CN103641262B - Method for recycling heavy metals in electroplating wastewater by using modified titanium nanotube - Google Patents
Method for recycling heavy metals in electroplating wastewater by using modified titanium nanotube Download PDFInfo
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- CN103641262B CN103641262B CN201310719188.0A CN201310719188A CN103641262B CN 103641262 B CN103641262 B CN 103641262B CN 201310719188 A CN201310719188 A CN 201310719188A CN 103641262 B CN103641262 B CN 103641262B
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Abstract
The invention discloses a method for recycling heavy metals in electroplating wastewater by using a modified titanium nanotube. The method comprises the following steps: soaking a titanium nanotube in absolute ethyl alcohol for 12-48 hours, and drying at 60-80 DEG C to obtain the modified titanium nanotube; adjusting pH of electroplating wastewater to 2-7, and then carrying out settling separation or filtering to remove solid impurities; filling the modified titanium nanotube into a packing column, introducing the pretreated electroplating wastewater into the modified titanium nanotube packing column, and carrying out ion exchange till the titanium nanotube is saturated by adsorption; and putting the modified titanium nanotube which is saturated by adsorption into a sodium hydroxide aqueous solution, soaking for 6-18 hours, then filtering out the modified titanium tube, and drying the solution by distillation to obtain heavy metal substances. According to the method disclosed by the invention, the heavy metal ions in the electroplating wastewater are caught and then recycled by the modified titanium nanotube; the modified titanium nanotube which is used for multiple times can also be used as a denitration catalyst, which is favorable for emission reduction of nitric oxides and having multiple benefits.
Description
Technical field
The invention belongs to electroplating wastewater processing field, be specifically related to a kind of method reclaiming heavy metal out of electroplating wastewater with Modified Titanium nanotube.
Background technology
Electroplating industry is one of the whole world three large contaminated industries.China's electroplating industry develops rapidly at present, and national Electroplate Factory's point about has 10,000.Electroplating industry produces waste water about 4,000,000,000 m every year
3, the problem of environmental pollution caused is quite serious, seriously governs its Sustainable development in China.Containing heavy metal ion such as nickel, copper, chromium, zinc, cadmium, silver in electroplating wastewater, they are difficult to biological degradation in the environment, are easy to accumulation, therefore can produce long-range detrimentally affect to environment and HUMAN HEALTH.How thoroughly to eliminate the heavy metal contamination of electroplating wastewater, reclaim the heavy metal resources in waste water simultaneously, become one of Important Problems that environmental area scholars pay close attention to.
The method of current process effluent containing heavy metal ions mainly contains four classes: the first kind is electrolytic process, utilize the electrochemical properties of metal, under galvanic effect, heavy metal compound is dissociated into metallics at anode, metal is become in cathodic reduction, thus the heavy metal ion in removing waste water; Equations of The Second Kind does not change heavy metal in waste water chemistry of particles form, carries out adsorbing, concentrating and the method be separated, and comprises xylogen absorption, charcoal absorption, solvent extration, ion exchange method etc.; 3rd class is according to solubility product principle, makes heavy metal generate the compound being insoluble in water, reaches the object of solid-liquid separation, comprise moderate water-cut stage, sulphide precipitation etc.; 4th class is by biological organism or the interaction between its meta-bolites and heavy metal, reaches the object of process heavy metal ions in wastewater, comprises bio-flocculation process, biosorption process and plant finishing method etc.
In general, the technology that can be used for processing heavy metal out of electroplating wastewater ion is at present numerous, but the technology that can realize heavy metal recovery is few.
