CN1562775A - Restoring method of activated carbon for decomposing, processing and adsorbing organic substance in waste water through microwave irradiation - Google Patents
Restoring method of activated carbon for decomposing, processing and adsorbing organic substance in waste water through microwave irradiation Download PDFInfo
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- CN1562775A CN1562775A CN 200410020410 CN200410020410A CN1562775A CN 1562775 A CN1562775 A CN 1562775A CN 200410020410 CN200410020410 CN 200410020410 CN 200410020410 A CN200410020410 A CN 200410020410A CN 1562775 A CN1562775 A CN 1562775A
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- 238000000034 method Methods 0.000 title claims description 83
- 238000012545 processing Methods 0.000 title claims description 11
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- 229910052799 carbon Inorganic materials 0.000 claims abstract description 46
- 238000001179 sorption measurement Methods 0.000 claims abstract description 35
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- 238000005516 engineering process Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
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- 239000000956 alloy Substances 0.000 claims description 2
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- 238000005520 cutting process Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
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- 229910001092 metal group alloy Inorganic materials 0.000 claims description 2
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- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachlorophenol Chemical compound OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 description 10
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
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Abstract
The characteristics are: adsorption of organic substances in waste water and regeneration of active carbon are all proceeded in a microwave irradiating regenerating unit, active carbon is granular, humidity is controlled in 35-55 percent, stuffing quantity is 1/3-4/5 of volume of reactor, microwave frequency is 2450 MHz or 915 MHz, power is 0.5-64 kw, temp. is increased to 800-1200 deg.C and kept 3-5 minutes, total irradiating time is 15 minutes. The microwave irradiating regenerating unit consists of magnetron, microwave cavity resonantor and reactor, in top of which water control valve and vapour exit are set on, and there is a blow head in the reactor and sample connection and water exit on bottom of the reactor, alkali solution absorbing tank connected to vapour exit and gas adsorption column.
Description
Technical field
The present invention relates to organic regeneration of activated carbon method and microwave exposure regenerating unit in the microwave exposure disaggregating treatment absorption waste water, be used to handle organic waste water, especially organic wastewater with difficult degradation thereby belongs to water treatment field.
Background technology
Gac is a kind of nonpoisonous and tasteless, has the superior adsorbent of flourishing pore structure and huge specific surface area.Early 1960s, European and American countries begins to use in a large number active carbon adsorption to handle urban drinking water and trade effluent.At present, active carbon adsorption has become a kind of effective means that municipal effluent, advanced treatment of industrial waste water and polluted source purify.Since early 1970s, adopt granular carbon to handle trade effluent, no matter be technically, still on range of application and treatment scale, all develop very fast, as all having had fairly large application, and obtained satisfied effect at aspects such as refinery water, explosive waste water, dyeing waste water, wastewater from chemical industry and electroplating wastewater processing.Along with the Application of Brand Active Carbon scope is extensive day by day, the recovery of gac has begun to obtain people's attention.If the exhausted gac can't reclaim,, also can cause secondary pollution to environment except the processing costs of waste water per ton will increase the 0.8-0.9 unit.Therefore, the regeneration of gac has especially important meaning.
For many years, there are a lot of regeneration method of active carbon to be suggested, to estimate and use.These methods or cause desorb, or use solvent exchange based on elevated temperature, or based on the Decomposition of heat, chemical, electrochemistry or microbial process.The method that is used for regeneration of activated carbon at present mainly contains hot method of reproduction, bio-regeneration method, wet oxidation and Catalytic Wet Oxidation method of reproduction, solvent regeneration process, electrochemical regeneration method, supercutical fluid method of reproduction etc.
Wherein, hot method of reproduction is to use the most sophisticated maximum, industrial regeneration method of active carbon at present.Handle gac behind the organic waste water in regenerative process, organic variation when being heated to differing temps generally is divided into drying, high temperature carbonization and activation three phases.In drying stage (being lower than 200 ℃), mainly remove the volatilizable composition on the gac.The high temperature carbonization stage is to make a part of organism boiling, the vaporization desorption that adsorbs on the gac, and a part of organism generation decomposition reaction generates the small molecule hydrocarbon desorption and comes out, and remaining composition is stayed becomes " fixed carbon " in the gac hole.In this stage, temperature will reach 800-900 ℃, for avoiding the oxidation of gac, generally vacuumize or inert atmosphere under carry out.In the ensuing activation stage, in reactor, feed CO
2, H
2Or gas such as water vapour, with the cleaning activated carbon capillary, make it recover absorption property, activation stage is the key of whole reclaiming process.Heat regeneration generally can't be carried out in-situ regeneration owing to need heat equipment, and the charcoal that needs to give up is transported to specific regeneration unit such as multiple hearth furnace or rotary kiln.General hot regeneration can cause loading capacity and surface-area loss 5-15% in each reprocessing cycle.This is because high temperature has destroyed carbon structure and aperture is blocked.Even loading capacity drops to zero after several cycles.Although hot regeneration can be used to all types of useless charcoals regeneration, its only for year treatment capacity be economically viable greater than 500,000 tons big system.In regenerative process, can produce a large amount of dusty gass, cause secondary pollution easily.
