CN106336067A - Domestic wastewater purifying treatment method - Google Patents
Domestic wastewater purifying treatment method Download PDFInfo
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Abstract
The invention relates to the water purification field, and discloses a domestic wastewater purifying treatment method. The method comprises the following steps: 1, allowing domestic wastewater to stand, and allowing the domestic water to go through a filter screen in order to remove granular impurities; 2, adding beta-cyclodextrin magnetic particles accounting for 1-2% of the mass of the domestic wastewater to the domestic wastewater obtained in step 1, allowing the obtained domestic wastewater to stand for 8-12 h, and recovering the beta-cyclodextrin magnetic particles by using magnet; 3, loading the domestic wastewater obtained in step 2 to a foam separation tower, carrying out bubbling treatment, separating a foam layer, and taking the obtained lower layer domestic wastewater; and 4, introducing the domestic wastewater obtained in step 3 into an oil-water separation tower, and carrying out oil-water separation, wherein the oil-water separation tower adopts composite aerogel as a filler. The method has the advantages of good filtering effect on the granular impurities, protein substances, oil stains and heavy metals, no recovery of a purifying agent, and no secondary pollution to water.
Description
Technical field
The present invention relates to Water warfare field, more particularly, to a kind of sanitary wastewater purifying treatment method.
Background technology
With the fast development of China's economy, at present, all in cumulative year after year, the wastewater flow rate discharged therewith is also being continuously increased domestic consumption.Due to the complexity of domestic water, in these sanitary wastewaters, mostly all contain the objectionable impurities such as graininess impurity, protein matter, greasy dirt, heavy metal ion.In order to protect increasingly destroyed environment it is necessary to purified treatment is carried out to these sanitary wastewaters.Existing sanitary wastewater purification method mainly has flocculence, physisorphtion, microbial degradation method etc..The application of wherein flocculence is relatively broad.
Chinese patent as Application No. 201310388675.3 discloses a kind of processing method of heavy metal containing sewage, comprising: (a) heavy metal containing sewage is introduced in sewage reaction tank；B () adds appropriate ion sedimentation agent to be settled in heavy metal containing sewage；C () adds appropriate flocculant to the heavy metal containing sewage after sedimentation and carries out efficient flocculating；D () heavy metal containing sewage to after add flocculant adds appropriate flocculation aid；E () will add the heavy metal containing sewage quiescent setting certain time after flocculation aid；Flocculation group f () will be precipitated after separates from heavy metal containing sewage.This invented technology flow process is simple, and medicament stock is easy to get, with low cost, and processing procedure does not produce new " three wastes ", obvious processing effect.
Chinese patent as Application No. 201310366271.4 discloses a kind of oily water water scavengine agent and preparation method thereof, this greasy dirt water scavengine agent contains following component: 15～30 parts of aluminium polychloride in terms of mass parts, 5～12 parts of PAMA, 7～16 parts of lime, 3～10 parts of sodium hypochlorite, 3～8 parts of sodium lignin sulfonate, 3～7 parts of diammonium hydrogen phosphate, 5～15 parts of benzene sulfonic acid sodium salt.The sanitary wastewater cleanser that this invention provides has very strong flocculation, and has good bactericidal effect.
Chinese patent as Application No. 201410380852.8 discloses a kind of condensed oil sewage and processes coagulant, include following components in percentage by weight: 15.0～25.0% aluminium polychloride, 5.0～10.0% poly- silicon zinc sulfate, 0.5～1.0% PDDA and 5.0～10.0% 3.0g polyamide-amide.Its preparation method is: by weight percentage, first aluminium polychloride and poly- silicon zinc sulfate are added to the water, dissolving adds PDDA and 3.0g polyamide-amide completely afterwards, stirs, adjust ph value to 3.0～5.0, obtain thick sanitary wastewater and process coagulant.Its advantage is: consumption is few, cheap, and is applied to the handling process of multifunctional rotary flow reactor；Have rp demulsification and water purification effect concurrently, to Heavy Oil High Temperature sewage, there is good clean-up effect；Its preparation method is simple.
Although particulate contaminant, protein matter, greasy dirt, heavy metal ion etc. can be removed from water by method to a certain extent that purify sanitary wastewater above by flocculence, but its detersive efficiency is relatively low, after flocculation, flocculent substance still easily remains in water body after filtration；And need when purifying to add in water various be dissolved in water itself and the chemical reagent that is not easily recycled, easily cause secondary pollution while decontamination.
