CN109467131A - A method of metal in electroplating sludge being extracted in the form of ferrite crystal to synthesize - Google Patents
A method of metal in electroplating sludge being extracted in the form of ferrite crystal to synthesize Download PDFInfo
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- CN109467131A CN109467131A CN201811227248.6A CN201811227248A CN109467131A CN 109467131 A CN109467131 A CN 109467131A CN 201811227248 A CN201811227248 A CN 201811227248A CN 109467131 A CN109467131 A CN 109467131A
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- electroplating sludge
- ferrite crystal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
-
- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- 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 belongs to Electroplating Sludge Technology fields, disclose a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal.Sodium hydroxide, sodium carbonate, Iron(III) chloride hexahydrate aqueous solution are added into electroplating sludge, mixing is uniformly dispersed, and obtains mixed liquor；Gained mixed liquor is heat-treated at 50~180 DEG C, cooled to room temperature after the completion of heat treatment, it stands, pour out supernatant liquor, by obtained solid slag through centrifugation, washing, drying, it adds hydrochloric acid and carries out pickling, through deionized water washing, drying after solid slag is separated with pickling solution, obtain ferrite crystal.The present invention solves the problems such as currently recycling Heavy Metals in Sludge method is at high cost, complicated for operation, generation secondary pollution and subsequent applications are unknown, realizes containing " materialized " extraction of metal sludge.
Description
Technical field
The invention belongs to Electroplating Sludge Technology fields, and in particular to a kind of to extract electricity in the form of ferrite crystal to synthesize
The method for plating metal in sludge.
Background technique
Electroplating sludge is typically containing metal sludge, is that the processing industries such as plating, electronic device, PCB surface processing are raw
Produce during generate dangerous solid waste, including electrolytic cell Anodic dissolve caused by body refuse and filtering gained body refuse with
And the sludge generated when using chemistry-precipitation method processing waste water.Electroplating sludge moisture content is high, and particle is tiny, and size is only to receive
Rice or micron order.Electroplating sludge complicated component, wherein containing the toxic heavy metals such as a large amount of nickel, chromium, manganese, zinc, cadmium, metal mostly with
Amorphous presence, or wherein with the states such as hydroxide, carbonate, oxide preservation.If electroplating sludge is stored for a long time and is not added
With processing, serious harm can be brought to ecological environment, or even bring more serious secondary pollution to ambient enviroment, jeopardize people
Health.
Currently, the processing method of electroplating sludge mainly has solidification method, thermochemical treatment method, (the pyrogenic process smelting of melting absorption method
Gold), leaching absorption method (hydrometallurgy).Leaching includes metal recovery two steps in the leaching and leachate of metal in absorption method
Suddenly --- the former most common method is the acid-hatching of young eggs and ammonia leaching process, and there are also developing bioleaching methods；The latter include extraction,
The precipitation method, reduction method, electrodeposition process.Silva J E et al. is using sulfuric acid and ammonia solution to Cu, Ni, Cr, Zn in electroplating sludge etc.
Metal leaching behavior carries out probing into discovery: although sulfuric acid leaching is high-efficient, and vitriol lixiviation does not select compared with ammonia leaches
Property, in addition to metal target leaches, other metals (such as Fe, Al, Ca etc.) also leach together.To reduce pollution and carrying out recycling
It utilizes, carrying out selective extraction to precious metals in electroplating sludge is necessary.CN102399991A is with novel
The compound extracting new system of green solvent " ionic liquid " and heavy metal organic complexing agent composition proposes to leach in electroplating sludge
Heavy metal nickel, though generating without new waste, ionic liquid is expensive, and process costs are high, and complicated for operation.CN105907972A
The technical solution of use includes oxidation pulp process, process is leached in P204 saponification, nickel anode liquid is all-trans and extracts process, iron back extraction and salt
Acid regeneration process, copper extraction electrodeposition process, heavy chromium process, P204 nickel soap process, P204 zinc extraction electrodeposition process, nickel electrodeposition work
Sequence, calcium nickel separation process, magnesium calcium separation process and industrial circulation water treatment process.It will plating although the invention is leached by saponification
Valuable metal in sludge enters to extract in organic phase, but cumbersome, and process is tediously long, is not to carry out plating dirt
The good method of landfill in mud.Ore Leaching is respectively adopted in CN101643243, vulcanization separation and concentration, hot-pressure leaching, extraction mention
Pure, chromium hot-pressure oxidation extracts chromic salts, the processes such as iron chloride is extracted to recycle copper, nickel, zinc, chromium, iron from electroplating sludge, substep
Extraction step is various, and it is big that heavy metal mixes separating difficulty；CN103290222A using acidleach, filtering, removal of impurities, repeatedly adjust pH,
Evaporative crystallization and etc. copper and mickel is recycled from electroplating sludge, in the process using a large amount of chemical agents generate fluoride precipitate, shape
The waste of Cheng Xin, method are simultaneously undesirable.By above example it can be seen that, it is current recycle in electroplating sludge metal process there are still
At high cost, complicated for operation, other heavy metals mix simultaneously can not separate, generate secondary pollution problems, change there are still biggish
Into space.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the purpose of the present invention is to provide one kind to synthesize iron
The method that hydrochlorate crystal form extracts metal in electroplating sludge.
