CN104857946A - Method for using zinc electroplating sludge to prepare azo dyes photocatalyst - Google Patents
Method for using zinc electroplating sludge to prepare azo dyes photocatalyst Download PDFInfo
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- CN104857946A CN104857946A CN201510238575.1A CN201510238575A CN104857946A CN 104857946 A CN104857946 A CN 104857946A CN 201510238575 A CN201510238575 A CN 201510238575A CN 104857946 A CN104857946 A CN 104857946A
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Abstract
The invention relates to a method for using zinc electroplating sludge to prepare an azo dyes photocatalyst. The method comprises the steps: using the electroplating sludge as the raw material, preparing the photocatalyst by roasting, and catalyzing and degrading the azo dyes in the visible light. The polluted water can be directly discharged into the river after treated to reach the discharge standard. The method is capable of effectively recycling the electroplating sludge, and simply, high-efficiently and safely treating the polluted water of the azo dyes.
Description
Technical field
The present invention relates to a kind of preparation method of degrade azo dyestuff photochemical catalyst, particularly a kind of method utilizing zinc electroplating sludge to prepare degrade azo dyestuff photochemical catalyst.
Technical background
Azo dyes is the dyestuff containing azo group in dye molecule.Its synthetic method is simple, and structure is changeable, is therefore the class that in dyestuff, kind is maximum, accounts for more than 50% of synthetic dyestuffs kind, is widely used in dyeing and the stamp of multiple natural and synthetic fibers, also for painting, plastics, rubber etc. painted.Azo dyes complex structure, chemical stability is high, becomes important pollution source of water body.At home and abroad, it is a kind of received method of administering azo dyes and polluting that azo dyes decomposes by utilization reaction, catalysis, therefore, finds the Ke Xunzhi road that a kind of economy, efficiently azo dyes react, catalyst becomes its pollution problem of control.
Zinc electroplating sludge is a kind of dangerous solid waste, derives from zinc electroplating wastewater.And zinc electroplating wastewater refers to the waste water produced in zinc plating production process, wherein main pollutant is each metal ion species, comprises Zn, Fe, Cr, Cu, Ni, Pb, Cd, Mn, Sn, Mg etc.These pollutants itself or its compound can produce toxic action to biology under certain condition, a lot of or even three cause material.According to incompletely statistics, China's Electroplate Factory's point about 20,000, annual electroplating wastewater about 4.0 hundred million m discharged
3.Chemical precipitation method makes to be the method for water-fast compound in the Metal Phase Transition of dissolved state in waste water, extensively be plated factory and apply to electroplating wastewater technical process by oneself, this method is a kind of ripe practical treatment technology, cost low and be convenient to management, processed waste water can reach discharge standard.But chemical precipitation method can produce a large amount of electroplating sludges, and intractability is large.Although the heavy metal in zinc electroplating sludge has the utilization prospects such as catalysis, not easily reclaim, lack recycling means.Therefore, be badly in need of finding suitable zinc electroplating sludge safe disposal and resource utilization method.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing zinc electroplating sludge to prepare degrade azo dyestuff photochemical catalyst.In order to solve the problem that azo dyes is badly in need of administering, zinc electroplating sludge is badly in need of safe handling and utilization, plan zinc electroplating sludge of the present invention prepares photochemical catalyst, carrys out degrade azo dyestuff.
For achieving the above object, the present invention adopts following technical scheme:
Utilize zinc electroplating sludge to prepare a method for degrade azo dyestuff photochemical catalyst, it is characterized in that the concrete steps of the method are:
A. dried by zinc electroplating sludge, ground 100 mesh sieves, obtain zinc electroplating sludge particle;
B. by step a gained zinc electroplating sludge impregnated with particles in the solution of pH=4, solid-to-liquid ratio is 1:5 ~ 1:100, stirs, and keeps the pH=4 of solution in whipping process; Be separated to obtain the mud of supernatant and precipitation;
C. the pH=10 of regulating step b gained supernatant, and obtain the solid being rich in zinc, wash this solid and step b gained mud with water rear mixing respectively, gained solid mixes with mass ratio 1:5 ~ 1:10 with water, and stir post-drying, and oven dry solid abrasive is crossed 100 mesh sieves;
D. by step c gained grind after solid oxygenous 5% ~ 20% atmosphere and 400 ~ 600
ounder C, roasting 2 ~ 8 h, obtains degrade azo dyestuff photochemical catalyst.