Sum up traditional hot method of reproduction and mainly have following a few point defect: the gac loss is often bigger in (1) regenerative process; (2) regeneration back activated carbon adsorptive capacity has obvious decline; The tail gas that produces when (3) regenerating can cause the secondary pollution of air; (4) the regeneration required time is longer; (5) can not realize in-situ regeneration.
The major cause that causes these shortcomings is that conventional heating is to realize by indirect heating processes such as conduction, convection current, radiation, and thermograde is by in the outer sensing, the outside temperature height, and internal temperature is low; And in the regeneration of activated carbon process, the mass transfer direction of gac internal contamination thing desorption is by outside the interior sensing, causes the heat and mass transfer direction opposite like this, is unfavorable for adsorbed contaminants desorption on the gac, therefore needs to feed carrier gas and promotes mass transfer process.Carrier gas promotes mass transfer, and efficient is not high on the one hand, causes the violent friction between the activated carbon granule on the other hand easily, causes the charcoal loss.The pollutent that desorption gets off is taken in a large amount of carrier gas that feed out of, can cause secondary pollution.Traditional indirect heating speed is slow, thereby the recovery time that needs is long.Traditional heating regenerative operation poor working environment, temperature can't be controlled flexibly, is difficult to realize in-situ regeneration.
Summary of the invention
Purpose of the present invention and task will overcome existing hot renovation process and exist: the gac loss is big in (1) regenerative process; (2) regeneration back activated carbon adsorptive capacity obviously descends; The tail gas that produces when (3) regenerating causes the secondary pollution of air; (4) the regeneration required time is long; (5) can not realize the deficiency of in-situ regeneration, and provide a kind of original position or dystopy of can realizing to regenerate, flexible operation, recovery time is short, energy consumption is low, regeneration back charcoal absorption is functional, the charcoal loss is little, and the microwave exposure disaggregating treatment of using of non-secondary pollution is adsorbed organic regeneration of activated carbon method in the waste water, special proposition technical solution of the present invention.
Basic design of the present invention is to make full use of microwave internal heating, the fast advantage of rate of heating.Microwave heating is heated material inside and outside simultaneously by dipole polarization and two kinds of heating of interfacial polarization principle, does not need heat conducting process, can reach heats at short notice; The another one importance of microwave heating is that it forms and the opposite thermograde of conventional heating direction.That is to say that the highest temperature is at the center of object, heat is outwards transmitted by the center, and for the such operation of regeneration of activated carbon, this effect is very useful.
The present invention is intended to utilize the traditional type of heating of microwave heating replacement that organic gac in the absorption waste water is regenerated.Control is convenient in microwave heating, starts microwave device, and heating begins immediately; Device is closed, and stops heating at once, does not have the heating lag-effect, helps realizing in-situ regeneration, good work environment.In the conventional hot renovation process, be the oxidation of avoiding gac in the high temperature carbonization stage, generally vacuumize or inert atmosphere under carry out; In ensuing activation stage, in reactor, feed CO
2, CO, H
2Or gas such as water vapour, with the cleaning activated carbon capillary, make it recover absorption property.In this renovation process, can omit this two steps, and activation stage carried out prior to the charing stage, because of microwave heating is internal heating, the gac internal temperature is higher than the outside, makes the liquid water of gac inside spray so that the form of steam is outside rapidly, can clear up activated carbon capillary effectively, make it recover absorption property, finish activation; In the process of moisture discharge, the oxygen in the reactor is supplanted, and forms nearly inert environments, can stop gac to burn in the high temperature carbonization stage.
Proposed by the invention adsorbs organic regeneration of activated carbon method in the waste water with the microwave exposure disaggregating treatment, comprises power control, time control, humidity control, absorption saturation detection and manipulation of regeneration, it is characterized in that:
A) manipulation of regeneration of gac adopts the microwave exposure method to carry out;
B) regeneration of organic absorption and gac all is to carry out in same microwave exposure regenerating unit [20] in the waste water [22];
C) gac that is adopted is a particulate state, and its mean particle size is at 2-5mm;
D) microwave exposure disaggregating treatment regeneration of activated carbon technology is:
The first step is packed pending gac in the reactor [10] into, and its humidity is controlled at 35-55%, and the loadings of gac is the 1/3-4/5 of reactor volume;
Second step, start the magnetron [12] of microwave generator, and startup blower fan [21], the microwave frequency that is adopted in the processing is 2450MHz or 915MHz, power is 0.5-64kW, and the gac temperature is elevated to 800-1200 ℃ gradually from room temperature in the regenerative process, keeps 3-5min under this temperature, adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, microwave exposure total time is 5-15min;
In the 3rd step, shut down.Close the power supply of microwave generator earlier, treat magnetron [12] and reactor [10] cooling after, the blowing-out machine.