The object of the invention is achieved through the following technical solutions:
A method of metal in electroplating sludge being extracted in the form of ferrite crystal to synthesize, and is included the following steps:
(1) sodium hydroxide, sodium carbonate, Iron(III) chloride hexahydrate aqueous solution are added into electroplating sludge, mixing is uniformly dispersed,
Obtain mixed liquor；
(2) mixed liquor of step (1) is heat-treated at 50~180 DEG C, cooled to room temperature after the completion of heat treatment,
It stands, supernatant liquor is poured out, by obtained solid slag through centrifugation, washing, drying；
(3) hydrochloric acid is added into step (2) treated solid slag and carries out pickling, passed through after solid slag is separated with pickling solution
Deionized water washing, drying, obtain ferrite crystal.
Preferably, in mixed liquor described in step (1), 0.5~3mol/L of concentration of sodium carbonate；The concentration of sodium hydroxide
0.5~6mol/L；The concentration of Iron(III) chloride hexahydrate is 0.1~0.3mol/L.
Preferably, the solid-liquid mass ratio of gained mixed liquor is 1:(0.5~10 in step (1)).
Preferably, heat treatment described in step (2), which refers to, directly heats processing or hydro-thermal method processing.
Preferably, in step (2) heat treatment time be 0.5~for 24 hours.
Preferably, time of repose is 0.5~48h in step (2).
Preferably, the concentration of hydrochloric acid is 0.1~2mol/L in step (3).
Preferably, the solid-liquid mass ratio that solid slag and hydrochloric acid are added in step (3) is 1:(0.5~5).
Preferably, acid cleaning process described in step (3) is stirring 0.5~3h, 0.5~1h of ultrasound.
Preferably, gained ferrite crystal is further directly inhaled after grinding using magnetic separator or magnetite in step (3)
Choosing.Obtain the higher ferrite crystal of purity.
The method of the present invention is not limited to electroplating sludge, stands good for other processing containing metal sludge.
The principle of the present invention are as follows: electroplating sludge original slag moisture content surpasses 50% or more, and particle is tiny, complicated component, wherein
Containing metals such as a large amount of calcium, iron, nickel, copper, chromium, magnesium, aluminium, zinc, metal mostly exists with amorphous state, or with calcium sulphate dihydrate,
The states such as half-H 2 O calcium sulphate, metal oxide preservation is wherein.Mixing, which is uniformly dispersed, in step (1) of the present invention makes to regulate and control medicament (hydrogen
Sodium oxide molybdena, sodium carbonate, Iron(III) chloride hexahydrate) dissolution is rapid, and comes into full contact with mud granule with medicament；Step (2)
When heat treatment, due to sodium carbonate two-step hydrolysis, carbanion therein and heavy metal (such as calcium ion) are combined, and are generated readily soluble
Hydroxide ion promotes the heavy metal in electroplating sludge in the carbonate (removing by pickling) of acid, sodium carbonate and sodium hydroxide
Ion achievees the effect that object phase change and crystal growth regulation, makes in sludge in conjunction with the ferro element in Iron(III) chloride hexahydrate
Slightly solubility metal be transferred among liquid phase from being detached from solid phase, and the ferrous acid of morphological rules is formed with the ferro element that adds
Salt crystal MFe2O4(M=Ni, Zn, Mn, Co, Mg etc.).During subsequent standing, the small crystalline substance of new object phase formed in former slag
Gradually the big crystal of long great achievement, subsequent wash are dry due to the variation of solubility with temperature and crystal growth are regular for body, obtain iron content
The mixing slag of hydrochlorate and a small amount of impurity；Acid cleaning process in step (3) washes away the impurity such as calcium carbonate to be formed, magnetic agitation
And ultrasound keeps pickling more thorough, and purer ferrite can be obtained.The ferrite of spinel structure has good chemical stabilization
Property, thermal stability, magnetic property and electric property, can be widely applied to the sides such as microwave device, sensor, catalytic and magnetic aspect
Face.
