CN103911896A - Method for normal-temperature normal-pressure electro-catalysis wet-type oxidation treatment on cotton pulp black liquor - Google Patents
Method for normal-temperature normal-pressure electro-catalysis wet-type oxidation treatment on cotton pulp black liquor Download PDFInfo
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Abstract
The invention provides a method for normal-temperature normal-pressure electro-catalysis wet-type oxidation treatment on a cotton pulp black liquor. According to the method, organic pollutants on the electrode surface are fast oxidized in a wet-type oxidation system. The method reduces wet-type oxidation temperature and pressure, shortens treatment time, forms a novel electro-catalysis wet-type oxidation technology, effectively reduces a COD value of the black liquor by the combination of electro-catalysis and catalytic wet-type oxidation and realizes decoloring. The waste water treated by the method has greatly improved biodegradability. Through the method, a COD removal rate is 82.6%, a chroma removal rate is 97.8%, and a BOD5/COD value is improved to 0.5 from less than 0.1.
Description
Technical field
The present invention relates to the processing of high-concentration hardly-degradable cotton pulp black liquor, the method that the electrolysis of employing combines with CWO, had not only reduced COD value of waste water, and but also can effectively decolour, improve wastewater biodegradability, was conducive to the follow-up biochemical treatment of waste water.
Background technology
Because China's cotton linter resource is abundant, in producing, China's purified pulp mainly makes the raw material of Cotton Pulp as various fiber products using cotton linter, and meeting produces a large amount of boilings alkalescence black liquor in pulp production technology, its COD value is high, colourity is large, be strong basicity, and difficult for biological degradation, realizing the comprehensive regulation is the emphasis that scholars pay close attention to and study.For the feature of the poor difficult degradation of cotton pulp black liquor biodegradability, mainly preliminary treatment+biochemical treatment to the method for its processing at present, and pretreated object is mainly to improve the biodegradability of black liquor, its pretreated method mainly contains acid-precipitation method (dilution method), Fenton reagent oxidation method, electrolysis, wet oxidation process etc., wherein large, the Fenton reagent price of acid-precipitation method acid consumption and electrolysis and wet oxidation also exist certain restraining factors, makes this several method be difficult to realize industrial applications.
Wherein electrochemical oxidation process and wet oxidation process are as two kinds of high-level oxidation technologies, the principle of its degrading waste water is to utilize the living radical with strong oxidizing property to remove to attack organic matter, make organic matter open loop, scission of link, allow large molecule hardly degraded organic substance be transformed into the small-molecule substance of easy degraded, even directly generate CO
2and H
2o and other inorganic matters, thus reach the organic object of oxidation removal.Electrochemical oxidation process can at normal temperatures and pressures, directly or indirectly produce hydroxyl radical free radical by the electrode reaction that has catalytic activity, thereby effectively degrades difficult biochemical pollutant.But for a long time,, the organic current efficiency of this process degradation is low, organic matter degradation rate is slow, energy consumption is high, is difficult to realize industrialization.Wet oxidation, as a kind of high-level oxidation technology that relatively has Research Prospects, is subject to Environmental Studies person's attention in recent decades always.Although but traditional wet oxidation process has good treatment effect for the organic wastewater of high concentration, difficult degradation, the some shortcomings of its existence and it is subject to certain restrictions in practical application: (1) to equipment and materials require high, must be high temperature high voltage resistant, corrosion-resistant, make the investment of equipment and maintenance cost large; (2) reaction is carried out under High Temperature High Pressure, and system need to maintain the condition of High Temperature High Pressure, and therefore, wet oxidation is only applicable to the wastewater treatment of low discharge high concentration, very uneconomical for the wastewater treatment of low concentration big yield.So, for the feature of cotton pulp black liquor, still there is no comparatively ripe, economic treatment process and method at present and be difficult to qualified discharge.
Publication number is method and the device that CN1654344's the patent of method and the device of high concentrated organic wastewater " the hydro-thermal catalytic oxidation process " has been set forth thermoelectricity treating high-concentration organic wastewater through catalytic oxidation under a kind of High Temperature High Pressure, its operating condition is High Temperature High Pressure, used catalyst is titanium oxide, ceria, ruthenium, bismuth oxide composition, and catalyst and waste water contact area little.And the present invention is a kind of preprocess method that is directed to specially cotton pulp black liquor, can improve after treatment wastewater biodegradability, adopting catalyst is Fe
2o
3-CeO
2/ Al
2o
3support type O composite metallic oxide catalyst, operating condition is normal temperature and pressure, reaction condition gentleness, and catalyst be scattered in reactor bottom increase with waste water contact area, easy operation control and cost are low, industrial applications prospect is wide.