Microwave exposure regenerating unit of the present invention [20], it is characterized in that: this device mainly is by the magnetron of microwave generator [12], the reactor [10] that sieve plate [13] are equipped with in microwave resonator [11] and bottom constitutes, base of microwave resonator [23] and loam cake [24], reactor is fastened on the central position of resonator cavity by bolt, magnetron [12] then is to be evenly distributed on the outer wall of resonator cavity, top at microwave exposure regenerating unit [20] is communicated with control valve [5] and vapour outlet [16] pipeline, top in reactor is provided with the shower nozzle [8] that communicates with control valve, the bottom is provided with thief hole [14] and water outlet [15], the side is equipped with the blower fan [21] to magnetron [12] and reactor [10] cooling usefulness, adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, the gas that produces in the reactor [10], through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying.
Use organic regeneration of activated carbon method and the microwave exposure regenerating unit in the microwave exposure disaggregating treatment absorption waste water of using proposed by the invention, it is characterized in that:
A) the microwave exposure regenerating unit [20] that organic regeneration of activated carbon method in the microwave exposure disaggregating treatment absorption waste water is used, can adopt its one or more place side by side with the organic regeneration of activated carbon method of microwave exposure disaggregating treatment absorption waste water [22] process flow sheet, be equipped with alkali lye tourie [17], gas adsorption post [18] and blower fan [21], the position that replaces adsorption tower among the raw wastewater processing technological flow figure, and the gac of in reactor [10], packing on request, then, top at microwave exposure regenerating unit [20] is communicated with control valve [5] and vapour outlet [16] pipeline, the bottom is provided with thief hole [14] and water outlet [15] communicates with reuse water pipeline or network of drains, the shower nozzle [8] that is connected with water inlet control valve [5] in addition on the top of microwave exposure regenerating unit [20], and realize that gac is to finish organic absorption and microwave to the regeneration of saturated activity charcoal in same device, i.e. in-situ regeneration;
B) technical process is: in the production, waste water [22] is by strainer [2], lift pump [3], under meter [4], control valve [5], enter active-carbon bed [9] in the reactor [10] through shower nozzle [8], in the active-carbon bed process of flowing through, gac has been finished organic absorption in the waste water, then, flow out from water outlet [15], during this time, want regularly organic concentration from thief hole [14] check water outlet, when a certain goes out water concentration and reaches controlling valu, should close the water inlet control valve [5] of this microwave exposure regenerating unit [20], and start microwave exposure regenerating unit [20], gac heats up, exhaust, finish activation, cooling.Adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, steam waste gas in its reaction reactivation process is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying, active-carbon bed after the regeneration cooled off through blower fan [21], open waste water control valve [5] again, again carry out adsorption operations, adsorb so repeatedly/the reclaiming process processing, at flooding velocity hour, adopt a microwave exposure regenerating unit, and can be equipped with a container for storing liquid [1], be used to store the water inlet in the microwave exposure recovery time section, when flooding quantity is big, should adopt many microwave exposure regenerating units [20], its each water inlet control valve [5] parallel arranged, control separately the device water inlet or cut off the water supply, charcoal absorption during water inlet, gac is regenerated according to said process when cutting off the water supply, when carrying out regenerative operation for one, but another or several still water flowing carry out the absorption program.
Using feature of the present invention also is: adopt relevant industry or department to need the regenerated gac because of the adsorb organic compound attitude that reaches capacity in producing, with method proposed by the invention, in microwave exposure regenerating unit [20], can carry out manipulation of regeneration separately, take out then and reuse, promptly realize dystopy regeneration, or in according to technical process method and step proposed by the invention, adopt microwave exposure regenerating unit [20], the gac for the treatment of manipulation of regeneration that to collect earlier, behind regeneration activating, take out stand-by or in production line, continue and use, regeneration re-uses, and promptly realizes in-situ regeneration.
Of the present invention being further characterized in that: adopt the enterprising mode that goes out down when waste water enters active-carbon bed [9], but, can take down the water intake mode that outes in order to become flexible service efficiency active-carbon bed and the raising gac; Microwave exposure regenerating unit [20], its microwave resonator [11] is the tubular article that the light metal alloy material with magnesium, zinc, aluminium, nickel is made into, its section is Polygons or circle, and its outer side wall is provided with an equally distributed 16-32 magnetron [12], and the power of each magnetron is 0.5-2.0kW; Reactor [10] in the microwave exposure regenerating unit [20], should be by saturating ripple, high temperature resistant, physical strength good and materials such as the silica glass that is easy to process and pottery are made; The sieve plate [13] that be equipped with the bottom of reactor [10] is the sieve aperture of the uniform Φ of being processed with 0.3-3.0mm on its plate face.