Compared with the existing technology, method of the invention have the following advantages that and the utility model has the advantages that
(1) present invention solve current recycling Heavy Metals in Sludge method it is at high cost, it is complicated for operation, generate secondary pollution and
The problems such as subsequent applications are unknown is realized containing " materialized " extraction of metal sludge.
(2) the method for the present invention is by " hydro-thermal+pickling " simple two-step process, by the metal in sludge with high level material ferrous acid
The form of salt crystal is directly separated out, very high for the recovery rate of metal target, such as to the recovery rate of nickel ion up to 94% with
On, obtained ferrite crystal purity is higher, reaches 90% or so；And the ferrite product for obtaining spinel structure has well
Chemical stability, thermal stability, magnetic property and electric property can be applied to microwave device, sensor, catalytic and magnetic aspect
Deng.
(3) processing method simple process of the invention, at low cost, not generate secondary pollution and subsequent applications clear, can be real
The recycling of existing sludge is extracted and is directly utilized, Social benefit and economic benefit with higher.
Detailed description of the invention
Fig. 1 is the outside drawing of the electroplating sludge original slag and treated product before handling in the embodiment of the present invention 1.
Fig. 2 is the XRD diagram of the electroplating sludge original slag and treated product before handling in the embodiment of the present invention 1.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) 4g electroplating sludge is taken, sodium hydroxide, sodium carbonate and Iron(III) chloride hexahydrate aqueous solution, which is added, makes solid-to-liquid ratio (w/
It w) is 1:10, the concentration of sodium carbonate is 3mol/L in gained mixed liquor, and the concentration of sodium hydroxide is 6mol/L, ferric chloride hexahydrate
Concentration be 0.3mol/L, be thoroughly mixed uniformly.
(2) mixed liquor of step (1) is transferred in water heating kettle, after closing water heating kettle, set temperature is 180 DEG C, heat preservation
For 24 hours, stop heating, be slowly cooled to room temperature naturally, stand for 24 hours；After standing, upper layer is poured out containing the upper of low-concentration heavy metal
Clear liquid carries out centrifuge washing dehydration to the solid slag after hydro-thermal process and filter residue and drying is obtained sepia or black solid.
(3) 2g step (2) resulting solid sample is taken, adding hydrochloric acid makes solid-to-liquid ratio (w/w) to be 1:5, the concentration of hydrochloric acid
For 2mol/L, stop after magnetic agitation 60min, ultrasonic 30min；Solid slag is separated with pickling solution, and gained nickel ferrite based magnetic loaded is brilliant
Body filter residue is washed with deionized and dries；Magnetic separation recovery processing is carried out to nickel ferrite based magnetic loaded crystal filter residue or is directly utilized.
The outside drawing of the product obtained after electroplating sludge original slag and processing before the present embodiment processing is as shown in Figure 1, by Fig. 1
It can be seen that products therefrom is in black powder after processing.The product obtained after electroplating sludge original slag and processing before the present embodiment processing
XRD diagram as shown in Fig. 2, the obtained product component known to the XRD diagram of Fig. 2 product is nickel ferrite based magnetic loaded.
The recovery rate of nickel reaches 93.76% in the electroplating sludge of the present embodiment, and the purity for obtaining nickel ferrite based magnetic loaded crystal is 88%
Left and right.
Embodiment 2
4kg electroplating sludge is taken to be put into water heating kettle, sodium hydroxide, sodium carbonate and Iron(III) chloride hexahydrate aqueous solution, which is added, to be made
Solid-to-liquid ratio (w/w) is 1:0.5, makes the concentration 0.5mol/L of sodium carbonate in gained mixed liquor, and the concentration of sodium hydroxide is
The concentration of 0.5mol/L, ferric chloride hexahydrate are 0.1mol/L, are sufficiently stirred, and water heating kettle is closed, and set temperature is 50 DEG C, heat preservation
0.5h stands 0.5h after stopping heating.Other technical process are same as Example 1.
The recovery rate of nickel reaches 79.30% in the electroplating sludge of the present embodiment, and the purity for obtaining nickel ferrite based magnetic loaded crystal is 67%
Left and right.
Embodiment 3
It takes 10kg electroplating sludge to be put into water heating kettle, sodium hydroxide, sodium carbonate and Iron(III) chloride hexahydrate aqueous solution is added
Making solid-to-liquid ratio (w/w) is 1:5, makes the concentration 2mol/L of sodium carbonate in gained mixed liquor, and the concentration of sodium hydroxide is 3mol/L,
The concentration of ferric chloride hexahydrate is 0.2mol/L, is sufficiently stirred, and water heating kettle is closed, and set temperature is 120 DEG C, keeps the temperature 12h, stops
It is stood for 24 hours after heating.Other technical process are same as Example 1.
