CN102557201B - Micro-electrolysis filling material and preparation method thereof - Google Patents
Micro-electrolysis filling material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a micro-electrolysis filling material. The method comprises the steps of mixing the raw materials including scrap iron, activated carbon and dispersant, calcinating the mixture at the temperature ranging from 1080 DEG C to 1180 DEG C and under oxygen-free conditions; cooling, crushing and screening, wherein the consumed scrap iron accounts for 60 to 70% of the total mass of the raw material, the consumed activated carbon accounts for 20 to 30% of the total mass of the raw material, and the consumed dispersant accounts for 5 to 10% of the total mass of the raw material. The micro-electrolysis filling material has remarkable effects on removing wastewater COD (Chemical Oxygen Demand) and lowering the chromaticness, can improve the biodegradability of wastewater well, avoids inactivation and hardening during treatment process, and is stable and effective during long-term operation, so that the reaction rate is high and only 30 to 60 minutes is required to treat industrial wastewater; the micro-electrolysis filling material is relatively lower in iron content, so that the specific weight is greatly reduced and convenience is provided for load, transportation and use; the application range of the activated carbon is expanded, so that convenience is provided for purchase and production; and a wide variety of dispersants can be used in the method and can be adjusted according to different kinds of wastewater, thereby having a better treatment effect on all kinds of wastewater.
Description
Technical field
The present invention relates to a kind of micro-electrolysis stuffing and preparation method thereof.
Background technology
Micro electrolysis tech is a kind of ideal technology of processing at present high concentrated organic wastewater, claims again internal electrolysis.It is in cold situation, utilizes the micro-electrolysis material self being filled in waste water to produce 1.2V potential difference waste water is carried out to electrolysis treatment, to reach the object of degradable organic pollutant.After system water flowing, in equipment, can form countless microbattery systems, at its action space, form an electric field.The nascent state producing in treating processes [H], Fe
2+deng can with waste water in many component generation redox reactions, such as can damaged colored chromophoric group or the auxochrome group of coloring matter in waste water, even chain rupture, reaches the effect of degradation and decolorization; The Fe generating
2+further be oxidized to Fe
3+their hydrate has stronger absorption-flocculation activity, particularly after adding adjusting PH with base value, generate ferrous hydroxide and ferric hydroxide colloid flocculation agent, the ferric hydroxide colloid that their adsorptive power obtains higher than general medicament hydrolysis far away, the molecule, metallics and the organic macromolecule that in planar water, disperse in a large number.The acting in conjunction of its principle of work based on electrochemistry, oxidation-reduction, physical adsorption and flocculation sediment processed waste water.That this method has is applied widely, treatment effect good, with low cost, convenient operating maintenance, do not need the advantages such as power consumption resource.This technique can reduce COD and colourity significantly for the processing of hard-degrading high concentrated waste water, improves the biodegradability of waste water, can have good effect to removing of ammonia nitrogen simultaneously.
The micro-electrolysis material that micro-electrolysis process adopts is traditionally generally iron filings and charcoal, before use, to add soda acid activation, in the process of using, being easy to passivation hardens, again because iron and charcoal are physical contacts, between be easy to form sealing coat micro-electrolysis can not be proceeded and ineffective, this has caused changing continually micro-electrolysis material, and not only the large cost height of workload also affects treatment effect and the efficiency of waste water.In addition, traditional micro-electrolysis material surface-area is too little also makes wastewater treatment need long time, has increased ton water cost of investment, and this has all had a strong impact on utilization and the popularization of micro-electrolysis process.
Summary of the invention
Technical problem to be solved by this invention is to have overcome the in use easy passivation of existing micro-electrolysis stuffing and hardens, thereby can not use for a long time, need to change continually micro-electrolysis stuffing, cause thus the defects such as ton water cost of investment height, a kind of novel micro-electrolysis stuffing and preparation method thereof is provided.Micro-electrolysis stuffing of the present invention has that specific surface area is large, light specific gravity, active strong, current density is large, make water use efficiency high, act on waste water and can efficiently remove COD, reduce colourity, improve biodegradability, treatment effect is stable, various types of trade effluents can be applicable to, filler passivation in operational process can be avoided, the phenomenon such as harden.
One of object of the present invention is to provide a kind of preparation method of micro-electrolysis stuffing, and it comprises the steps: raw material: iron filings, gac and dispersant; Under oxygen free condition, be warming up to 1080 ℃-1180 ℃, in this roasting temperature; Cooling, broken rear screening; Wherein, the 60-70% that the consumption of described iron filings is described raw materials quality; The consumption of described gac is the 20-30% of described raw materials quality; The consumption of described dispersion agent is the 5-10% of described raw materials quality, is preferably 9-10%; Described raw material refers to iron filings, gac and dispersion agent.