When described photochemical catalyst catalytic performance declines, 400 ~ 600
ounder C aerobic conditions after roasting 1 ~ 4 h, carbon is calcined through aerobic, is converted into carbon dioxide, and the thaumatropy of catalyst is mixed-metal oxides-zinc oxide structures, add in electroplating sludge as raw material, thus participate in the Formation and regeneration of degrade azo dyestuff photochemical catalyst.
Photocatalytic mechanism: the degrade azo dyestuff photochemical catalyst prepared in the present invention is a kind of carbon-carried transition metal doping zinc-oxide catalyst, zinc oxide is the excellent semi-conducting material of a kind of photocatalysis performance, the doping of hybrid transition metal oxide can reduce the bandwidth of zinc oxide, under making visible ray, just valence-band electrons transition can be there is, produce light induced electron and hole, the existence of carbon serves the function served as bridge being separated light induced electron and hole, improve the efficiency producing hydroxyl radical free radical, hydroxyl radical free radical has very strong oxidation susceptibility, thus be carbon dioxide by Degradation of Azo Dyes, the Small molecular such as water and nitrogen.
Detailed description of the invention
Embodiment one: (1) gets 500g zinc electroplating sludge, by mud 105 from zinc electroplating sludge factory
odry 24h under C, take 10g, milled 100 mesh sieves; (2) by impregnated with particles in the salpeter solution of the pH=4 of 1L, then regulate pH with the salpeter solution of pH=3, make the pH of solution be stabilized in 4; (3) pour out supernatant, with the ammoniacal liquor of pH=11, it is precipitated, pH is adjusted to 10; (4) wash three times by precipitating and pouring out the base sludge after supernatant, in intermediate water, the two is carried out mix and blend 24h; (5) by the solid of gained 105
odry under C, under the atmosphere of oxygenous 5% ~ 20%, carry out 400 ~ 600
othe roasting of C, take 0.2g and obtain the Congo red of material input 500mL, 10mg/L, under 500W xenon lamp irradiates, degradation rate Congo red after 2h reaches 50.1%.
Embodiment two: (1) gets 400g zinc electroplating sludge, by mud 105 from zinc electroplating sludge factory
odry 24h under C, take 5g, milled 100 mesh sieves; (2) by impregnated with particles in the salpeter solution of the pH=4 of 25mL, then regulate pH with the salpeter solution of pH=3, make the pH of solution be stabilized in 4; (3) pour out supernatant, with the ammoniacal liquor of pH=11, it is precipitated, pH is adjusted to 10; (4) wash three times by precipitating and pouring out the base sludge after supernatant, in 25mL intermediate water, the two is carried out mix and blend 24h; (5) by the solid of gained 105
odry under C, under the atmosphere of oxygenous 5% ~ 20%, carry out 400 ~ 600
othe roasting of C, take 0.2g and obtain the methyl orange that material drops into 500mL, 10mg/L, under 500W xenon lamp irradiates, degradation rate Congo red after 2h reaches 62.3%.
Embodiment three: (1) gets 600g zinc electroplating sludge, by mud 105 from zinc electroplating sludge factory
odry 24h under C, take 15g, milled 100 mesh sieves; (2) by impregnated with particles in the salpeter solution of the pH=4 of 1.5L, then regulate pH with the salpeter solution of pH=3, make the pH of solution be stabilized in 4; (3) pour out supernatant, with the ammoniacal liquor of pH=11, it is precipitated, pH is adjusted to 10; (4) wash three times by precipitating and pouring out the base sludge after supernatant, in 150mL intermediate water, the two is carried out mix and blend 24h; (5) by the solid of gained 105
odry under C, under the atmosphere of oxygenous 5% ~ 20%, carry out 400 ~ 600
othe roasting of C, take 0.2g and obtain the methyl orange that material drops into 500mL, 10mg/L, under 500W xenon lamp irradiates, degradation rate Congo red after 2h reaches 71.4%.