Titanium nanotube is a kind of emerging one dimension titanium base material, presents unique nanotube pattern.The conventional preparation method of titanium nanotube has three kinds: highly basic hydrothermal method, masterplate method, anonizing.The hydrothermal preparing process of titanium nanotube is generally: mixed with strong base solution by titanium dioxide granule, then carries out hydro-thermal reaction at moderate temperatures, the dilute acid soln washing several of the throw out after hydro-thermal, and then optionally with deionized water wash several.The general internal diameter of titanium nanotube that highly basic hydro-thermal legal system obtains is 3 ~ 5 nanometers, and external diameter is 8 ~ 10 nanometers, and length is 50 ~ 150 nanometers.In acid cleaning process after hydro-thermal reaction, H
+meeting and Na
+there is ion-exchange, therefore contain a large amount of proton in titanium-based nano pipe.Due to titanium-based nano pipe both ends open, the proton therefore between inside pipe wall and wall layers has very strong ion-exchange capacity, alkalimetal ion Li
+, Na
+, K
+, Rb
+, Cs
+and Co
2+, Ni
2+, Cu
2+, Zn
2+, Cd
2+all ion-exchange can be carried out with it Deng transition metal ion.Different metal ion is different from the exchange capacity of proton, and ion exchange the most easily occurs basic metal comparatively speaking, and the ability that transition metal ion and proton carry out exchanging is more weak.That is familiar with titanium nanotube physicochemical property along with Chinese scholars deepens continuously, and its Application Areas is constantly expanded.At present in field widespread uses such as photochemistry, electrochemistry, catalytic chemistries.
Patent of invention CN102974305A discloses the method for heavy metal ion in a kind of efficient removal water, to be specially with the titanate nanotube of water heat transfer as adsorptive, to utilize its ion-exchange capacity Adsorption heavy metal ion.But as result of study both domestic and external shows, the titanium nanotube of conventional hydrothermal method synthesis is comparatively strong to the exchange capacity of alkalimetal ion, but limited to the exchange capacity of other transition metal ions, and this certainly will affect the collection efficiency of titanium nanotube heavy metal ion.Containing heavy metal ion such as nickel, copper, chromium, zinc, cadmium, silver in electroplating wastewater, to improve titanium nanotube to the collection efficiency of these heavy metal ion, then its ion-exchange capacity must be strengthened.
Summary of the invention
For solving the shortcoming and defect part of prior art, the object of the present invention is to provide a kind of method reclaiming heavy metal out of electroplating wastewater with Modified Titanium nanotube.
For achieving the above object, the present invention adopts following technical scheme:
Reclaim a method for heavy metal out of electroplating wastewater with Modified Titanium nanotube, comprise the following steps:
(1) Wastewater Pretreatment: the pH value of electroplating wastewater is adjusted to 2 ~ 7 by pH value regulator, then settlement separate or filtration, removes the solid impurity in electroplating wastewater;
(2) heavy metals trapping: Modified Titanium nanotube is packed into glass or stainless stee l packed column, then will introduce Modified Titanium nanotube packed column through the pretreated electroplating wastewater of step (1), carry out ion-exchange, saturated to the absorption of titanium nanotube;
(3) heavy metal recovery: the saturated Modified Titanium nanotube of absorption in step (2) is put into the aqueous sodium hydroxide solution of 0.1 ~ 1mol/L, soaks 6 ~ 18 hours, then leach Modified Titanium nanotube, and by solution evaporate to dryness, obtain heavy metal substance;
Wherein preparation method's concrete steps of Modified Titanium nanotube are: titanium nanotube is soaked 12 ~ 48 hours in dehydrated alcohol, then 60 ~ 80 DEG C of oven dry, obtain described Modified Titanium nanotube.
The present invention's alcohol immersion titanium nanotube, ethanol enters after between the pipe interior of titanium nanotube and wall layers, can bring CH
3cH
2oHH
+group, and then the ion-exchange capacity significantly improving titanium nanotube.Effectively can improve the dispersiveness between single nanotube simultaneously, and protect the tubular structure of titanium nanotube to a certain extent.Soak time is less than the lifting effect that can weaken ion-exchange capacity for 12 hours, and bake out temperature can destroy small part titanium nano tube structure more than 80 DEG C.
Preferably, the loading capacity of described Modified Titanium nanotube heavy metal is 0.15 ~ 0.8mol/mol.
Preferred, described heavy metal comprise in nickel ion, cupric ion, chromium ion, zine ion, cadmium ion and silver ions more than one.