About determining of microwave exposure regenerating unit operating parameter, must note the problem of following several aspects: before regeneration of activated carbon, it is very necessary keeping gac that certain humidity is arranged, can clear up activated carbon capillary in the outside process that sprays of water vapor that water forms on the one hand under the microwave exposure effect, water vapor is discharged the oxygen in the reactor on the other hand, can prevent that charing stage gac from burning; The loadings of gac can not be very few, because amounts of activated carbon can not absorb microwave when very few effectively, do not reach the required temperature of regeneration; Can select suitable microwave power and irradiation time according to what and its intensification situation under microwave action of handled amounts of activated carbon in the actual mechanical process.
Precaution when adopting microwave exposure regenerating unit of the present invention to carry out regeneration of activated carbon: answer the integrity of inspection apparatus, equipment and pipeline and each junction that ne-leakage is arranged before (1) device starts; (2) check being connected and security of power supply system and power unit; (3) leak case of inspection microwave source; (4) after guaranteeing that above-mentioned three check results are qualified, can start the microwave exposure regenerating unit, start the blower fan cooling system simultaneously to guarantee that magnetron does not heat up; (5) to note being used for the permission upper limit of thermometric thermopair, avoid causing its damage; (6) before the end of run, must close microwave power supply earlier, and blower fan works on to magnetron and cools off fully.
Major advantage of the present invention is: (1) starts microwave device because control is convenient in microwave heating, and heating begins immediately; Device is closed, and stops heating at once, does not have the heating lag-effect, helps realizing in-situ regeneration; (2) because microwave heating is internal heating, the thermograde of formation is consistent with the mass transfer direction of regeneration of activated carbon, so the regeneration efficiency height; Rate of heating is fast, so the recovery time is short, energy consumption is low; (3) because micro wave regeneration does not need to feed carrier gas, rubbing effect not taking place between the charcoal particle, reduces the charcoal loss; (4) device takes up space less; (5) owing to need not feed carrier gas and activated gas, do not produce non-secondary pollution.
Description of drawings
Further specify details of the present invention below in conjunction with accompanying drawing:
The present invention establishes 4 accompanying drawings altogether, and Fig. 1 is a process flow diagram synoptic diagram of the present invention; Fig. 2 is that the microwave exposure regenerating unit is faced cross-sectional view; Fig. 3 is in the cross-sectional view of facing that adopts a microwave exposure regenerating unit in the process flow sheet; Fig. 4 is the cross-sectional view of facing that is in the process flow sheet microwave exposure regenerating unit that adopts two parallel connections.
Fig. 1 is a process flow diagram synoptic diagram of the present invention.
Waste water [22] passes through pipeline, enter active-carbon bed [9] in the reactor [10] via strainer [2], lift pump [3], under meter [4], control valve [5], in the active-carbon bed process of flowing through, gac has been finished organic absorption in the waste water, then, flow out from water outlet [15].When water outlet reaches controlling concn, should close water inlet control valve [5], start microwave exposure regenerating unit [20], gac intensification, exhaust, lower the temperature, finish activation.The steam waste gas of its reaction in reactivation process is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying.Regenerated is active-carbon bed opens water inlet control valve [5] again after blower fan [21] cooling, waste water enters active-carbon bed [9] again, carries out adsorption operations again.Solid arrow is represented current direction, and dotted arrow is represented steam and residual exhaust flow direction.
Fig. 2 is that the microwave exposure regenerating unit is faced cross-sectional view
Microwave exposure regenerating unit [20] mainly is made of magnetron [12], microwave resonator [11] and reactor [10].Magnetron is evenly distributed on the outer wall of microwave resonator [11], and reactor is placed on the position at the interior center of microwave resonator [11], and base [23] and loam cake [24] by microwave resonator [11] are fixed with bolt.Reactor [10] internal upper part is provided with shower nozzle [8], and the bottom is equipped with sieve plate [13], is used for the support gac.Shower nozzle [8] is communicated with control valve [5], vapour outlet [16] be located at resonator cavity [11] on cover, the bottom is provided with thief hole [14] and water outlet [15].The mensuration of active-carbon bed [9] temperature adopts K-type armoured thermocouple [7] and electronic temp indicator [6], and thermopair [7] is inserted to active-carbon bed [9] central position.This microwave exposure regenerating unit [20] can be connected among the sewage treatment technology process figure by control valve [5] and water outlet [15], replaces the position of adsorption tower, and vapour outlet [16] then is connected with alkali lye tourie, gas adsorption post, residual exhaust emptying.By starting and closing microwave exposure regenerating unit [20] and close and opening controlling valve [5], realization is to the in-situ regeneration of the gac of adsorb organic compound.The direction of arrow is represented the Inlet and outlet water flow path direction, and dotted arrow is represented steam and residual exhaust flow direction, and symbol [21] is a blower fan.