Wherein, described iron filings can adopt common iron filings, also can adopt Industry Waste iron filings, consider and control cost, and preferably adopt and reclaim waste iron filing.Described iron filings preferably pass through drying and processing before use, and described drying and processing can adopt this area ordinary method to carry out, and are preferably to dry 1-1.5 hour in 180-220 ℃.The particle diameter of described iron filings is preferably that more than 200 orders this particle size range is wider compared with prior art scope, is more convenient for producing.In the present invention, can adopt the method for this area routine to make the particle diameter of described iron filings meet above-mentioned requirements, as grind rear mistake 200 eye mesh screens.
Wherein, described gac can market purchasing, and it preferably needs to meet following parameter request: 0.15% methylene blue sorptive force >=12ml; PH value is 7-9; Total iron content≤0.10wt%; Chloride content≤0.25wt%; Calcium magnesium (in MgO)≤0.25; Acid-soluble material content≤3.5wt%; Ignition residue≤8wt%; Dry loss of weight≤10wt%, wt% is the per-cent that accounts for described quality of activated carbon.
Wherein, described dispersion agent can be according to general knowledge, thereby select not react and affect the dispersion agent of its performance dispersion effect with waste water, is preferably one or more in aluminum oxide, sodium tetraborate and silicon-dioxide etc.Described dispersion agent can effectively reduce iron mud output, slows down the scale inhibition that scabs.
Wherein, described roasting can adopt the roasting apparatus of this area routine to carry out, and preferably in High Temperature Furnaces Heating Apparatus, carries out.
Wherein, the time of described roasting can be selected according to this area ordinary method, is preferably 9-11 hour.
Wherein, described intensification preferably for to be warming up to 1080 ℃-1180 ℃ from room temperature in 4 hours.Described cooling be preferably that from roasting the cooling 8-10 of temperature hour is to room temperature.
Wherein, the screening of described fragmentation in screening was afterwards preferably screen clothes more than 200 orders.
Two of object of the present invention has been to provide a kind of micro-electrolysis stuffing being made by above-mentioned preparation method.The chemical composition of described micro-electrolysis stuffing is: iron 60-70%, carbon 20-30%, dispersion agent 5-10%.
In the present invention, above-mentioned optimum condition can arbitrary combination on the basis that meets this area general knowledge, obtains each preferred embodiment of the present invention.
Raw material of the present invention and reagent is commercially available obtaining all.
Positive progressive effect of the present invention is:
1, micro-electrolysis stuffing of the present invention can guarantee the continuous action of " galvanic cell " effect, can easily as the assembly of iron charcoal physical mixed not occur that anode and cathode is separated, affects galvanic cell reaction.Micro-electrolysis stuffing of the present invention is micropore alloy structure, specific surface area is large, active strong, not passivation, does not harden, and anode and cathode is carried out proportioning for different waste water, to wastewater treatment, provide larger current density and better micro-electrolysis reaction effect, speed of reaction is fast, and commonly industrial wastewater only needs 30-60 minute, and long-time running is effectively stable.
2, the proportion of described micro-electrolysis stuffing is: 0.8-1.0 ton/cubic meter, specific surface area: 1.0-1.5 meters squared per gram, voidage: 50-60%, physical strength>=1500Kg/cm
2.The size of described micro-electrolysis stuffing can customize according to actual needs.With respect to existing micro-electrolysis stuffing, micro-electrolysis stuffing iron level of the present invention is relatively lower, therefore greatly reduces proportion, is more conducive to shipment, easy to use.The use range of gac increases, and is convenient to buying and produces.The kind of the spendable dispersion agent of the present invention increases, and can be regulated according to different waste water.Micro-electrolysis stuffing of the present invention has good treatment effect to various waste water.
3, micro-electrolysis stuffing of the present invention is for the removal of waste water COD, and the reduction of colourity has significant effect, and can improve well the biodegradability of waste water, and treatment effect is stable.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.
The parameter of the gac using in following embodiment is: 0.15% methylene blue sorptive force (ml) >=12; PH value is 7-9; Total iron content (%)≤0.10; Muriate (wt%)≤0.25; Calcium magnesium (in MgO)≤0.25; Acid-soluble material (wt%)≤3.5; Ignition residue (wt%)≤8; Dry loss of weight (wt%)≤10; Wt% is the per-cent that accounts for quality of activated carbon.
COD examination criteria is GB/T 11914-1989;
B/C is GB/T 7488-1987 than examination criteria;
Colorimetric detection standard is GB/T 11903-1989.