Preferably, described Modified Titanium nanotube is recycled and reused for process electroplating wastewater 10 ~ 20 times, and the same step of working method (1) is to (3); The Modified Titanium nanotube exceeding access times through deionized water wash, 40 ~ 90 DEG C to dry and after 250 ~ 450 DEG C of roastings, as denitrating catalyst.
Modified Titanium nanotube is recycled and reused for process electroplating wastewater 10 ~ 20 times, exceed in the Modified Titanium nanotube of access times and remained part heavy metal, can be used as denitrating catalyst, Modified Titanium nanotube plays the part of the effect of support of the catalyst, the elements such as nickel, copper, chromium, zinc, cadmium, silver become the active ingredient of catalyzer, under its effect, ammonia and oxynitride react, and generate nontoxic nitrogen G&W.
Preferably, described titanium nanotube is obtained by highly basic hydro-thermal legal system.
Preferably, the pH value regulator described in step (1) is NaOH and/or dilute hydrochloric acid; Described electroplating wastewater refers to more than one the electroplating wastewater contained in nickel ion, cupric ion, chromium ion, zine ion, cadmium ion and silver ions.
Preferred, described dilute hydrochloric acid concentration is 0.1 ~ 1mol/L.
Principle of the present invention is: contain abundant sodium ion and proton between the titanium nanotube layer that highly basic hydro-thermal legal system is standby and in tube chamber, these sodium ions and proton can exchange with the heavy metal ion in electroplating wastewater, and this exchange process is reversible.In sour environment, heavy metal ion is exchanged, and fixes between titanium nanotube layer and tube chamber; In weakly alkaline environment, between titanium nanotube layer and intraluminal heavy metal ion by sodium ion exchange, and to enter in solution.The present invention is based on the further investigation to titanium nanotube ion exchange property, by ethanol modifier titanium nanotube, significantly promote its ion-exchange capacity, be then applied to electroplating wastewater processing, and the perfect methods such as the recycling of titanium nanotube, heavy metal recovery, the disposal of waste and old titanium nanotube.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention is with the titanium nanotube of ethanol modifier for raw material, by the heavy metal in its ion-exchange capacity trapping electroplating wastewater, can reuse 10 ~ 20 times, reach the heavy metal removing rate of more than 95%, economical, efficient.
(2) the present invention can not produce secondary pollution, reaches the object that heavy metal ion is turned waste into wealth.Heavy metal ion in electroplating wastewater is modified, and the trapping of titanium nanotube is rear reclaims, and the Modified Titanium nanotube after repeatedly using also can be used as denitrating catalyst, is conducive to the reduction of discharging of oxynitride, has multiple benefits.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) Modified Titanium nanotube is prepared: titanium nanotube to be added in excessive dehydrated alcohol immersion treatment 12 hours, then 60 DEG C of oven dry, obtain Modified Titanium nanotube; The loading capacity of every mole titanium nanotube Adsorption of Chromium is about 0.8 mole after testing;
In the present embodiment to the detection method of Modified Titanium nanotube loading capacity be: configuration chromium nitrate solution, adds Modified Titanium nanotube, the total chromium concn before and after test adds.
(2) process is containing chromium ion electroplating wastewater:
(1) Wastewater Pretreatment: the pH value to 7 regulating chromium plating wastewater with sodium hydroxide, filters and removes solid impurity;
(2) heavy metals trapping: above-mentioned Modified Titanium nanotube is inserted glass or stainless stee l packed column, then will introduce Modified Titanium nanotube packed column through the pretreated electroplating wastewater of step (1), carry out ion-exchange, saturated to the absorption of titanium nanotube;
(3) heavy metal recovery: the saturated Modified Titanium nanotube of absorption in step (2) is put into the aqueous sodium hydroxide solution of 0.1mol/L, soaks 6 hours, then leach Modified Titanium nanotube, and by solution evaporate to dryness, obtain chromium metallics; Chromium metal removal rate is 100%;
(4) recycle of Modified Titanium nanotube and disposal: Modified Titanium nanotube is recycled and reused for process electroplating wastewater 10 times, and the same step of working method (1) is to (3); The Modified Titanium nanotube exceeding access times after deionized water wash, 40 DEG C of oven dry, 250 DEG C of roastings, as denitrating catalyst, temperature of reaction be 120 ~ 350 DEG C, air speed is about 40000h
-1time, the denitration efficiency of more than 90% can be reached.