Fig. 3 is in the cross-sectional view of facing that adopts a microwave exposure regenerating unit in the process flow sheet
Microwave exposure regenerating unit shown in Figure 2 [20] is placed sewage treatment technology process figure, the position that replaces former adsorption tower, the control valve [5] on microwave resonator [11] top links to each other with under meter [4] with the lift pump [3] of water inlet, and vapour outlet [16] links to each other with gas adsorption column [18] with alkali lye tourie [17], to handle the steam that regenerative process produces.The water outlet [15] of microwave resonator [11] bottom links to each other with reuse water pipeline or network of drains.At flooding velocity hour, waste water [22] is through container for storing liquid [1], strainer [2], lift pump [3], under meter [4], control valve [5], enter gac [9] bed in the reactor [10] through shower nozzle [8], in the active-carbon bed process of flowing through, gac has been finished organic absorption in the waste water, then, flow out from water outlet [15].When water outlet reaches controlling concn, close water inlet control valve [5], start microwave exposure regenerating unit [20], the steam of generation is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying.Be reused for adsorption operations after the active-carbon bed cooling after the regeneration.The same Fig. 2 of other symbols.The direction of arrow is represented the Inlet and outlet water flow path direction, and dotted arrow is represented steam and residual exhaust flow direction.
Fig. 4 is the cross-sectional view of facing that is in the process flow sheet microwave exposure regenerating unit that adopts two parallel connections
At waste water [22] flooding quantity under big and situation water inlet continuously, can adopt the use in parallel of a plurality of microwave exposure regenerating units, what this figure adopted is that two microwave exposure regenerating units are connected in parallel, and shows two microwave exposure regenerating units in parallel among the figure, wherein, the device on the left side is to be in the adsorption operations process, and shower nozzle [8] is to active-carbon bed water spray, and the device on the right is be in activating and regenerating at this moment the treatment stage, shower nozzle stops water spray, and promptly control valve [5] is a closing condition.Its technical process is: behind waste water [22] process strainer [2], the lift pump [3], enter two tributary under meters [4], control valve [5] in parallel, enter active-carbon bed [9] in the microwave exposure regenerating unit [20] through shower nozzle [8], in each active-carbon bed process of flowing through, finished organic absorption in the waste water, flowed out from water outlet [15] then.During this time, regularly to detect organic concentration the water outlet, when wherein which reaches controlling concn, just close which flow control valve [5] from thief hole [14].In this moment, the water concentration in the device on its right reaches controlling concn just, and therefore, its control valve is closed.Then, start the microwave exposure regenerating unit [20] on the right, start blower fan [21] simultaneously, active-carbon bed intensification, exhaust, finish activation, the cooling, adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, the steam waste gas in its regenerative process is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying.Under the effect of blower fan [21], after active-carbon bed [9] lower the temperature rapidly, open a flow control valve [5] of this microwave exposure regenerating unit [20] again, carry out adsorption operations again.Reach controlling concn if find the water outlet of another microwave exposure regenerating unit [20], carry out regeneration of activated carbon by above-mentioned treating processes, remaining microwave exposure regenerating unit is proceeded to handle to waste water, realizes the uninterrupted continuously of a large amount of waste water handled.The same Fig. 2 of other symbols.
