and filtrate, the filter cake is zinc hydroxide；
(4) filtrate that distilation steps (3) obtain, it is 40~70 DEG C to control vapo(u)rizing temperature, recycle-water.
The organic liquid waste containing zinc ion and copper ion that the present invention purifies is the organic liquid waste containing zinc ion and copper ion, further
Ground says, for caused by during production hexachlorobutadiene containing zinc, copper ion organic liquid waste, its main component include organic solvent,
Copper bromide, cuprous bromide and zinc bromide.Wherein organic solvent is the organic solvent used in hexachlorobutadiene preparation process.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, as a preferred mode, the step
Suddenly in (1), distillation can be vacuum distillation or air-distillation.When to be evaporated under reduced pressure, vapo(u)rizing temperature is preferably 60~85 DEG C,
It is preferably 500~3000Pa to be evaporated under reduced pressure pressure.When for air-distillation when, vapo(u)rizing temperature is preferably 45~65 DEG C.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, uses sulfurous acid in the step (2)
Sodium solution.As preferable mode, the mass concentration of the sodium sulfite solution is 3~50%.As further preferred mode,
The mass concentration of the sodium sulfite solution is 5~30%.
For the dosage in step (2) using sodium sulfite solution, in terms of sodium sulfite, it is preferred that the sodium sulfite
Mol ratio with copper ion is 0.03~0.2:1.It may further be preferable that the mol ratio of the sodium sulfite and copper ion
For 0.05~0.15:1.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, in the step (2), reaction temperature
Preferably 5~50 DEG C, and more preferably 15~35 DEG C.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, in the step (2), as one kind
Preferable mode, first the waste liquid that step (1) obtains is diluted with water, adds sodium sulfite solution.The water and waste liquid
Volume ratio be preferably 0.3~5:1.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, in the step (2), the nothing that uses
Machine acid preferably dilute sulfuric acid and/or watery hydrochloric acid, and more preferably dilute sulfuric acid.The mass concentration of the inorganic acid, preferably 5~
50%, and more preferably 10~30%.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, in the step (3), the nothing that uses
Machine aqueous slkali, it is preferred that the inorganic alkali solution is selected from sodium hydroxide solution and/or potassium hydroxide solution.The inorganic alkali soluble
The mass concentration of liquid, preferably 10~60%, and more preferably 20~50%.
The method of organic liquid waste of the purifying containing zinc ion and copper ion provided by the invention, in the step (3), as one kind
Preferable mode, inorganic alkali solution is added in the filtrate obtained toward step (2), until the pH value of the filtrate is 7.9~9,
Zinc ion is generated zinc hydroxide, be filtrated to get filter cake and filtrate, the filter cake is zinc hydroxide.
Embodiment
The present invention is further described with reference to specific embodiment, but does not limit the invention to these specific implementations
Mode.It is one skilled in the art would recognize that all alternative present invention encompasses what may be included in Claims scope
Scheme, improvement project and equivalents.
The preparation of embodiment 1, hexachlorobutadiene
In 2000ml four-hole boiling flasks, zinc powder about 65g is added, 1-METHYLPYRROLIDONE 600g, is stirred at room temperature down, is passed through trifluoro bromine
Ethene 160g, exothermic heat of reaction, control are passed through speed, and keeping temperature is no more than 70 DEG C, after having led to, and continues stirring reaction 1h.
Above-mentioned reactant mixture is cooled to 5 DEG C, and 226g anhydrous CuBr is added dropwise21-METHYLPYRROLIDONE 400g solution is dissolved in,
Kept for less than 10 DEG C, 2h is added dropwise, be then heated to 40 DEG C of reaction 2h, product is collected with the steel cylinder being placed in -60 DEG C of refrigerator-freezers, obtained
To 125g crude products, content 93.5%.
Collect and mainly contained in the waste liquid of product：Solvent N-methyl pyrilidone, zinc bromide, cuprous bromide, unreacted bromine
Change copper etc..
Embodiment 2, organic liquid waste purifying
(1) precipitation
The 500g waste liquids of the preparation of embodiment 1 are weighed, the recycling design 1-METHYLPYRROLIDONE by the way of vacuum distillation, are subtracted
It is about 84 DEG C to press vapo(u)rizing temperature, and vacuum distillation pressure is 1000Pa, obtains 1-METHYLPYRROLIDONE 340g.
