CN104857946B - The method that degraded azo dyes photochemical catalyst is prepared using zinc electroplating sludge - Google Patents
The method that degraded azo dyes photochemical catalyst is prepared using zinc electroplating sludge Download PDFInfo
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- CN104857946B CN104857946B CN201510238575.1A CN201510238575A CN104857946B CN 104857946 B CN104857946 B CN 104857946B CN 201510238575 A CN201510238575 A CN 201510238575A CN 104857946 B CN104857946 B CN 104857946B
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Abstract
The present invention relates to a kind of method that utilization zinc electroplating sludge prepares degraded azo dyes photochemical catalyst.The present invention prepares photochemical catalyst, under visible light catalytic degradation azo dyes using electroplating sludge as raw material by roasting.Discharge standard is reached after polluted-water is processed, river can be discharged directly into.Present approach provides a kind of efficient resource utilization electroplating sludge, and simply, efficiently, the method for safe handling azo dyes polluted-water.
Description
Technical field
It is particularly a kind of to utilize zinc electroplating sludge the present invention relates to a kind of preparation method of azo dyes photochemical catalyst of degrading
The method for preparing degraded azo dyes photochemical catalyst.
Technical background
Azo dyes is the dyestuff containing azo group in dye molecule.Its synthetic method is simple, and structure is changeable, therefore is dye
The most class of kind, accounts for more than the 50% of synthetic dyestuffs kind in material, is widely used in the dyeing of various natural and synthetic fibers
And stamp, it is also used for the coloring of paint, plastics, rubber etc..Azo dyes complex structure, chemical stability is high, becomes weight
The pollution source of water body wanted.At home and abroad, it is to be generally accepted a kind of improvement azo to be decomposed azo dyes using reaction, catalysis
The method of dye discoloration, therefore, a kind of economic, efficient azo dyes reaction, catalyst are found as its pollution problem of preventing and treating
Can Xun Zhi roads.
Zinc electroplating sludge is a kind of dangerous solid waste, from zinc electroplating wastewater.And zinc electroplating wastewater refers to zinc electricity
Plating production process in produce waste water, wherein main pollutant be each metal ion species, including Zn, Fe, Cr, Cu, Ni, Pb,
Cd, Mn, Sn, Mg etc..These pollutants are in itself or its compound can give birth to toxic action to bio under certain condition, much very
To being three cause materials.According to incompletely statistics, Electroplate Factory of China point about 20,000, the m of electroplating wastewater about 4.0 hundred million of annual discharge3。
Chemical precipitation method is made in waste water in the method that the Metal Phase Transition of dissolved state is water insoluble compound, and factory is plated extensively
Apply to voluntarily process electroplating wastewater technical process, the method is a kind of ripe practical treatment technology, low cost and be easy to management,
Processed waste water can reach discharge standard.But, chemical precipitation method can produce substantial amounts of electroplating sludge, and intractability is big.Zinc electricity
Although there is the heavy metal in plating sludge catalysis etc. to use prospect, it is not easily recycled, lacks recycling means.Therefore,
It is badly in need of finding the safe disposal of suitable zinc electroplating sludge and resource utilization method.
The content of the invention
It is an object of the invention to provide a kind of method that utilization zinc electroplating sludge prepares degraded azo dyes photochemical catalyst.