Content of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of good to particulate contaminant, protein matter, greasy dirt, heavy metal filter efficiency, cleanser need not be reclaimed, and water body will not be caused with the sanitary wastewater purifying treatment method of secondary pollution.
The concrete technical scheme of the present invention is: a kind of sanitary wastewater purifying treatment method, comprises the following steps:
1) sanitary wastewater is stood, and particulate contamination is removed by filter screen.
First to sanitary wastewater standing, filter；On the one hand particulate contamination can be removed to purify water, on the other hand the removal being capable of particulate contamination is conducive to the foam fraction factor in subsequent step and water-oil separating: if there being the presence of a large amount of granule foreigns in foam fraction factor, the foaming characteristic of sanitary wastewater can be affected, thus leading to not the emulsifying agent in sanitary wastewater be carried out separate；And in water-oil separating, if sanitary wastewater has a large amount of granule foreigns, filler can be resulted in blockage, not only affect the oil absorbing effect of filler, and the permeability of filler can be reduced, lead to water speed to reduce.
2) add the beta-schardinger dextrin magnetic particle of sanitary wastewater quality 1-2% in the sanitary wastewater to after process through step 1), after standing 8-12h, with magnet, beta-schardinger dextrin magnetic particle is reclaimed.
Usually contain substantial amounts of protein matter in sanitary wastewater, the flocculants such as shitosan, aluminium hydroxide is usually used it is flocculated, but flocculent substance is not only difficult to carry out separating from water body, and separating rate is very slow, has had a strong impact on Water warfare efficiency.The present invention is adsorbed to protein matter from beta-schardinger dextrin magnetic particle, and beta-schardinger dextrin has end group hydrophilic and hydrophobic internal cavities, has good adsorptivity and adsorbance to protein matter.And with beta-schardinger dextrin, magnetic particle is wrapped up, just can carry out adsorption recovery to it with magnet, advantages of good adsorption effect, the rate of recovery is high, will not cause secondary pollution to water body.
3) by through step 2) process after sanitary wastewater be loaded in foam separating tower and carry out bubbling process, and separate froth bed, take off a layer sanitary wastewater.
Due to usually containing emulsifying agents various in a large number in sanitary wastewater, these have in the long-time presence of emulsifying agent and water body of surface-active, sanitary wastewater is made to define relatively stable oil-in-water emulsion, if directly the filler in practical water-oil separating tower carries out oil suction to it, due to profit one, adsorption efficiency is relatively low.In order to solve this technical problem, the present invention is after removing particulate contamination to sanitary wastewater, then carries out foam fraction factor to it.Because emulsifying agent has very strong surface-active, after liquid produces bubble, emulsifying agent can concentrate on gas-liquid interface (foam surface), if being collected, can effectively reduce the content of emulsifying agent in sanitary wastewater to foam, thus the emulsifiability of sanitary wastewater substantially reduces, oil-in-water system is disintegrated, oil phase is separated from the water, finally reuses filler and carries out oil suction to sanitary wastewater, purification efficiency is largely increased.
3) by through step 2) process after sanitary wastewater be passed through in water-oil separating tower and carry out water-oil separating；Described water-oil separating tower adopts composite aerogel as filler.
Water-oil separating is carried out to the sanitary wastewater after emulsion breaker, because water-oil separating degree is high, the method using physical absorption carries out oil suction, not only will not cause secondary pollution to water body, and good purification, efficiency high.And above-mentioned composite aerogel heavy metal ion also has very strong adsorption capacity.
The preparation process of described composite aerogel includes: butyl titanate, CNT, brucite fiber, carboxylated nano-crystal cellulose, absolute ethyl alcohol, toluene 1:0.1-0.2:0.1-0.2:0.2-0.4:10-30:0.01-0.03 in mass ratio is mixed, obtained solution a；Absolute ethyl alcohol, the glacial acetic acid of 0.5-1.5mol/l are mixed with water 10-20:4-6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50-60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；Sol solutionses are obtained after stirring 1-2h；By sol solutionses aging 24-48h at room temperature, then add absolute ethyl alcohol in sol solutionses and carry out solvent displacement 24-48h, then add n-hexane again in sol solutionses and carry out solvent displacement 24-48h, it is separated off n-hexane, obtain wet gel, with the mixed solution of organo-silicon compound and n-hexane, hydrophobically modified is carried out to wet gel；Eventually pass and composite aerogel after being dried, is obtained.