Embodiment
Embodiment 1
Adopt a microwave exposure regenerating unit that simulation high density Pentachlorophenol waste water and regeneration of activated carbon are handled
There are long, problem such as processing efficiency is low of treatment time in traditional Pentachlorophenol treatment process such as biological process, chemical oxidization method, metallic reducing method etc.Choosing commercially available chemical pure Pentachlorophenol pressed powder adds alkali and is mixed with the simulated wastewater that concentration is 2000mg/L, go out water concentration after requiring to handle and be lower than 200mg/L, the charcoal absorption capacity restoration is to more than 80% of its initial value, adopt the microwave exposure regenerating unit among the present invention, and place the production technique streamline, carry out charcoal absorption/microwave exposure regeneration test, step is:
The first step is feeded, and selects the reactor [10] of silica glass material for use, and gac is the ature of coal particulate state, mean particle size 5mm, effluent north Chengde distance of travel of roc gac factory provides, and loadings is 5 kilograms, 15 centimetres of quartz reactor internal diameters, 120 centimetres of height, the gac loading height is about 100 centimetres;
Second step, adsorption operations, waste water [22] is by strainer [2], lift pump [3], under meter [4], control valve [5], enter active-carbon bed [9] in the reactor [10] through shower nozzle [8], in the active-carbon bed process of flowing through, gac has been finished organic absorption in the waste water, then, flow out from water outlet [15].Flow is 88L/h, and the empty bed residence time is about 12min.Controlling out water concentration is 10% of influent concentration, i.e. 200mg/L, and closed control valve [5] when checking that water outlet reaches this concentration, absorption stops.When adopting new gac, adsorption time is about 2 hours 50 minutes, and water outlet reaches controlling concn, stops into water.When treating that charcoal bed bottom no longer there are flowing out, open microwave reactor and regenerate.This moment, active-carbon bed humidity was 55%;
The 3rd step started microwave exposure regenerating unit [20], and the microwave power of selecting for use is 64kW, and frequency is 2450MHz, and temperature rises to 800 ℃, kept 5min, and the total time of microwave exposure is 15min.Open blower fan [21] in regenerative process and after the regeneration and make magnetron [12] and active-carbon bed [9] cooling.Adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, the steam waste gas in its regenerative process is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying;
The 4th step, when active-carbon bed temperature is reduced to below 50 ℃, close blower fan, open control valve once more, carry out second and third step operation repeatedly, continuous adsorption/regeneration 7 times;
In the 5th step, regeneration effect detects, the time of break-through after each regeneration all about 3 hours, even indivedual 1 twice near 4 hours.Get that gac behind new gac and the micro wave regeneration 7 times has carried out iodine number, specific surface area and to the mensuration of Pentachlorophenol adsorption isothermal line.Discovery is behind micro wave regeneration, and iodine number increases to 1000.05mg/g by 949.37mg/g; Specific surface area is by 896.5m
2/ g increases to 937.7m
2/ g also strengthens the adsorptive power of Pentachlorophenol.Also the adsorption tower exit gas is carried out the GC/MS analysis in addition, do not had organic molecule to be detected.Illustrate that method of the present invention is fine to the regeneration of activated carbon effect.
Adopt two microwave exposure regenerating units arranged side by side to Dalian * * insecticide factory's factory effluent handles
This be an annual output * * ten thousand tons * * * insecticide factory, agricultural chemicals synthetic wastewater amount is 10 ton per days, waste water COD is 4000-10000mg/L, adopts burning method to handle in the past, the processing costs height has secondary pollution.Adopt two microwave exposure regenerating units [20] of installing side by side among the present invention to carry out charcoal absorption/microwave exposure regeneration test, step is as follows:
The first step, the sampling of wastewater analysis, from Dalian * * waste water that insecticide factory fetches, no-sundries in the water, and more transparent, waste water COD is 6784mg/L;
Second step, charging, gac in the quartz reactor [10] of two cover microwave exposure regenerating units [20] is almond base particulate state, mean particle size 3mm, effluent north Chengde distance of travel of roc gac factory provides, and loadings is 4 kilograms, 15 centimetres of quartz reactor internal diameters, highly be 120 centimetres, loading height is about 75 centimetres;
The 3rd step, carry out the absorption regeneration operation, two microwave exposure regenerating units are placed the technological process of production, start water inlet after the bug check, so waste water [22] enters each tributary under meter [4], control valve [5] through behind the strainer [2], lift pump [3], enter active-carbon bed [9] in the microwave exposure regenerating unit [20] through separately shower nozzle [8], in each active-carbon bed process of flowing through, finished organic absorption in the waste water, flowed out from water outlet [15] then.Wastewater flow is 176L/h, empty bed about 6min of the residence time, and controlling out water concentration is 10% of influent concentration.This moment, active-carbon bed humidity was 50%.During this time, regularly detect organic concentration in the water outlet, when wherein which reaches controlling concn, just close which flow control valve [5].Then, start this microwave exposure regenerating unit [20], the microwave power of selecting for use is 32kW, and frequency is 915MHz, and temperature rises to 1000 ℃, keeps 4min, and the total time of microwave exposure is 15min.Active-carbon bed intensification, exhaust, finish activation, the cooling, adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, the steam waste gas in its regenerative process is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying.After treating active-carbon bed [9] cooling, open a flow control valve [5] of this microwave exposure regenerating unit [20], carry out adsorption operations again.Reach controlling concn if find the water outlet of another microwave exposure regenerating unit [20], carry out regeneration of activated carbon by above-mentioned treating processes;
The 4th step, every covering device is all carried out second, third step operation repeatedly, adsorb continuously/regenerate 7 times;
In the 5th step, regeneration effect detects, and test-results slightly fluctuates, the time of break-through after each regeneration all about 1 hour, even indivedual 1 twice near 2 hours.Getting gac behind new charcoal and the micro wave regeneration 7 times has carried out specific surface area and the methylene blue adsorption isothermal line has been measured.Discovery is behind micro wave regeneration, though total specific surface area is by 704.4m
2/ g is reduced to 605.5m
2/ g, but the adsorptive power of methylene blue is strengthened.Analyzing its reason is that methylene blue belongs to macromole, and what its absorption was played a major role is middle bore portion, and middle hole area is by 212.7m
2/ g increases to 239.0m
2/ g.Find also simultaneously that after microwave treatment the basicity of gac increases, the pH value raises, and is the destructive result because the activated carbon surface oxy radical is decomposed.To the GC/MS analysis revealed that the adsorption tower exit gas carries out, there is not organic molecule to be detected.