(2) reducing process obtains cuprous bromide
In the raffinate obtained after toward step (1) precipitation, water 80g is added, adds 20% sodium sulfite solution 25g, room temperature is stirred
After mixing 2h, 25% dilute sulfuric acid is added dropwise, adjusts pH value about 3, filtering, 50mL washing filter cakes, obtains filter cake and filtrate.Will
Filter cake is dried, and obtains cuprous bromide 53g.
(3) precipitation method obtain zinc hydroxide
In the filtrate obtained toward step (2), add 20% sodium hydroxide solution and adjust pH value to 8.6 or so, make zinc hydroxide
Separate out, filtering, be filtrated to get filter cake and filtrate.Filter cake is washed with 100g, and zinc hydroxide 38g is obtained after drying.
Simultaneously by obtained filtrate with atomic absorption method carries out copper, Zn content detection, as a result show copper content 2.5ppm in filtrate,
Zn content 4.6ppm, the copper, this recovery of zinc-base in hexachlorobutadiene waste liquid are complete.
(4) waste water is reclaimed
The filtrate that step (3) obtains is evaporated under reduced pressure, vacuum distillation temperature is 55 DEG C, and vacuum distillation pressure is 1500Pa.
Waste water and solid residue are reclaimed, obtains the solid residue 102g based on sodium sulphate and sodium bromide mixture.The waste water of recovery can be with
Applied mechanically.
Embodiment 3, organic liquid waste purifying
(1) precipitation
The 500g waste liquids of the preparation of embodiment 1 are weighed, the recycling design 1-METHYLPYRROLIDONE by the way of vacuum distillation, are subtracted
It is about 81 DEG C to press vapo(u)rizing temperature, and vacuum distillation pressure is 650Pa, obtains 1-METHYLPYRROLIDONE 344g.
(2) reducing process obtains cuprous bromide
In the raffinate obtained after toward step (1) precipitation, water 100g is added, adds 0% sodium sulfite solution 35g, room temperature is stirred
After mixing 2h, 25% dilute sulfuric acid is added dropwise, adjusts pH value about 3.2, filtering, 50mL washing filter cakes, obtains filter cake and filtrate.
Filter cake is dried, obtains cuprous bromide 51.6g.
(3) precipitation method obtain zinc hydroxide
In the filtrate obtained toward step (2), add 20% sodium hydroxide solution and adjust pH value to 9 or so, analyse zinc hydroxide
Go out, filter, be filtrated to get filter cake and filtrate.Filter cake is washed with 100g, and zinc hydroxide 37g is obtained after drying.
Simultaneously by obtained filtrate with atomic absorption method carries out copper, Zn content detection, as a result show copper content 3.6ppm in filtrate,
Zn content 5.7ppm, the copper, this recovery of zinc-base in hexachlorobutadiene waste liquid are complete.
In the filtrate obtained to step 2,20% sodium hydroxide solution of addition regulation pH value to 9 or so, separate out zinc hydroxide,
Filtering, obtains zinc hydroxide precipitation, and filter cake is washed with 100g, zinc hydroxide precipitation drying, weight 37g, off-white powder.
(4) waste water is reclaimed
The filtrate that step (3) obtains is evaporated under reduced pressure, vacuum distillation temperature is 50 DEG C, and vacuum distillation pressure is 1000Pa.
Waste water and solid residue are reclaimed, obtains the solid residue 100g based on sodium sulphate and sodium bromide mixture.The waste water of recovery can be with
Applied mechanically.
Claims (11)
- A kind of 1. method for purifying the organic liquid waste containing zinc ion and copper ion, it is characterised in that methods described includes：(1) organic liquid waste is distilled, it is 50~90 DEG C to control vapo(u)rizing temperature, reclaims organic solvent, remaining is waste liquid；(2) toward sodium sulfite solution is added in waste liquid, copper ion is made to be reduced into cuprous bromide, adding inorganic acid makes waste liquid PH value is 3~3.5, and filtering waste liquid obtains filter cake and filtrate, and the filter cake is cuprous bromide；(3) inorganic alkali solution is added in the filtrate obtained toward step (2), until the pH value of the filtrate is 7~9.5, made Zinc ion generates zinc hydroxide, is filtrated to get filter cake and filtrate, the filter cake is zinc hydroxide；(4) filtrate that distilation steps (3) obtain, it is 40~70 DEG C to control vapo(u)rizing temperature, recycle-water.