The recovery rate of nickel reaches 85.27% in the electroplating sludge of the present embodiment, and the purity for obtaining nickel ferrite based magnetic loaded crystal is 78%
Left and right.
Embodiment 4
1 ton of electroplating sludge is taken to be put into water heating kettle, sodium hydroxide, sodium carbonate and Iron(III) chloride hexahydrate aqueous solution, which is added, to be made
Solid-to-liquid ratio (w/w) is 1:5, makes the concentration 2.5mol/L of sodium carbonate in gained mixed liquor, and the concentration of sodium hydroxide is 3mol/L,
The concentration of ferric chloride hexahydrate is 0.2mol/L, is sufficiently stirred, and water heating kettle is closed, and set temperature is 120 DEG C, and heat preservation for 24 hours, stops
12h is stood after heating.Other technical process are same as Example 1.
The recovery rate of nickel reaches 87.97% in the electroplating sludge of the present embodiment, and the purity for obtaining nickel ferrite based magnetic loaded crystal is 75%
Left and right.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal, it is characterised in that including walking as follows
It is rapid:
(1) sodium hydroxide, sodium carbonate, Iron(III) chloride hexahydrate aqueous solution are added into electroplating sludge, mixing is uniformly dispersed, obtains
Mixed liquor；
(2) mixed liquor of step (1) is heat-treated at 50~180 DEG C, cooled to room temperature after the completion of heat treatment is quiet
It sets, pours out supernatant liquor, by obtained solid slag through centrifugation, washing, drying；
(3) hydrochloric acid is added into step (2) treated solid slag and carries out pickling, gone after solid slag is separated with pickling solution from
Sub- water washing, drying, obtain ferrite crystal.
2. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
It is characterized in that: in mixed liquor described in step (1), 0.5~3mol/L of concentration of sodium carbonate；The concentration 0.5 of sodium hydroxide~
6mol/L；The concentration of Iron(III) chloride hexahydrate is 0.1~0.3mol/L.
3. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: the solid-liquid mass ratio of gained mixed liquor is 1:(0.5~10 in step (1)).
4. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: heat treatment described in step (2), which refers to, directly heats processing or hydro-thermal method processing.
5. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: in step (2) heat treatment time be 0.5~for 24 hours.
6. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: time of repose is 0.5~48h in step (2).
7. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: the concentration of hydrochloric acid is 0.1~2mol/L in step (3).
8. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: the solid-liquid mass ratio that solid slag and hydrochloric acid are added in step (3) is 1:(0.5~5).
9. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: acid cleaning process described in step (3) is stirring 0.5~3h, 0.5~1h of ultrasound.
10. a kind of method to synthesize metal in extraction electroplating sludge in the form of ferrite crystal according to claim 1,
Be characterized in that: gained ferrite crystal further directly inhales choosing using magnetic separator or magnetite after grinding in step (3).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527838A (en) * | 2019-09-29 | 2019-12-03 | 华南理工大学 | A kind of method that hydro-thermal cooperates with chromium in extraction electroplating sludge with oxidation |
| CN113120977A (en) * | 2021-04-30 | 2021-07-16 | 佛山经纬纳科环境科技有限公司 | Method for preparing nickel ferrite nano material from nickel-containing iron electroplating wastewater and application |
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| CN101792226A (en) * | 2010-03-17 | 2010-08-04 | 上海大学 | Ferrite treatment method for electroplating wastewater and pickle liquor by using microwave hydrothermal |
| CN103232231A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of spinel-type NiCuZn ferrite |
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2018
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| CN101792226A (en) * | 2010-03-17 | 2010-08-04 | 上海大学 | Ferrite treatment method for electroplating wastewater and pickle liquor by using microwave hydrothermal |
| CN103232231A (en) * | 2013-04-09 | 2013-08-07 | 昆明理工大学 | Preparation method of spinel-type NiCuZn ferrite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110527838A (en) * | 2019-09-29 | 2019-12-03 | 华南理工大学 | A kind of method that hydro-thermal cooperates with chromium in extraction electroplating sludge with oxidation |
| CN113120977A (en) * | 2021-04-30 | 2021-07-16 | 佛山经纬纳科环境科技有限公司 | Method for preparing nickel ferrite nano material from nickel-containing iron electroplating wastewater and application |
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| CN109467131B (en) | 2021-05-14 |
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