In order to solve the problems, such as that azo dyes urgent need is administered, zinc electroplating sludge is badly in need of safe handling and is utilized, plan of the present invention is electroplated with zinc
Sludge prepares photochemical catalyst come azo dyes of degrading.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of method that utilization zinc electroplating sludge prepares degraded azo dyes photochemical catalyst, it is characterised in that the tool of the method
Body step is：
A. zinc electroplating sludge is dried, ground 100 mesh sieve obtains zinc electroplating sludge particle；
B. step a gained zinc electroplating sludge particles are immersed in the solution of pH=4, solid-to-liquid ratio is 1:5~1:100, fully
Stir, the pH=4 of solution is kept in whipping process；Separate to obtain supernatant and the sludge for precipitating；
C. the pH=10 of regulating step b gained supernatant, and the solid rich in zinc is obtained, by the solid and step b gained
Sludge mixes after washing with water respectively, and gained solid is with water with mass ratio 1:5~1:10 mixing, and dry after stirring,
And drying solid abrasive is crossed into 100 mesh sieves；
D. by the solid after step c gained grindings in oxygenous 5% ~ 20% atmosphere and 400 ~ 600o2 ~ 8 are calcined under C
H, obtains azo dyes photochemical catalyst of degrading.
When described photochemical catalyst catalytic performance declines, 400 ~ 600oAfter being calcined 1 ~ 4 h under C aerobic conditions, carbon passes through
Aerobic calcining, is converted into carbon dioxide, and the thaumatropy of catalyst is mixed-metal oxides-zinc oxide structures, used as raw material
In addition electroplating sludge, so as to participate in the preparation and regeneration of degraded azo dyes photochemical catalyst.
Photocatalytic mechanism：The degraded azo dyes photochemical catalyst prepared in the present invention is a kind of carbon-carried transition metal doping oxygen
Change zinc catalyst, zinc oxide is a kind of excellent semi-conducting material of photocatalysis performance, and the doping of hybrid transition metal oxide can
To reduce the bandwidth of zinc oxide so that under visible ray, valence-band electrons transition just can occur, produce light induced electron and hole,
The presence of carbon serves the function served as bridge for separating light induced electron and hole, improves the efficiency for producing hydroxyl radical free radical, and hydroxyl is certainly
There is very strong oxidation susceptibility by base, so as to be the small molecules such as carbon dioxide, water and nitrogen by Degradation of Azo Dyes.
Specific embodiment
Embodiment one：（1）500g zinc electroplating sludges are taken from zinc electroplating sludge factory, by sludge 105o24h is dried under C, is weighed
10g, milled 100 mesh sieve；（2）Particle is immersed in the salpeter solution of the pH=4 of 1L, is then adjusted with the salpeter solution of pH=3
Section pH, makes the pH stabilizations of solution 4；（3）Supernatant is poured out, it is precipitated with the ammoniacal liquor of pH=11, pH is adjusted to 10；（4）
To precipitate and pour out the base sludge after supernatant to wash three times, the two is carried out into mixing 24h in secondary water；（5）Will
The solid of gained is 105oDried under C, 400 ~ 600 are carried out under oxygenous 5% ~ 20% atmosphereoThe roasting of C, weighs 0.2g and is obtained
Material input 500mL, 10mg/L's is Congo red, and under the irradiation of 500W xenon lamps, Congo red degradation rate reaches 50.1% after 2h.
Embodiment two：（1）400g zinc electroplating sludges are taken from zinc electroplating sludge factory, by sludge 105o24h is dried under C, is weighed
5g, milled 100 mesh sieve；（2）Particle is immersed in the salpeter solution of the pH=4 of 25mL, is then adjusted with the salpeter solution of pH=3
Section pH, makes the pH stabilizations of solution 4；（3）Supernatant is poured out, it is precipitated with the ammoniacal liquor of pH=11, pH is adjusted to 10；（4）
To precipitate and pour out the base sludge after supernatant to wash three times, the two is carried out into mixing 24h in 25mL secondary waters；
（5）By the solid of gained 105oDried under C, 400 ~ 600 are carried out under oxygenous 5% ~ 20% atmosphereoThe roasting of C, weighs
0.2g is obtained the methyl orange that material puts into 500mL, 10mg/L, and under the irradiation of 500W xenon lamps, Congo red degradation rate reaches after 2h
62.3%。
Embodiment three：（1）600g zinc electroplating sludges are taken from zinc electroplating sludge factory, by sludge 105o24h is dried under C, is weighed
15g, milled 100 mesh sieve；（2）Particle is immersed in the salpeter solution of the pH=4 of 1.5L, then with the salpeter solution of pH=3
Regulation pH, makes the pH stabilizations of solution 4；（3）Supernatant is poured out, it is precipitated with the ammoniacal liquor of pH=11, pH is adjusted to 10；
（4）To precipitate and pour out the base sludge after supernatant to wash three times, mixed the two in 150mL secondary waters
24h；（5）By the solid of gained 105oDried under C, 400 ~ 600 are carried out under oxygenous 5% ~ 20% atmosphereoThe roasting of C, claims
Take 0.2g and the methyl orange that material puts into 500mL, 10mg/L is obtained, under the irradiation of 500W xenon lamps, Congo red degradation rate reaches after 2h
To 71.4%.