Aeroge is the minimum material of the density that finds in the world so far, and has the porosity of superelevation, wherein being most widely used of aerosil.The preparation process of aeroge is generally divided into colloidal sol preparation, gel preparation and drying steps.After prepared gel, contain a large amount of holes and three-dimensional net structure in gel, under gel state, the filling due to there being liquid supports, and its structure is relatively stable.But during gel drying is for aeroge, due to the loss of liquid, and the frame strength of gel is not high, easily caves in it is not easy to shape, after leading to become aeroge, its porosity declines.
The composite aerogel of present invention preparation, using CNT, brucite fiber, carboxylated nano-crystal cellulose etc. is as matrix material, CNT is the tubular material of nano-scale, brucite fiber also has nano-scale, carboxylated nano-crystal cellulose is nano-scale crystal fibre element, after above-mentioned material and titanium dioxide carry out being combined, three-dimensional net structure can be played a supporting role under gel state, can be cross-linked with each other between carboxylated nano-crystal cellulose, in dry run, its structure is not caved in, ensure that porosity, and CNT, brucite fiber all has heat-resisting quantity, in dry run, stability is strong, after being prepared into composite aerogel simultaneously, the intensity of aeroge can be significantly increased.In addition, because CNT itself also has hollow structure, after being combined with titanium dioxide, the network-like cross-linked structure of complexity can be formed, the porosity of composite aerogel can't excessively be reduced, and because the hole of CNT is specific to self structure, be not to pass through crosslinked gained the later stage, therefore stability is higher, and intensity is higher.
Carboxylated nano-crystal cellulose in addition to above-mentioned effect, relatively adsorbed although heavy metal also can be spent by force, but ability is weaker by the oil absorption due to aeroge.And in sanitary wastewater, contain plurality of heavy metal.Carboxylated nano-crystal cellulose has excellent heavy metal adsorption, the shortcoming being capable of reinforcement aeroge.
Because common aerogel material is that have preferably hydrophilic, accordingly act as can not playing a role very well during oil absorption material, therefore the present invention has carried out hydrophobically modified to aerogel composite, it is possible to increase efficiency of deoiling.
After composite aerogel filler oil suction reaches saturation state, because titanium dioxide has efficient photocatalytic, only ultraviolet light irradiation need to be carried out it becomes possible to degrade to oil to composite aerogel filler.
Further, the preparation method of described beta-schardinger dextrin magnetic particle is: the beta-schardinger dextrin of 1.5-2 weight portion is added in the container filling 100 weight portion water, forms beta-schardinger dextrin solution, and leads to nitrogen 15-25min at 55-65 DEG C；By 0.5-0.55 weight portion fecl3·6h2O and 0.19-0.20 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammoniacal liquor ph, after reaction 10-15min, generate beta-schardinger dextrin magnetic particle, hold beta-schardinger dextrin magnetic particle with magnet across chamber wall, after pouring out liquid, after beta-schardinger dextrin magnetic particle is cleaned, carry out vacuum freeze drying standby.
The present invention just adds beta-schardinger dextrin during the generation of Fe 3 O 4 magnetic particle, and so, beta-schardinger dextrin just can be crosslinked with it in Fe 3 O 4 magnetic particle generating process, and parcel fastness is high, difficult for drop-off, will not cause secondary pollution to water body.
Further, when step 3) carries out bubbling, air-blowing is carried out to the bottom of foam separating tower, from the collected overhead foam of foam separating tower；Wherein, the water corresponding to every cubic metre, blow rate is 20-40l/min.Carry out foam fraction factor with this understanding, bubble effect is good, and separating degree is higher.
Further, when step 3) carries out bubbling, sanitary wastewater water temperature is 25-35 DEG C, and in foam separating tower, the loading height of sanitary wastewater and the internal diameter of foam separating tower ratio is for 10-20:1.Carry out foam fraction factor with this understanding, bubble effect is good, and separating degree is higher.
Further, in step 4), flow velocity in the filler that the every square metre cross-section of water-oil separating tower is amassed for the sanitary wastewater is 800-1200l/min.