Embodiment 1
Get waste iron filing drying and processing cooling mistake 200 mesh sieves after 1 hour at 200 ℃, by raw material: waste iron filing 68%, gac 22% and aluminum oxide 10% mix tinning (per-cent is the per-cent that accounts for raw materials quality), enter High Temperature Furnaces Heating Apparatus reduction, insulation in 4 hours to the 1080 ℃ cooling in 10 hours that heats up under oxygen free condition is come out of the stove after cooling for 8 hours, after fragmentation, cross 200 mesh sieves, obtain micro-electrolysis stuffing.Wherein iron level 64%, gac 22%, and aluminum oxide 10%, surplus is impurity.The performance index of micro-electrolysis stuffing: proportion is: 0.9 ton/cubic metre, specific surface area: 1.2 meters squared per gram, voidage: 52%, physical strength 1550Kg/cm
2.
Embodiment 2
Get waste iron filing drying and processing cooling mistake 200 mesh sieves after 1.5 hours at 180 ℃, waste iron filing 70%, gac 21% and sodium tetraborate 9% are mixed to tinning (per-cent is the per-cent that accounts for raw materials quality), enter High Temperature Furnaces Heating Apparatus reduction, insulation in 4 hours to the 1080 ℃ cooling in 10 hours that heats up under oxygen free condition is come out of the stove after cooling for 8 hours, after fragmentation, cross 200 mesh sieves, obtain micro-electrolysis stuffing.Wherein iron level 70%, gac 21%, and sodium tetraborate 8%, surplus is impurity.The performance index of micro-electrolysis stuffing: proportion is: 0.99 ton/cubic metre, specific surface area: 1.1 meters squared per gram, voidage: 51%, physical strength is 1600Kg/cm
2.
Embodiment 3
Get waste iron filing drying and processing cooling mistake 200 mesh sieves after 1.5 hours at 180 ℃, by raw material: waste iron filing 60%, gac 30% and silica 1 0% mix tinning (per-cent is the per-cent that accounts for raw materials quality), enter High Temperature Furnaces Heating Apparatus reduction, insulation in 3 hours to the 1180 ℃ cooling in 9 hours that heats up under oxygen free condition is come out of the stove after cooling for 10 hours, after fragmentation, cross 200 mesh sieves, obtain micro-electrolysis stuffing.Wherein iron level 59%, gac 30%, and silica 1 0%, surplus is impurity.The performance index of micro-electrolysis stuffing: proportion is: 0.8 ton/cubic metre, specific surface area: 1.25 meters squared per gram, voidage: 56%, physical strength is 1510Kg/cm
2.
Embodiment 4
Get waste iron filing drying and processing cooling mistake 200 mesh sieves after 1.5 hours at 180 ℃, by raw material: waste iron filing 65%, gac 30% and silicon-dioxide 5% mix tinning (per-cent is the per-cent that accounts for raw materials quality), enter High Temperature Furnaces Heating Apparatus reduction, insulation in 4 hours to the 1180 ℃ cooling in 11 hours that heats up under oxygen free condition is come out of the stove after cooling for 10 hours, after fragmentation, cross 200 mesh sieves, obtain micro-electrolysis stuffing.Wherein iron level 64%, gac 30%, and silicon-dioxide 4%, surplus is impurity.The performance index of micro-electrolysis stuffing: proportion is: 0.8 ton/cubic metre, specific surface area: 1.0 meters squared per gram, voidage: 60%, physical strength is 1500Kg/cm
2.
The removal effect test of effect embodiment 1 micro-electrolysis stuffing to COD
1, with the micro-electrolysis stuffing of embodiment 2, printing and dyeing mill's waste water is processed COD value after Check processing.
Testing method is: get printing and dyeing mill's waste water and carry out 5t/h wastewater treatment test, tank body total residence time 2 hours, 1.0 hours micro-electrolysis stuffing residence time, applies National Standard Method and carry out COD detection after water outlet flocculation sediment.Micro-electrolysis stuffing not passivation in treating processes, do not harden.
Test result is in Table 1:
Table 1
The COD value that can significantly reduce waste water after sewage being processed with micro-electrolysis stuffing of the present invention as seen by table 1, clearance can reach 55%.And table 1 is also shown in, micro-electrolysis stuffing of the present invention is highly stable for the removal effect of COD, still can arrive the clearance substantially consistent with previous test after repetition test.
2, with the micro-electrolysis stuffing of embodiment 1, printing and dyeing industry garden waste water is processed the COD value after Check processing.
Testing method is: get printing and dyeing industry garden waste water and carry out 5t/h wastewater treatment test, tank body total residence time 1.5 hours, 50 minutes condiment residence time, applies National Standard Method and carry out COD detection after water outlet flocculation sediment.Test result is in Table 2:
The COD value that can significantly reduce waste water after sewage being processed with micro-electrolysis stuffing of the present invention as seen by table 1 and table 2, clearance even can reach 58%.