Embodiment four: (1) gets 300g zinc electroplating sludge, by mud 105 from zinc electroplating sludge factory
odry 24h under C, take 20g, milled 100 mesh sieves; (2) by impregnated with particles in the salpeter solution of the pH=4 of 1.2L, then regulate pH with the salpeter solution of pH=3, make the pH of solution be stabilized in 4; (3) pour out supernatant, with the ammoniacal liquor of pH=11, it is precipitated, pH is adjusted to 10; (4) wash three times by precipitating and pouring out the base sludge after supernatant, in 160mL intermediate water, the two is carried out mix and blend 24h; (5) by the solid of gained 105
odry under C, under the atmosphere of oxygenous 5% ~ 20%, carry out 400 ~ 600
othe roasting of C, take 0.2g and obtain the methyl orange that material drops into 500mL, 10mg/L, under 500W xenon lamp irradiates, degradation rate Congo red after 2h reaches 59.6%.
Claims (1)
1. utilize zinc electroplating sludge to prepare a method for degrade azo dyestuff photochemical catalyst, it is characterized in that the concrete steps of the method are:
A. dried by zinc electroplating sludge, ground 100 mesh sieves, obtain zinc electroplating sludge particle;
B. by step a gained zinc electroplating sludge impregnated with particles in the solution of pH=4, solid-to-liquid ratio is 1:5 ~ 1:100, stirs, and keeps the pH=4 of solution in whipping process; Be separated to obtain the mud of supernatant and precipitation;
C. the pH=10 of regulating step b gained supernatant, and obtain the solid being rich in zinc, wash this solid and step b gained mud with water rear mixing respectively, gained solid mixes with mass ratio 1:5 ~ 1:10 with water, and stir post-drying, and oven dry solid abrasive is crossed 100 mesh sieves;
D. by step c gained grind after solid oxygenous 5% ~ 20% atmosphere and 400 ~ 600
ounder C, roasting 2 ~ 8 h, obtains degrade azo dyestuff photochemical catalyst.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510238575.1A CN104857946B (en) | 2015-05-12 | 2015-05-12 | The method that degraded azo dyes photochemical catalyst is prepared using zinc electroplating sludge |
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| CN201510238575.1A CN104857946B (en) | 2015-05-12 | 2015-05-12 | The method that degraded azo dyes photochemical catalyst is prepared using zinc electroplating sludge |
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| CN104857946A true CN104857946A (en) | 2015-08-26 |
| CN104857946B CN104857946B (en) | 2017-05-31 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| HK61278A (en) * | 1973-06-01 | 1978-10-27 | Leigh Interests Ltd | Improvements in and relating to the conversion of liquid hazardous wastes to solid form |
| CN1935709A (en) * | 2006-09-21 | 2007-03-28 | 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 |
| CN102179253A (en) * | 2011-03-10 | 2011-09-14 | 上海大学 | Method for preparing catalyst by using electrolysis waste water and electrolysis sludge |
| CN102380379A (en) * | 2011-09-20 | 2012-03-21 | 上海大学 | Ag/ZnO-AC photochemical catalyst and preparation method thereof |
| CN103028412A (en) * | 2012-12-10 | 2013-04-10 | 上海大学 | Method for preparing carbon black-metallic oxide composite catalyst by using electroplating wastewater or sludge |
-
2015
- 2015-05-12 CN CN201510238575.1A patent/CN104857946B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| HK61278A (en) * | 1973-06-01 | 1978-10-27 | Leigh Interests Ltd | Improvements in and relating to the conversion of liquid hazardous wastes to solid form |
| CN1935709A (en) * | 2006-09-21 | 2007-03-28 | 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 |
| CN102179253A (en) * | 2011-03-10 | 2011-09-14 | 上海大学 | Method for preparing catalyst by using electrolysis waste water and electrolysis sludge |
| CN102380379A (en) * | 2011-09-20 | 2012-03-21 | 上海大学 | Ag/ZnO-AC photochemical catalyst and preparation method thereof |
| CN103028412A (en) * | 2012-12-10 | 2013-04-10 | 上海大学 | Method for preparing carbon black-metallic oxide composite catalyst by using electroplating wastewater or sludge |
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