Further, described carboxylated nano-crystal cellulose preparation method is: the microcrystalline cellulose of 1 weight portion is mixed for 0.5-1.5mol/l ammonium persulfate solution with 40-45 weight portion concentration, after dipping 10-20min, mixed solution is carried out with ultrasonic agitation and processes 25-35min, obtain suspension, wherein ultrasonic frequency is 45-55khz, and temperature is 45-55 DEG C；Centrifugal treating is carried out to described suspension, and the solid obtaining is washed till neutrality, it is to dissolve in 1mol/l citric acid solution that solid is added to 30-40 weight portion concentration, and react 150-200min under the conditions of above-mentioned ultrasonic agitation, again to product after centrifugation, washing, dissolving, dialysis, prepared carboxylated nano-crystal cellulose.
The carboxylated nano-crystal cellulose that said method is obtained has preferable bridging property, and the high adsorption capacity of heavy metal.
Further, during preparing composite aerogel, when solution a is added drop-wise in solution b, add the sodium acid carbonate of 0.02-0.03 times that quality is solution a in solution a simultaneously.The effect of sodium acid carbonate is as toluene, it is as pore-foaming agent, but both pore principles are different, cooperate the different types of hole that can make, hole containing three kinds of different origins therefore in this composite aerogel: the hole that hole that aeroge is cross-linked to form, the tubulus of CNT itself, pore-foaming agent are made, these three pore-sizes differ, therefore, it is possible to form difference in size alienation, for different greasy dirts, respective adsorption efficiency is also different, therefore, it is possible to improve the overall oil absorbing effect of composite aerogel.
Further, described CNT, brucite fiber are respectively through activation process: CNT or brucite fiber be impregnated in the 10wt% hydrochloric acid solution of 150-250 times of quality, and carry out water-bath vibration 1-2h at a temperature of 50-60 DEG C；After CNT or brucite fiber are taken out and clean, calcine 2-5h at a temperature of 400-500 DEG C.CNT after overactivation, brucite fiber not only have higher intensity, and CNT has more preferable adsorption activity.The particle diameter of described CNT is 400-800nm.
Further, solution b is to the rate of addition 0.5-1.5ml/s of solution a.Need the strict rate of addition controlling solution b, under this speed, form the network-like structure that colloidal sol can form high-crosslinking-degree, improve intensity on the premise of ensureing porosity.
Further, during hydrophobically modified, in the mixed solution of described organo-silicon compound and n-hexane, organo-silicon compound are 1-2:5 with the volume ratio of n-hexane, and organo-silicon compound are 100:10-20 with the mixed solution of n-hexane and the mass ratio of wet gel；Modification temperature is 50-60 DEG C, modification time 36-50h.Described organo-silicon compound are selected from HMDO, HMDS, HMDS, MTMS, trim,ethylchlorosilane.
It is compared with the prior art, the invention has the beneficial effects as follows: the inventive method is good to particulate contaminant, protein matter, greasy dirt, heavy metal filter efficiency, cleanser need not be reclaimed, and will not cause secondary pollution to water body.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of sanitary wastewater purifying treatment method, comprises the following steps:
1) sanitary wastewater is stood, and particulate contamination is removed by filter screen.
2) add the beta-schardinger dextrin magnetic particle of sanitary wastewater quality 1.5% in the sanitary wastewater to after process through step 1), after standing 10h, with magnet, beta-schardinger dextrin magnetic particle is reclaimed.
The preparation method of described beta-schardinger dextrin magnetic particle is: the beta-schardinger dextrin of 1.75 weight portions is added in the container filling 100 weight portion water, forms beta-schardinger dextrin solution, and leads to nitrogen 20min at 60 DEG C；By 0.525 weight portion fecl3·6h2O and 0.195 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammoniacal liquor ph, after reaction 12.5min, generate beta-schardinger dextrin magnetic particle, hold beta-schardinger dextrin magnetic particle with magnet across chamber wall, after pouring out liquid, after beta-schardinger dextrin magnetic particle is cleaned, carry out vacuum freeze drying standby.
3) by through step 2) process after sanitary wastewater be loaded in foam separating tower, air-blowing is carried out to the bottom of foam separating tower, from the top separation foam of foam separating tower, takes off a layer sanitary wastewater.Wherein, the water corresponding to every cubic metre, blow rate is 30l/min.Sanitary wastewater water temperature is 30 DEG C, and in foam separating tower, the loading height of sanitary wastewater and the internal diameter of foam separating tower ratio is for 15:1.