Embodiment 2
(1) Modified Titanium nanotube is prepared: titanium nanotube to be added in excessive dehydrated alcohol immersion treatment 48 hours, then 80 DEG C of oven dry, obtain Modified Titanium nanotube; The capacity of every mole titanium nanotube absorbing copper is about 0.8 mole after testing;
In the present embodiment to the detection method of Modified Titanium nanotube loading capacity be: configuration copper nitrate solution, adds Modified Titanium nanotube, the total copper concentration before and after test adds.
(2) process is containing chromium ion electroplating wastewater:
(1) Wastewater Pretreatment: the pH value to 2 regulating copper plating wastewater with sodium hydroxide, filters and removes solid impurity;
(2) heavy metals trapping: loaded by above-mentioned Modified Titanium nanotube and insert glass or stainless stee l packed column, then will introduce Modified Titanium nanotube packed column through the pretreated electroplating wastewater of step (1), carry out ion-exchange, saturated to the absorption of titanium nanotube;
(3) heavy metal recovery: the saturated Modified Titanium nanotube of absorption in step (2) is put into the aqueous sodium hydroxide solution of 1mol/L, soaks 18 hours, then leach Modified Titanium nanotube, and by solution evaporate to dryness, obtain copper metallics; Copper metal removal rate is 100%;
(4) recycle of Modified Titanium nanotube and disposal: Modified Titanium nanotube is recycled and reused for process electroplating wastewater 20 times, and the same step of working method (1) is to (3); The Modified Titanium nanotube exceeding access times after deionized water wash, 90 DEG C of oven dry, 450 DEG C of roastings, as denitrating catalyst, temperature of reaction be 120 ~ 350 DEG C, air speed is about 40000h
-1time, the denitration efficiency of more than 90% can be reached.
Embodiment 3
(1) Modified Titanium nanotube is prepared: titanium nanotube to be added in excessive dehydrated alcohol immersion treatment 36 hours, then 60 DEG C of oven dry, obtain Modified Titanium nanotube; The capacity of every mole titanium nanotube absorbed Ni is about 0.8 mole after testing;
In the present embodiment to the detection method of Modified Titanium nanotube loading capacity be: configuration nickel nitrate solution, adds Modified Titanium nanotube, the total nickel concentration before and after test adds.
(2) process is containing chromium ion electroplating wastewater:
(1) Wastewater Pretreatment: use the dilute hydrochloric acid of sodium hydroxide and 1mol/L to regulate the pH value to 5 of nickel-plating waste water, filter and remove solid impurity;
(2) heavy metals trapping: loaded by above-mentioned Modified Titanium nanotube and insert glass or stainless stee l packed column, then will introduce Modified Titanium nanotube packed column through the pretreated electroplating wastewater of step (1), carry out ion-exchange, saturated to the absorption of titanium nanotube;
(3) heavy metal recovery: the saturated Modified Titanium nanotube of absorption in step (2) is put into the aqueous sodium hydroxide solution of 0.2mol/L, soaks 12 hours, then leach Modified Titanium nanotube, and by solution evaporate to dryness, obtain nickel metallics; Nickel metal removal rate is 100%;
(4) recycle of Modified Titanium nanotube and disposal: Modified Titanium nanotube is recycled and reused for process electroplating wastewater 15 times, and the same step of working method (1) is to (3); The Modified Titanium nanotube exceeding access times after deionized water wash, 80 DEG C of oven dry, 350 DEG C of roastings, as denitrating catalyst, temperature of reaction be 120 ~ 350 DEG C, air speed is about 40000h
-1time, the denitration efficiency of more than 90% can be reached.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. reclaim a method for heavy metal out of electroplating wastewater with Modified Titanium nanotube, it is characterized in that, comprise the following steps:
(1) Wastewater Pretreatment: the pH value of electroplating wastewater is adjusted to 2 ~ 7 by pH value regulator, then settlement separate or filtration, removes the solid impurity in electroplating wastewater;
(2) heavy metals trapping: Modified Titanium nanotube is packed into glass or stainless stee l packed column, then Modified Titanium nanotube packed column will be introduced through the pretreated electroplating wastewater of step (1), carry out ion-exchange, saturated to the absorption of titanium nanotube;
(3) heavy metal recovery: the saturated Modified Titanium nanotube of absorption in step (2) is put into the aqueous sodium hydroxide solution of 0.1 ~ 1mol/L, soak 6 ~ 18 hours, then leach Modified Titanium nanotube, and by solution evaporate to dryness, obtain heavy metal substance;
Wherein preparation method's concrete steps of Modified Titanium nanotube are: titanium nanotube is soaked 12 ~ 48 hours in dehydrated alcohol, then 60 ~ 80 DEG C of oven dry, obtain described Modified Titanium nanotube; Described Modified Titanium nanotube is recycled and reused for process electroplating wastewater 10 ~ 20 times, and the same step of working method (1) is to (3); The Modified Titanium nanotube exceeding access times through deionized water wash, 40 ~ 90 DEG C to dry and after 250 ~ 450 DEG C of roastings, as denitrating catalyst; Described heavy metal comprise in nickel ion, cupric ion, chromium ion, zine ion, cadmium ion and silver ions more than one.
2. method according to claim 1, is characterized in that, the loading capacity of described Modified Titanium nanotube heavy metal is 0.15 ~ 0.8mol/mol.
3. method according to claim 1, is characterized in that, described titanium nanotube is obtained by highly basic hydro-thermal legal system.
4. method according to claim 1, is characterized in that, the pH value regulator described in step (1) is NaOH and/or dilute hydrochloric acid; Described electroplating wastewater refers to more than one the electroplating wastewater contained in nickel ion, cupric ion, chromium ion, zine ion, cadmium ion and silver ions.
5. method according to claim 4, is characterized in that, described dilute hydrochloric acid concentration is 0.1 ~ 1mol/L.
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| CN109264888A (en) * | 2018-10-09 | 2019-01-25 | 藤县加裕电子科技有限公司 | Electrolytic etching of metal acid-bearing wastewater is concentrated and separated recovery process and device and waste water treatment system |
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| CN104803520A (en) * | 2015-05-05 | 2015-07-29 | 山东师范大学 | System and method for treating chromium (VI) in electroplating wastewater by utilizing ferrimanganic composite oxides |
| CN107487812A (en) * | 2017-09-02 | 2017-12-19 | 长沙埃比林环保科技有限公司 | A kind of Treating Electroplate Wastewater Containing Nickel exchanges membrane processing method |
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| CN103071446A (en) * | 2013-02-02 | 2013-05-01 | 南京理工大学 | Two-step hydrothermal preparation method of magnetic sodium titanate nanotubes and application of magnetic sodium titanate nanotubes to adsorption removal of Pb<2+> in water |
| CN103272552A (en) * | 2013-05-08 | 2013-09-04 | 上海交通大学 | Recyclable titanate nanometer material capable of treating waste water and application method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103071446A (en) * | 2013-02-02 | 2013-05-01 | 南京理工大学 | Two-step hydrothermal preparation method of magnetic sodium titanate nanotubes and application of magnetic sodium titanate nanotubes to adsorption removal of Pb<2+> in water |
| CN103272552A (en) * | 2013-05-08 | 2013-09-04 | 上海交通大学 | Recyclable titanate nanometer material capable of treating waste water and application method thereof |
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| CN109264888A (en) * | 2018-10-09 | 2019-01-25 | 藤县加裕电子科技有限公司 | Electrolytic etching of metal acid-bearing wastewater is concentrated and separated recovery process and device and waste water treatment system |
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