Dystopy regeneration to the waste active carbon after sewage work's tertiary treatment
Take from the waste active carbon that produces after the tertiary treatment of Dalian sewage work, utilize technology of the present invention and microwave exposure regenerating unit to carry out dystopy regeneration.The concrete operations step is as follows:
The first step, the supplied materials sampling analysis: this gac is the ature of coal granulated active carbon, its mean particle size is 2mm.With this gac oven dry, measure its iodine number and specific surface area earlier, be respectively 334.18mg/g and 284.6m
2/ g;
Second step, charging: the resonator cavity loam cake [24] of opening microwave exposure regenerating unit [20], to internal diameter is 15 centimetres, highly be 2.5 kilograms of the waste active carbons of oven dry of packing in 120 centimetres the quartz reactor [10], the gac loading height is about 50 centimetres, then that loam cake is fastening, with shower nozzle [8] water spray, its humidity is adjusted to 35%;
In the 3rd step, start microwave exposure regenerating unit [20] and regenerate: power is 8kW, and frequency is 915MHz, temperature rises to 1200 ℃, keep 3min, the total time of microwave exposure is 15min, opens blower fan [21] in regenerative process and after the regeneration and makes magnetron [12] and reactor [10] cooling;
In the 4th step, regeneration effect detects: after the cooling of question response device, open the microwave resonator loam cake, with the gac stirring and evenly mixing after the regeneration in the reactor, sampling and measuring finds that iodine number and specific surface area all improve a lot, and are respectively 756.34mg/g and 687.2m
2/ g.Illustrate that this device regenerability is good, can be transported to each producer and be used for producing.
Claims (8)
1. with organic regeneration of activated carbon method in the microwave exposure disaggregating treatment absorption waste water, comprise power control, time control, humidity control, absorption saturation detection and manipulation of regeneration, it is characterized in that:
A) manipulation of regeneration of gac adopts the microwave exposure method to carry out;
B) regeneration of organic absorption and gac all is to carry out in same microwave exposure regenerating unit [20] in the waste water [22];
C) gac that is adopted is a particulate state, and its mean particle size is at 2-5mm;
D) microwave exposure disaggregating treatment regeneration of activated carbon technology is:
The first step is packed pending gac in the reactor [10] into, and its humidity is controlled at 35-55%, and the loadings of gac is the 1/3-4/5 of reactor volume;
Second step, start the magnetron [12] of microwave generator, and startup blower fan [21], the microwave frequency that is adopted in the processing is 2450MHz or 915MHz, power is 0.5-64kW, and the gac temperature is elevated to 800-1200 ℃ gradually from room temperature in the regenerative process, keeps 3-5min under this temperature, adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, microwave exposure total time is 5-15min;
In the 3rd step, shut down.Close the power supply of microwave generator earlier, treat magnetron [12] and reactor [10] cooling after, the blowing-out machine.
2. according to claim 1 with organic regeneration of activated carbon method in the microwave exposure disaggregating treatment absorption waste water, it is characterized in that: adopt the enterprising mode that goes out down when waste water [22] enters active-carbon bed [9], but, can take down the water intake mode that outes in order to become flexible service efficiency active-carbon bed and the raising gac.
3. use claim 1 described with organic regeneration of activated carbon method in the microwave exposure disaggregating treatment absorption waste water, it is characterized in that: the microwave exposure regenerating unit [20] that is adopted, it mainly is magnetron [12] by microwave generator, the reactor [10] that sieve plate [13] are equipped with in microwave resonator [11] and bottom constitutes, base of microwave resonator [23] and loam cake [24] are fastened on reactor by bolt the central position of resonator cavity, magnetron [12] then is to be evenly distributed on the outer wall of resonator cavity, top at microwave exposure regenerating unit [20] is communicated with control valve [5] and vapour outlet [16] pipeline, be provided with the shower nozzle [8] that communicates with control valve on active-carbon bed top, the bottom is provided with thief hole [14] and water outlet [15], the side is equipped with the blower fan [21] to magnetron [12] and reactor [10] cooling usefulness, adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, the gas that produces in the reactor [10], through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying.