4) sanitary wastewater after processing through step 3) is passed through in water-oil separating tower and carries out water-oil separating.Described water-oil separating tower adopts composite aerogel as filler.Wherein, flow velocity in the filler that the every square metre cross-section of water-oil separating tower is amassed for the sanitary wastewater is 1000l/min.
The preparation process of described composite aerogel includes:
The preparation of carboxylated nano-crystal cellulose: the microcrystalline cellulose of 1 weight portion is mixed for 1mol/l ammonium persulfate solution with 42.5 weight portion concentration, after dipping 15min, mixed solution is carried out with ultrasonic agitation and processes 30min, obtain suspension, wherein ultrasonic frequency is 50khz, and temperature is 50 DEG C；Centrifugal treating is carried out to described suspension, and the solid obtaining is washed till neutrality, it is to dissolve in 1mol/l citric acid solution that solid is added to 35 weight portion concentration, and react 175min under the conditions of above-mentioned ultrasonic agitation, again to product after centrifugation, washing, dissolving, dialysis, prepared carboxylated nano-crystal cellulose.
Butyl titanate, CNT, brucite fiber, carboxylated nano-crystal cellulose, absolute ethyl alcohol, toluene 1:0.15:0.15:0.3:20:0.02 in mass ratio are mixed, obtained solution a；Absolute ethyl alcohol, the glacial acetic acid of 1mol/l are mixed with water 15:5:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 55 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality with the speed of 1ml/s；Add the sodium acid carbonate of 0.025 times that quality is solution a simultaneously in solution a, after stirring 1.5h, sol solutionses are obtained.The particle diameter of described CNT is 400-800nm
By sol solutionses aging 36h at room temperature, in sol solutionses, then add absolute ethyl alcohol carry out solvent displacement 36h, then add n-hexane again in sol solutionses and carry out solvent displacement 36h, be separated off n-hexane, obtain wet gel.With the mixed solution of organo-silicon compound and n-hexane, hydrophobically modified is carried out to wet gel, in the mixed solution of described organo-silicon compound and n-hexane, organo-silicon compound are 1.5:5 with the volume ratio of n-hexane, and organo-silicon compound are 100:15 with the mixed solution of n-hexane and the mass ratio of wet gel；Modification temperature is 55 DEG C, modification time 43h.Described organo-silicon compound are HMDO.
Eventually pass and composite aerogel after being dried, is obtained.
Embodiment 2
A kind of sanitary wastewater purifying treatment method, comprises the following steps:
1) sanitary wastewater is stood, and particulate contamination is removed by filter screen.
2) add the beta-schardinger dextrin magnetic particle of sanitary wastewater quality 1% in the sanitary wastewater to after process through step 1), after standing 12h, with magnet, beta-schardinger dextrin magnetic particle is reclaimed.
The preparation method of described beta-schardinger dextrin magnetic particle is: the beta-schardinger dextrin of 1.5 weight portions is added in the container filling 100 weight portion water, forms beta-schardinger dextrin solution, and leads to nitrogen 25min at 55 DEG C；By 0.5 weight portion fecl3·6h2O and 0.19 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammoniacal liquor ph, after reaction 10min, generate beta-schardinger dextrin magnetic particle, hold beta-schardinger dextrin magnetic particle with magnet across chamber wall, after pouring out liquid, after beta-schardinger dextrin magnetic particle is cleaned, carry out vacuum freeze drying standby.
3) by through step 2) process after sanitary wastewater be loaded in foam separating tower, air-blowing is carried out to the bottom of foam separating tower, from the top separation foam of foam separating tower, takes off a layer sanitary wastewater.Wherein, the water corresponding to every cubic metre, blow rate is 20l/min.Sanitary wastewater water temperature is 25 DEG C, and in foam separating tower, the loading height of sanitary wastewater and the internal diameter of foam separating tower ratio is for 10:1.
4) sanitary wastewater after processing through step 3) is passed through in water-oil separating tower and carries out water-oil separating.Described water-oil separating tower adopts composite aerogel as filler.Wherein, flow velocity in the filler that the every square metre cross-section of water-oil separating tower is amassed for the sanitary wastewater is 800l/min.