- 2. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (1) In, distill to be evaporated under reduced pressure, vapo(u)rizing temperature is 60~85 DEG C, and vacuum distillation pressure is 500~3000Pa.
- 3. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (1) In, it is 45~65 DEG C to distill for air-distillation, vapo(u)rizing temperature.
- 4. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (2) In, the mass concentration of sodium sulfite solution is 3~50%, and the mol ratio of sodium sulfite and copper ion is 0.03~0.2:1, instead It is 5~50 DEG C to answer temperature.
- 5. according to the method for organic liquid waste of the purifying described in claim 4 containing zinc ion and copper ion, it is characterised in that the step (2) In, the mass concentration of sodium sulfite solution is 5~30%, and the mol ratio of sodium sulfite and copper ion is 0.05~0.15:1, instead It is 15~35 DEG C to answer temperature.
- 6. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (2) In, first the waste liquid that step (1) obtains is diluted with water, adds sodium sulfite solution, the volume ratio of the water and waste liquid For 0.3~5:1.
- 7. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (2) In, the inorganic acid is dilute sulfuric acid and/or watery hydrochloric acid, and the mass concentration of inorganic acid is 5~50%.
- 8. according to the method for organic liquid waste of the purifying described in claim 7 containing zinc ion and copper ion, it is characterised in that the step (2) In, the inorganic acid is dilute sulfuric acid, and the mass concentration of inorganic acid is 10~30%.
- 9. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (3) In, inorganic alkali solution is selected from sodium hydroxide solution and/or potassium hydroxide solution, and the mass concentration of inorganic alkali solution is 10~60%, The pH value of the filtrate is 7.9~9.
- 10. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that the step (3) in, the mass concentration of inorganic alkali solution is 20~50%.
- 11. according to the method for organic liquid waste of the purifying described in claim 1 containing zinc ion and copper ion, it is characterised in that described to contain zinc The organic liquid waste of ion and copper ion contains organic solvent, copper bromide, cuprous bromide and zinc bromide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610319149.5A CN107365910A (en) | 2016-05-13 | 2016-05-13 | A kind of method of the purifying containing zinc ion and copper ion organic liquid waste |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610319149.5A CN107365910A (en) | 2016-05-13 | 2016-05-13 | A kind of method of the purifying containing zinc ion and copper ion organic liquid waste |
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| CN107365910A true CN107365910A (en) | 2017-11-21 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434442A (en) * | 2008-12-22 | 2009-05-20 | 冯圣君 | Comprehensive utilization method for industrial waste acid containing cupric ion and special equipment therefor |
| CN101760613A (en) * | 2008-12-02 | 2010-06-30 | 中国恩菲工程技术有限公司 | Method for leaching zinc-containing ores |
| CN102311189A (en) * | 2011-08-12 | 2012-01-11 | 马前 | System for treatment of acid mine drainage and resource recovery of iron, aluminum, copper and zinc in drainage |
| CN102888513A (en) * | 2012-10-15 | 2013-01-23 | 甘肃民族师范学院 | Method of fully separating copper, manganese, zinc, cobalt and calcium chloride solution |
-
2016
- 2016-05-13 CN CN201610319149.5A patent/CN107365910A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760613A (en) * | 2008-12-02 | 2010-06-30 | 中国恩菲工程技术有限公司 | Method for leaching zinc-containing ores |
| CN101434442A (en) * | 2008-12-22 | 2009-05-20 | 冯圣君 | Comprehensive utilization method for industrial waste acid containing cupric ion and special equipment therefor |
| CN102311189A (en) * | 2011-08-12 | 2012-01-11 | 马前 | System for treatment of acid mine drainage and resource recovery of iron, aluminum, copper and zinc in drainage |
| CN102888513A (en) * | 2012-10-15 | 2013-01-23 | 甘肃民族师范学院 | Method of fully separating copper, manganese, zinc, cobalt and calcium chloride solution |
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Application publication date: 20171121 |