4. adsorb organic regeneration of activated carbon method in the waste water according to claim 1 or the 3 described microwave exposure disaggregating treatment of using, it is characterized in that: microwave exposure regenerating unit [20], its microwave resonator [11] is the tubular article that the light metal alloy material with magnesium, zinc, aluminium, nickel is made into, its section is Polygons or circle, its outer side wall is provided with an equally distributed 16-32 magnetron [12], and the power of each magnetron is 0.5-2.0kW.
5. adsorb organic regeneration of activated carbon method in the waste water according to claim 1 or the 3 described microwave exposure disaggregating treatment of using, it is characterized in that: the reactor [10] in the microwave exposure regenerating unit [20], should be by saturating ripple, high temperature resistant, physical strength good and materials such as the silica glass that is easy to process and pottery are made.
6. adsorb organic regeneration of activated carbon method in the waste water according to claim 1 or the 3 described microwave exposure disaggregating treatment of using, it is characterized in that: the sieve plate [13] that be equipped with the bottom of reactor [10] is the sieve aperture of the uniform Φ of being processed with 0.3-3.0mm on its plate face.
7. application rights requires the 1 or 3 described microwave exposure disaggregating treatment of using to adsorb organic regeneration of activated carbon method and microwave exposure regenerating unit in the waste water, it is characterized in that:
A) the microwave exposure regenerating unit [20] that organic regeneration of activated carbon method in the microwave exposure disaggregating treatment absorption waste water is used, can adopt its one or more place side by side with the organic regeneration of activated carbon method of microwave exposure disaggregating treatment absorption waste water [22] process flow sheet, be equipped with alkali lye tourie [17], gas adsorption post [18] and blower fan [21], the position that replaces adsorption tower among the raw wastewater processing technological flow figure, and the gac of in reactor [10], packing on request, then, top at microwave exposure regenerating unit [20] is communicated with control valve [5] and vapour outlet [16] pipeline, the bottom is provided with thief hole [14] and water outlet [15] communicates with reuse water pipeline or network of drains, the shower nozzle [8] that is connected with water inlet control valve [5] in addition on the top of microwave exposure regenerating unit [20], and realize that gac is to finish organic absorption and microwave to the regeneration of saturated activity charcoal in same device, i.e. in-situ regeneration;
B) technical process is: in the production, waste water [22] is by strainer [2], lift pump [3], under meter [4], control valve [5], enter active-carbon bed [9] in the reactor [10] through shower nozzle [8], in the active-carbon bed process of flowing through, gac has been finished organic absorption in the waste water, then, flow out from water outlet [15], during this time, want regularly organic concentration from thief hole [14] check water outlet, when a certain goes out water concentration and reaches controlling valu, should close the water inlet control valve [5] of this microwave exposure regenerating unit [20], and start microwave exposure regenerating unit [20], gac heats up, exhaust, finish activation, cooling.Adopt K-type armoured thermocouple [7] and electronic temp indicator [6] indicated temperature, steam waste gas in its reaction reactivation process is through vapour outlet [16], alkali lye tourie [17], gas adsorption post [18], last residual exhaust [19] emptying, active-carbon bed after the regeneration cooled off through blower fan [21], open waste water control valve [5] again, again carry out adsorption operations, adsorb so repeatedly/the reclaiming process processing, at flooding velocity hour, adopt a microwave exposure regenerating unit, and can be equipped with a container for storing liquid [1], be used to store the water inlet in the microwave exposure recovery time section, when flooding quantity is big, should adopt many microwave exposure regenerating units [20], its each water inlet control valve [5] parallel arranged, control separately the device water inlet or cut off the water supply, charcoal absorption during water inlet, gac is regenerated according to said process when cutting off the water supply, when carrying out regenerative operation for one, but another or several still water flowing carry out the absorption program.
8. application rights requires the 1 or 3 described microwave exposure disaggregating treatment of using to adsorb organic regeneration of activated carbon method and microwave exposure regenerating unit in the waste water, it is characterized in that: adopt relevant industry or department to need the regenerated gac because of the adsorb organic compound attitude that reaches capacity in producing, with method proposed by the invention, in microwave exposure regenerating unit [20], carry out manipulation of regeneration separately, take out then and reuse, promptly realize dystopy regeneration, or in according to technical process method and step proposed by the invention, adopt microwave exposure regenerating unit [20], the gac for the treatment of manipulation of regeneration that to collect earlier, behind regeneration activating, take out stand-by or in production line, continue and use, regeneration re-uses, and promptly realizes in-situ regeneration.
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