The preparation process of described composite aerogel includes:
The preparation of carboxylated nano-crystal cellulose: the microcrystalline cellulose of 1 weight portion is mixed for 0. mol/l ammonium persulfate solution with 40 weight portion concentration, after dipping 10min, mixed solution is carried out with ultrasonic agitation and processes 25min, obtain suspension, wherein ultrasonic frequency is 45khz, and temperature is 55 DEG C；Centrifugal treating is carried out to described suspension, and the solid obtaining is washed till neutrality, it is to dissolve in 1mol/l citric acid solution that solid is added to 30 weight portion concentration, and react 150min under the conditions of above-mentioned ultrasonic agitation, again to product after centrifugation, washing, dissolving, dialysis, prepared carboxylated nano-crystal cellulose.
CNT, brucite fiber be impregnated in respectively in the 10wt% hydrochloric acid solution of 200 times of quality, and carry out water-bath vibration 1.5h at a temperature of 55 DEG C；After CNT, brucite fiber being taken out respectively and cleaning, calcine 3.5h at a temperature of 450 DEG C.The particle diameter of described CNT is 400-800nm
Butyl titanate, CNT, brucite fiber, carboxylated nano-crystal cellulose, absolute ethyl alcohol, toluene 1:0.1:0.1:0.2:10:0.01 in mass ratio are mixed, obtained solution a；Absolute ethyl alcohol, the glacial acetic acid of 0.5mol/l are mixed with water 10:4:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality with the speed of 0.5ml/s；Add the sodium acid carbonate of 0.02 times that quality is solution a simultaneously in solution a, after stirring 1h, sol solutionses are obtained.
By sol solutionses aging 24h at room temperature, in sol solutionses, then add absolute ethyl alcohol carry out solvent displacement 24h, then add n-hexane again in sol solutionses and carry out solvent displacement 24h, be separated off n-hexane, obtain wet gel.With the mixed solution of organo-silicon compound and n-hexane, hydrophobically modified is carried out to wet gel, in the mixed solution of described organo-silicon compound and n-hexane, organo-silicon compound are 1:5 with the volume ratio of n-hexane, and organo-silicon compound are 100:10 with the mixed solution of n-hexane and the mass ratio of wet gel；Modification temperature is 50 DEG C, modification time 50h.Described organo-silicon compound are HMDS.
Eventually pass and composite aerogel after being dried, is obtained.
Embodiment 3
A kind of sanitary wastewater purifying treatment method, comprises the following steps:
1) sanitary wastewater is stood, and particulate contamination is removed by filter screen.
2) add the beta-schardinger dextrin magnetic particle of sanitary wastewater quality 2% in the sanitary wastewater to after process through step 1), after standing 12h, with magnet, beta-schardinger dextrin magnetic particle is reclaimed.
The preparation method of described beta-schardinger dextrin magnetic particle is: the beta-schardinger dextrin of 2 weight portions is added in the container filling 100 weight portion water, forms beta-schardinger dextrin solution, and leads to nitrogen 15min at 65 DEG C；By 0.55 weight portion fecl3·6h2O and 0.20 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammoniacal liquor ph, after reaction 15min, generate beta-schardinger dextrin magnetic particle, hold beta-schardinger dextrin magnetic particle with magnet across chamber wall, after pouring out liquid, after beta-schardinger dextrin magnetic particle is cleaned, carry out vacuum freeze drying standby.
3) by through step 2) process after sanitary wastewater be loaded in foam separating tower, air-blowing is carried out to the bottom of foam separating tower, from the top separation foam of foam separating tower, takes off a layer sanitary wastewater.Wherein, the water corresponding to every cubic metre, blow rate is 40l/min.Sanitary wastewater water temperature is 35 DEG C, and in foam separating tower, the loading height of sanitary wastewater and the internal diameter of foam separating tower ratio is for 20:1.
4) sanitary wastewater after processing through step 3) is passed through in water-oil separating tower and carries out water-oil separating.Described water-oil separating tower adopts composite aerogel as filler.Wherein, flow velocity in the filler that the every square metre cross-section of water-oil separating tower is amassed for the sanitary wastewater is 1200l/min.
The preparation process of described composite aerogel includes:
The preparation of carboxylated nano-crystal cellulose: the microcrystalline cellulose of 1 weight portion is mixed for 1.5mol/l ammonium persulfate solution with 45 weight portion concentration, after dipping 20min, mixed solution is carried out with ultrasonic agitation and processes 35min, obtain suspension, wherein ultrasonic frequency is 55khz, and temperature is 45 DEG C；Centrifugal treating is carried out to described suspension, and the solid obtaining is washed till neutrality, it is to dissolve in 1mol/l citric acid solution that solid is added to 40 weight portion concentration, and react 200min under the conditions of above-mentioned ultrasonic agitation, again to product after centrifugation, washing, dissolving, dialysis, prepared carboxylated nano-crystal cellulose.