Normal temperature and pressure electricity-the CWO of the present invention's design is processed the method for cotton pulp black liquor, reaction condition gentleness, industrial applications prospect are large, on the basis of wet oxidation and these two kinds of high-level oxidation technologies of electrochemical oxidation, wet oxidation system is incorporated in electrochemical oxidation system, utilization has the self-control load metal oxide complex catalyst of catalytic activity, produce hydroxyl radical free radical, cause the radical chain reaction of wet oxidation, greatly shorten the induction period of free radical and obtain outstanding treatment effect; Simultaneously, the organic pollution of electrode surface is oxidized rapidly in wet oxidation system, the method can reduce temperature and the pressure of wet oxidation, shorten the processing time, form novel electricity-CWO technology, the mode combining with electrolysis and CWO effectively reduces COD value, the realization decolouring of black liquor, and wastewater biodegradability after treatment increases substantially, and then adopt bioanalysis to cotton pulp black liquor processing, reach sewage drainage standard.
Summary of the invention
The object of the invention is to: the method can reduce temperature and the pressure of wet oxidation, shorten the processing time, form a kind of novel electricity-CWO technology, wastewater biodegradability after treatment increases substantially, and then can adopt bioanalysis to realize black liquor processing qualified discharge.
The present invention seeks to realize like this: a kind of normal temperature and pressure electricity-CWO is processed the method for cotton pulp black liquor, implements step by step;
Step 1 regulates cotton pulp black liquor with technical hydrochloric acid, makes pH to 5;
Step 2 electrolysis reactor cathode-anode plate adopts stainless steel, titanium alloy, size 2cm × 4cm, logical voltage constant 15v, polar plate spacing 4.5cm; In passing to constant voltage, add the load metal oxide complex catalyst of 20g/L to reactor bottom, and continuous aeration, aeration rate 2.0L/min carries out electrocatalytic reaction, time 2h under normal temperature, normal pressure; Wherein catalyst activity, selects the one in Fe or Cu or Mn or Zn, and content is 1.0-2.5wt%, helper component Ce, and content is 0.2-0.5wt%;
Step 3 adopts layering preparation catalyst: by content at 90-96wt%, the Al after activated
2o
3be immersed in the cerous nitrate solution of 0.1mol/L, under room temperature, flood after 10-16h, outwell supernatant, steam 8-12h at 75 DEG C, water-bath, be placed in vacuum drying chamber, at 105 DEG C, dry 2-4h, be placed in Muffle furnace, at 400-500 DEG C, roasting 3h, obtain CeO
2-Al
2o
3; Carry out again secondary load, by the CeO obtaining
2-Al
2o
3be immersed in the iron nitrate solution of 0.5-1.5mol/L, under room temperature, flood after 12-14h, outwell supernatant, steam 8-10h in 85 DEG C, water-bath, in vacuum drying chamber at 110 DEG C, dry 3-5h, then be placed in Muffle furnace, at 450 DEG C, roasting 4-6h, obtain support type Fe
2o
3-CeO
2/ Al
2o
3, CuO-CeO
2/ Al
2o
3, MnO
2-CeO
2/ Al
2o
3, ZnO-CeO
2/ Al
2o
3catalyst; Maceration extract in wherein secondary load process also can be selected copper nitrate, manganese nitrate, zinc nitrate.
Know-why of the present invention: the normal temperature and pressure electricity-CWO providing is processed the method for cotton pulp black liquor, on the basis of wet oxidation and these two kinds of high-level oxidation technologies of electrochemical oxidation, wet oxidation system is incorporated in electrochemical oxidation system, utilization has the self-control load metal oxide complex catalyst of catalytic activity, produce hydroxyl radical free radical, cause the radical chain reaction of wet oxidation, greatly shorten the induction period of free radical and obtain outstanding treatment effect.
Technique effect of the present invention: after the catalyst treatment that employing the method makes, the COD clearance of black liquor can reach 82.6%, and chroma removal rate can reach 97.8%, BOD
5/ COD value can be brought up to 0.5(and works as BOD by being less than 0.1 before processing
5when/COD>0.3, be considered to adopt biochemical process processing), process and realize qualified discharge thereby be conducive to following adopted biochemical process, show technological progress.