Table 2
Effect embodiment 2
1, with the micro-electrolysis stuffing of embodiment 3, carry out color removal test.
Testing method is: get all kinds of waste water and carry out 5t/h wastewater treatment test, tank body total residence time 2 hours, 50 minutes micro-electrolysis stuffing residence time, after water outlet flocculation sediment, apply National Standard Method and carry out colorimetric detection, micro-electrolysis stuffing not passivation in treating processes, do not harden.Test result is in Table 3:
Table 3
| Kind of waste water | Water inlet colourity | Biochemical after catalysis and micro-electrolysis |
| DDNP waste water | 5000 | ＜30 |
| Dyeing waste water | 800 | ＜40 |
| Surface active agent wastewater | 200 | ＜30 |
| Pharmacy waste water | 500 | ＜20 |
| Grease processing waste water | 5000 | ＜50 |
From table 3, waste water colourity after micro-electrolysis stuffing of the present invention is processed is reduced to below 50, and fall is very obvious.
2, the chromaticity removing effect of micro-electrolysis stuffing of the present invention and common flocculation agent contrast, test result is in Table 4:
Table 4
From table 4, the chromaticity removing effect of micro-electrolysis stuffing of the present invention is apparently higher than common flocculation agent.
Effect embodiment 3
The micro-electrolysis stuffing of embodiment 3 is carried out to biodegradability detection.
Testing method is: get all kinds of waste water and carry out 5t/h wastewater treatment test, tank body total residence time 2 hours, 50 minutes filler residence time, applies National Standard Method and carry out BOD and COD detection, the variation of counter B/C value after water outlet flocculation sediment.Test result is in Table 5:
Table 5
Use micro-electrolysis stuffing of the present invention to carry out after micro-electrolysis, B/C value significantly improves, and has significantly improved biochemical treatment ability.
Claims (9)
1. a preparation method for micro-electrolysis stuffing, is characterized in that: it comprises the steps: raw material: iron filings, gac and dispersant; Under oxygen free condition, be warming up to 1080 ℃-1180 ℃, in this roasting temperature; Cooling, broken rear screening; Wherein, the 60-70% that the consumption of described iron filings is described raw materials quality; The consumption of described gac is the 20-30% of described raw materials quality; The consumption of described dispersion agent is the 5-10% of described raw materials quality; Described dispersion agent is one or more in aluminum oxide, sodium tetraborate and silicon-dioxide; The time of described roasting is 9-11 hour.
2. preparation method as claimed in claim 1, is characterized in that: described iron filings are for reclaiming waste iron filing.
3. preparation method as claimed in claim 1 or 2, is characterized in that: described iron filings pass through drying and processing before use.
4. preparation method as claimed in claim 3, is characterized in that: described drying and processing is for drying 1-1.5 hour in 180-220 ℃.
5. preparation method as claimed in claim 1 or 2, is characterized in that: the particle diameter of described iron filings is more than 200 orders.
6. preparation method as claimed in claim 1 or 2: it is characterized in that: the parameter request of described gac is: 0.15% methylene blue sorptive force >=12ml; PH value is 7-9; Total iron content≤0.10wt%; Chloride content≤0.25wt%; Calcium-magnesium content≤0.25 in MgO; Acid-soluble material content≤3.5wt%; Ignition residue≤8wt%; Dry loss of weight≤10wt%, wt% is the per-cent that accounts for described quality of activated carbon.
7. preparation method as claimed in claim 1 or 2, is characterized in that: described intensification for to be warming up to 1080 ℃-1180 ℃ from room temperature in 4 hours; Described is cooled to from the cooling 8-10 of maturing temperature hour to room temperature.
8. preparation method as claimed in claim 1, is characterized in that: the screening of described fragmentation described in screening was afterwards screen clothes more than 200 orders.
9. the micro-electrolysis stuffing being made by the preparation method described in any one in claim 1～8.
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| CN104261518B (en) * | 2014-09-18 | 2016-01-06 | 武汉理工大学 | A kind of manganese charcoal catalyzed internal electrocatalysis filler and preparation method thereof and application |
| CN104550939B (en) * | 2015-02-06 | 2016-08-24 | 宁夏鸿裕机械科技有限公司 | A kind of micro-electrolysis stuffing and preparation method and application |
| CN107012316B (en) * | 2017-04-07 | 2018-11-09 | 江西理工大学 | With the method for the more first micro-electrolysis stuffings of lateritic nickel ore production Regularization Fe-Ni-C |
| CN113880197B (en) * | 2021-11-17 | 2023-11-24 | 扬州优境环境工程有限公司 | Preparation method of high-concentration industrial wastewater cracking reducing agent |
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