Example IV：（1）300g zinc electroplating sludges are taken from zinc electroplating sludge factory, by sludge 105o24h is dried under C, is weighed
20g, milled 100 mesh sieve；（2）Particle is immersed in the salpeter solution of the pH=4 of 1.2L, then with the salpeter solution of pH=3
Regulation pH, makes the pH stabilizations of solution 4；（3）Supernatant is poured out, it is precipitated with the ammoniacal liquor of pH=11, pH is adjusted to 10；
（4）To precipitate and pour out the base sludge after supernatant to wash three times, mixed the two in 160mL secondary waters
24h；（5）By the solid of gained 105oDried under C, 400 ~ 600 are carried out under oxygenous 5% ~ 20% atmosphereoThe roasting of C, claims
Take 0.2g and the methyl orange that material puts into 500mL, 10mg/L is obtained, under the irradiation of 500W xenon lamps, Congo red degradation rate reaches after 2h
To 59.6%.
Claims (1)
1. a kind of method that utilization zinc electroplating sludge prepares degraded azo dyes photochemical catalyst, it is characterised in that the method it is specific
Step is：
A. zinc electroplating sludge is dried, ground 100 mesh sieve obtains zinc electroplating sludge particle；
B. step a gained zinc electroplating sludge particles are immersed in the solution of pH=4, solid-to-liquid ratio is 1:5~1:100, it is sufficiently stirred for
Uniformly, the pH=4 of solution is kept in whipping process；Separate to obtain supernatant and the sludge for precipitating；
C. the pH=10 of regulating step b gained supernatant, and the solid rich in zinc is obtained, by the solid and step b gained sludge
Mix after washing with water respectively, gained solid is with water with mass ratio 1:5~1:10 mixing, and dry after stirring, and will
Drying solid abrasive crosses 100 mesh sieves；
D. by the solid after step c gained grindings in oxygenous 5% ~ 20% atmosphere and 400 ~ 600o2 ~ 8 h are calcined under C, are obtained
To degraded azo dyes photochemical catalyst.
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| CN104857946B true CN104857946B (en) | 2017-05-31 |
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1485625A (en) * | 1973-06-01 | 1977-09-14 | Chappell C | Conversion of liquid hazardous wastes to solid form |
| CN100431722C (en) * | 2006-09-21 | 2008-11-12 | 上海大学 | Electroplating sludge hydrothermal ferritizing treating method |
| CN101565304A (en) * | 2009-04-30 | 2009-10-28 | 上海大学 | Method for treating electroplating sludge and pickle liquor cooperative with hydrothermal ferrite |
| CN102179253B (en) * | 2011-03-10 | 2012-08-08 | 上海大学 | Method for preparing catalyst by using electrolysis waste water and electrolysis sludge |
| CN102380379B (en) * | 2011-09-20 | 2014-04-02 | 上海大学 | Ag/ZnO-AC photochemical catalyst and preparation method thereof |
| CN103028412B (en) * | 2012-12-10 | 2014-10-15 | 上海大学 | Method for preparing carbon black-metallic oxide composite catalyst by using electroplating wastewater or sludge |
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