Brief description of the drawings
The present invention is described further by reference to the accompanying drawings.
Accompanying drawing is the structural representation of static electrolysis reactor;
Accompanying drawing: 1-reactor, 2-positive plate, 3-cotton pulp black liquor, 4-passes into air hose, 5-minus plate, 6-metal oxide catalyst particle.
As shown in the figure: uniform the metal oxide catalyst particle 6 in the bottom of reactor 1 that is loaded with cotton pulp black liquor 3, the left side that passes into air hose 4 being arranged in cotton pulp black liquor 3 arranges positive plate 2, and right side arranges minus plate 5.
Detailed description of the invention
The present invention is described further in conjunction with the embodiments.
Embodiment
Electrolysis unit and operation instruction:
Device: by reactor 1, positive plate 2, cotton pulp black liquor 3, pass into air hose 4, minus plate 5, metal oxide catalyst particle 6 and form;
Operation: with technical hydrochloric acid adjusting cotton pulp black liquor 3, make pH to 5, wherein positive plate 2 is connected to respectively power positive cathode with minus plate 5 by copper cash, when passing to 15v constant voltage, in reactor 1, add the load metal oxide complex catalyst particle 6 of 20g/L, and be dispersed in reactor bottom, and pass into continuously air hose 4 aerations, aeration rate is 2.0L/min, and whole electro-catalysis process is carried out under normal temperature, normal pressure, and the reaction time is 2h.
Electrolysis processing:
Adopt independent electrolysis to process cotton pulp black liquor, the pH=12.5 of pending black liquor, treating capacity is 1L, and COD value is 20790.5mg/L, and the value of BOD/COD is less than 0.1.
Before electrolysis, need to regulate wastewater pH with technical hydrochloric acid, wherein operate governing factor and comprise pH, the polar plate spacing after decomposition voltage, time, waste water regulate, taking final COD clearance as experimental index, do orthogonal test.Wherein table 1 is three levels under operation factors and the each factor in orthogonal test.
Table 1 electrolysis is processed black liquor experiment factor level table
Upper table is that electrolysis is processed operation factors in black liquor orthogonal test and three levels under each factor.
Table 2 electrolysis is processed black liquor experiment orthogonal table
Learnt by upper table data: according to factor primary and secondary and optimum combination, respectively with empirical factor A
3b
3c
2d
1, A
3b
3c
2d
2, A
3b
3c
2d
3do confirmatory experiment, its COD clearance is respectively: 55.6%, 54.8%, 53.9%, draw A
3b
3c
2d
1for optimum combination factor, i.e. operating voltage=15v when electrolysis, reaction time=120min, the pH=5 after acid adding regulates, polar plate spacing=4.5cm, final COD clearance is 55.6%, chroma removal rate is that 65%, BOD/COD=0.2(works as BOD
5when/COD<0.25, be considered to adopt biochemical process processing), but after processing, water outlet still should not adopt biochemical process processing.
CWO embodiment:
Adopt independent catalytic wet air oxidation to process cotton pulp black liquor, black liquor character is with electrolysis embodiment, and operation is carried out at normal temperatures and pressures, wherein catalyst Fe
2o
3-CeO
2/ Al
2o
3preparation:
Al by content after 90-96wt% activated
2o
3be immersed in the cerous nitrate solution of 0.1mol/L, outwell supernatant after flooding 10-16h under room temperature, 8-12h are steamed in 75 DEG C of water-baths, in vacuum drying chamber, at 105 DEG C, dry 2-4h, then in Muffle furnace at 400-500 DEG C roasting 3h, obtain CeO
2-Al
2o
3, then carry out secondary load, the CeO that is about to obtain
2-Al
2o
3be impregnated in the iron nitrate solution that impregnation concentration is 0.5-1.5mol/L, after flooding 12-14h under room temperature, outwell supernatant, steam 8-10h in 85 DEG C of water-baths, in vacuum drying chamber, at 110 DEG C, dry 3-5h, again in Muffle furnace at 450 DEG C roasting 4-6h, obtain support type Fe
2o
3-CeO
2/ Al
2o
3metal oxide composite catalyst.
Table 3 catalytic wet air oxidation is processed black liquor experiment factor level table
Upper table is that catalytic wet air oxidation is processed operation factors in the orthogonal test of black liquor and three levels under each factor.