CNT, brucite fiber be impregnated in respectively in the 10wt% hydrochloric acid solution of 250 times of quality, and carry out water-bath vibration 1h at a temperature of 60 DEG C；After CNT, brucite fiber being taken out respectively and cleaning, calcine 2h at a temperature of 500 DEG C.The particle diameter of described CNT is 400-800nm
Butyl titanate, CNT, brucite fiber, carboxylated nano-crystal cellulose, absolute ethyl alcohol, toluene 1:0.2:0.2:0.4:30:0.03 in mass ratio are mixed, obtained solution a；Absolute ethyl alcohol, the glacial acetic acid of 1.5mol/l are mixed with water 20:6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality with the speed of 1.5ml/s；Add the sodium acid carbonate of 0.03 times that quality is solution a simultaneously in solution a, after stirring 2h, sol solutionses are obtained.
By sol solutionses aging 48h at room temperature, in sol solutionses, then add absolute ethyl alcohol carry out solvent displacement 48h, then add n-hexane again in sol solutionses and carry out solvent displacement 48h, be separated off n-hexane, obtain wet gel.With the mixed solution of organo-silicon compound and n-hexane, hydrophobically modified is carried out to wet gel, in the mixed solution of described organo-silicon compound and n-hexane, organo-silicon compound are 2:5 with the volume ratio of n-hexane, and organo-silicon compound are 100:20 with the mixed solution of n-hexane and the mass ratio of wet gel；Modification temperature is 60 DEG C, modification time 36h.Described organo-silicon compound are MTMS.
Eventually pass and composite aerogel after being dried, is obtained.
The composite aerogel filler that embodiment 1-3 is obtained, its porosity can reach 92-95%, and specific surface area reaches 500-600 m2/ g, density reaches 3.5-4.2kg/m3.After embodiment 1-3 methods described purifies to sanitary wastewater, after purification, water quality oil content can control within 2.8mg/l, can reach more than 95% to the adsorption rate of protein matter, the adsorption rate of heavy metal ion can reach more than 90%.
Raw materials used in the present invention, equipment, unless otherwise noted, is conventional raw material, the equipment of this area；Method therefor in the present invention, unless otherwise noted, is the conventional method of this area.
The above, be only presently preferred embodiments of the present invention, not the present invention imposed any restrictions, every any simple modification, change and equivalent transformation substantially above example made according to the technology of the present invention, all still falls within the protection domain of technical solution of the present invention.
Claims (10)
1. a kind of sanitary wastewater purifying treatment method is it is characterised in that comprise the following steps:
1) sanitary wastewater is stood, and particulate contamination is removed by filter screen；
2) add the beta-schardinger dextrin magnetic particle of sanitary wastewater quality 1-2% in the sanitary wastewater to after process through step 1), after standing 8-12h, with magnet, beta-schardinger dextrin magnetic particle is reclaimed；
3) by through step 2) process after sanitary wastewater be loaded in foam separating tower and carry out bubbling process, and separate froth bed, take off a layer sanitary wastewater；
4) sanitary wastewater after processing through step 3) is passed through in water-oil separating tower and carries out water-oil separating；Described water-oil separating tower adopts composite aerogel as filler；
The preparation process of described composite aerogel includes: butyl titanate, CNT, brucite fiber, carboxylated nano-crystal cellulose, absolute ethyl alcohol, toluene 1:0.1-0.2:0.1-0.2:0.2-0.4:10-30:0.01-0.03 in mass ratio is mixed, obtained solution a；Absolute ethyl alcohol, the glacial acetic acid of 0.5-1.5mol/l are mixed with water 10-20:4-6:1 in mass ratio, obtained solution b；Supersonic oscillations process is carried out at 50-60 DEG C to solution a, solution b is added drop-wise in the solution a of 2 times of quality；Sol solutionses are obtained after stirring 1-2h；By sol solutionses aging 24-48h at room temperature, then add absolute ethyl alcohol in sol solutionses and carry out solvent displacement 24-48h, then add n-hexane again in sol solutionses and carry out solvent displacement 24-48h, it is separated off n-hexane, obtain wet gel, with the mixed solution of organo-silicon compound and n-hexane, hydrophobically modified is carried out to wet gel；Eventually pass and composite aerogel after being dried, is obtained.