Table 4 catalytic wet air oxidation is processed black liquor experiment orthogonal table
Learnt by upper table data: according to factor primary and secondary and optimum combination, respectively with empirical factor C
3d
3b
1a
1, C
3d
3b
1a
2, C
3d
3b
1a
3do confirmatory experiment, its COD clearance is respectively: 41.0%, 40.7%, 38.8%, because pH is the secondary cause that the method is processed black liquor, regulate pH lower, acid consumption is larger, in order to reduce costs, select with the identical pH value of electrolysis, be the pH=5 after CWO acid adding regulates, aeration rate=2.0L/min, catalyst amount=20g/L, reaction time=120min, final COD clearance is 40.7%, and chroma removal rate is that 60%, BOD/COD=0.1(works as BOD
5when/COD<0.25, be considered to adopt biochemical process processing).But after processing, water outlet still should not adopt biochemical process processing.
Comparative example 1:
Process cotton pulp black liquor with electrolysis-CWO coupled method, black liquor character is with above embodiment, used catalyst is the catalyst of CWO while processing black liquor separately, implementation and operation condition is the optimal conditions of above-mentioned two kinds of implementation processes, each as follows: pH=5, voltage=15v, polar plate spacing=4.5cm, aeration rate=2L/min, catalyst amount=20g/L, reaction time=120min.
Processing this black liquor COD clearance through electricity-catalytic wet air oxidation is 82.6%, and chroma removal rate is 97.8%.BOD
5the value of/COD is that 0.5(works as BOD
5when/COD>0.3, be considered to adopt biochemical process processing).Follow-uply adopt biochemical treatment to realize qualified discharge.Can find out thus that electrolysis and CWO are coupled and the effect of processing cotton pulp black liquor under normal temperature and pressure is better than two kinds of methods and processes separately the effect of black liquor.
Comparative example 2:
Operating process is with comparative example 1.
Selected catalyst is metal oxide catalyst (non-composite oxide catalysts) catalyst Fe
2o
3/ Al
2o
3preparation method: be the Al of 97g after activated by content
2o
3be impregnated in the iron nitrate solution of 0.5-1.5mol/L, outwell supernatant after flooding 12-14h under room temperature, steam 8-10h in 85 DEG C of water-baths, in vacuum drying chamber, at 110 DEG C, dry 3-5h, then in Muffle furnace at 450 DEG C roasting 4-6h, obtain Fe
2o
3/ Al
2o
3metal oxide catalyst.
Waste water COD clearance is 62.2% after treatment, and chroma removal rate is 75%.BOD
5the value of/COD is that 0.22(works as BOD
5when/COD<0.25, be considered to adopt biochemical process processing), follow-up difficult employing biochemical treatment.Composite type metallic oxide catalyst Fe is described in the time that electricity-catalytic wet air oxidation is processed cotton pulp black liquor
2o
3-CeO
2/ Al
2o
3treatment effect be obviously better than Fe
2o
3/ Al
2o
3.
Claims (2)
1. normal temperature and pressure electricity-CWO is processed a method for cotton pulp black liquor, it is characterized in that: implement step by step;
1) regulate cotton pulp black liquor with technical hydrochloric acid, its pH is 5;
2) electrolysis reactor cathode-anode plate adopts stainless steel, titanium alloy, size 2cm × 4cm, logical voltage constant 15v, polar plate spacing 4.5cm; In passing to constant voltage, add the load metal oxide complex catalyst of 20g/L to reactor bottom, and continuous aeration, aeration rate 2.0L/min carries out electrocatalytic reaction, time 2h under normal temperature, normal pressure;
Wherein catalyst activity, selects the one in Fe or Cu or Mn or Zn, and content is 1.0-2.5wt%, helper component Ce, and content is 0.2-0.5wt%;
Wherein adopt layering preparation catalyst: by content at 90-96wt%, the Al after activated
2o
3be immersed in the cerous nitrate solution of 0.1mol/L, under room temperature, flood after 10-16h, outwell supernatant, steam 8-12h at 75 DEG C, water-bath, be placed in vacuum drying chamber, at 105 DEG C, dry 2-4h, then be placed in Muffle furnace, at 400-500 DEG C, roasting 3h, obtain CeO
2-Al
2o
3; Carry out again secondary load, by the CeO obtaining
2-Al
2o
3be immersed in the iron nitrate solution of 0.5-1.5mol/L, under room temperature, flood after 12-14h, outwell supernatant, steam 8-10h in 85 DEG C, water-bath, be placed in vacuum drying chamber, be at 110 DEG C, dry 3-5h, be placed in again Muffle furnace, at 450 DEG C, roasting 4-6h, obtain support type Fe
2o
3-CeO
2/ Al
2o
3, CuO-CeO
2/ Al
2o
3, MnO
2-CeO
2/ Al
2o
3, ZnO-CeO
2/ Al
2o
3catalyst; Wherein the maceration extract of secondary load also can be selected copper nitrate, manganese nitrate, zinc nitrate.