2. a kind of sanitary wastewater purifying treatment method as claimed in claim 1, it is characterized in that, step 2) described in the preparation method of beta-schardinger dextrin magnetic particle be: the beta-schardinger dextrin of 1.5-2 weight portion is added in the container filling 100 weight portion water, form beta-schardinger dextrin solution, and lead to nitrogen 15-25min at 55-65 DEG C；By 0.5-0.55 weight portion fecl3·6h2O and 0.19-0.20 weight portion fecl2·4h2O is dissolved in the water of 10 weight portions, it is added to after logical nitrogen in described container, it is adjusted to 9-10 with ammoniacal liquor ph, after reaction 10-15min, generate beta-schardinger dextrin magnetic particle, hold beta-schardinger dextrin magnetic particle with magnet across chamber wall, after pouring out liquid, after beta-schardinger dextrin magnetic particle is cleaned, carry out vacuum freeze drying standby.
3. as claimed in claim 1 a kind of sanitary wastewater purifying treatment method it is characterised in that when step 3) carries out bubbling, air-blowing is carried out to the bottom of foam separating tower, from the collected overhead foam of foam separating tower；Wherein, the water corresponding to every cubic metre, blow rate is 20-40l/min.
4. as claimed in claim 3 a kind of sanitary wastewater purifying treatment method it is characterised in that when step 3) carries out bubbling, sanitary wastewater water temperature is 25-35 DEG C, in foam separating tower, the loading height of sanitary wastewater and the internal diameter of foam separating tower ratio is for 10-20:1.
5. as claimed in claim 1 a kind of sanitary wastewater purifying treatment method it is characterised in that in step 4) sanitary wastewater the every square metre cross-section of water-oil separating tower amass filler in flow velocity be 800-1200l/min.
6. a kind of sanitary wastewater purifying treatment method as claimed in claim 1, it is characterized in that, described carboxylated nano-crystal cellulose preparation method is: the microcrystalline cellulose of 1 weight portion is mixed for 0.5-1.5mol/l ammonium persulfate solution with 40-45 weight portion concentration, after dipping 10-20min, mixed solution is carried out with ultrasonic agitation and processes 25-35min, obtain suspension, wherein ultrasonic frequency is 45-55khz, and temperature is 45-55 DEG C；Centrifugal treating is carried out to described suspension, and the solid obtaining is washed till neutrality, it is to dissolve in 1mol/l citric acid solution that solid is added to 30-40 weight portion concentration, and react 150-200min under the conditions of above-mentioned ultrasonic agitation, again to product after centrifugation, washing, dissolving, dialysis, prepared carboxylated nano-crystal cellulose.
7. a kind of sanitary wastewater purifying treatment method it is characterised in that during preparing composite aerogel, when solution a is added drop-wise in solution b, adds the sodium acid carbonate of 0.02-0.03 times that quality is solution a in solution a simultaneously as claimed in claim 1.
8. a kind of sanitary wastewater purifying treatment method as claimed in claim 1, it is characterized in that, described CNT, brucite fiber are respectively through activation process: CNT or brucite fiber be impregnated in the 10wt% hydrochloric acid solution of 150-250 times of quality, and carry out water-bath vibration 1-2h at a temperature of 50-60 DEG C；After CNT or brucite fiber are taken out and clean, calcine 2-5h at a temperature of 400-500 DEG C；The particle diameter of described CNT is 400-800nm.
9. as claimed in claim 1 a kind of sanitary wastewater purifying treatment method it is characterised in that rate of addition 0.5-1.5ml/s from solution b to solution a.
10. a kind of sanitary wastewater purifying treatment method as claimed in claim 1, it is characterized in that, during hydrophobically modified, in the mixed solution of described organo-silicon compound and n-hexane, organo-silicon compound are 1-2:5 with the volume ratio of n-hexane, and organo-silicon compound are 100:10-20 with the mixed solution of n-hexane and the mass ratio of wet gel；Modification temperature is 50-60 DEG C, modification time 36-50h；Described organo-silicon compound are selected from HMDO, HMDS, HMDS, MTMS, trim,ethylchlorosilane.
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