2. according to method described in claim 1, it is characterized in that: adopt this catalyst treatment COD to remove rate and reach 82.6%, chroma removal rate reaches 97.8%, BOD
5/ COD value can bring up to 0.5 by being less than 0.1 before processing.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105906112A (en) * | 2016-06-08 | 2016-08-31 | 浙江奇彩环境科技股份有限公司 | Method for treating organic wastewater through wet oxidation and photoelectric catalysis |
| CN108547079A (en) * | 2018-06-08 | 2018-09-18 | 北京鹏盛天纤科技有限公司 | A kind of absorbent cotton green continous way production integrating device and technique |
| CN108855049A (en) * | 2018-05-30 | 2018-11-23 | 江苏开放大学（江苏城市职业学院） | A kind of cerium suitable for alkaline sewage catalytic wet oxidation, manganese binary catalyst material |
| CN108940262A (en) * | 2017-05-22 | 2018-12-07 | 中国石油天然气股份有限公司 | A kind of preparation method of the wet oxidizing catalyst suitable for high concentrated organic wastewater |
| CN108940301A (en) * | 2017-05-22 | 2018-12-07 | 中国石油天然气股份有限公司 | A kind of preparation method of copper-based wet oxidizing catalyst |
| CN111108835A (en) * | 2019-11-27 | 2020-05-08 | 同济大学 | Method for improving low organic soil |
| CN113019382A (en) * | 2019-12-25 | 2021-06-25 | 北京国环莱茵环保科技股份有限公司 | Electrocatalytic oxidation catalyst for landfill leachate and preparation method and application thereof |
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Cited By (10)
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|---|---|---|---|---|
| CN105906112A (en) * | 2016-06-08 | 2016-08-31 | 浙江奇彩环境科技股份有限公司 | Method for treating organic wastewater through wet oxidation and photoelectric catalysis |
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| CN108940301A (en) * | 2017-05-22 | 2018-12-07 | 中国石油天然气股份有限公司 | A kind of preparation method of copper-based wet oxidizing catalyst |
| CN108940301B (en) * | 2017-05-22 | 2021-05-28 | 中国石油天然气股份有限公司 | Preparation method of copper-based wet oxidation catalyst |
| CN108940262B (en) * | 2017-05-22 | 2021-06-01 | 中国石油天然气股份有限公司 | Preparation method of wet oxidation catalyst suitable for high-concentration organic wastewater |
| CN108855049A (en) * | 2018-05-30 | 2018-11-23 | 江苏开放大学（江苏城市职业学院） | A kind of cerium suitable for alkaline sewage catalytic wet oxidation, manganese binary catalyst material |
| CN108547079A (en) * | 2018-06-08 | 2018-09-18 | 北京鹏盛天纤科技有限公司 | A kind of absorbent cotton green continous way production integrating device and technique |
| CN108547079B (en) * | 2018-06-08 | 2023-10-10 | 北京鹏盛天纤科技有限公司 | Green continuous production integrated device and process for absorbent cotton |
| CN111108835A (en) * | 2019-11-27 | 2020-05-08 | 同济大学 | Method for improving low organic soil |
| CN113019382A (en) * | 2019-12-25 | 2021-06-25 | 北京国环莱茵环保科技股份有限公司 | Electrocatalytic oxidation catalyst for landfill leachate and preparation method and application thereof |
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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 830013 Urumqi high tech Zone (new city) North Industrial Park, blue sky road, No. 216, No. Patentee after: DELAND WATER TECHNOLOGY Co.,Ltd. Address before: 830013, 216, Lantian Road, North Industrial Zone, hi tech Zone, the Xinjiang Uygur Autonomous Region, Urumqi Patentee before: XINJIANG DELAND Co.,Ltd. |