CN101597102A - A kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique - Google Patents
A kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique Download PDFInfo
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- CN101597102A CN101597102A CNA2009100997404A CN200910099740A CN101597102A CN 101597102 A CN101597102 A CN 101597102A CN A2009100997404 A CNA2009100997404 A CN A2009100997404A CN 200910099740 A CN200910099740 A CN 200910099740A CN 101597102 A CN101597102 A CN 101597102A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000007885 magnetic separation Methods 0.000 title claims abstract description 15
- 238000012545 processing Methods 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000007921 spray Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000002269 spontaneous effect Effects 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000006557 surface reaction Methods 0.000 claims abstract description 4
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 229910052845 zircon Inorganic materials 0.000 claims description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 15
- 230000004043 responsiveness Effects 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005189 flocculation Methods 0.000 description 32
- 230000016615 flocculation Effects 0.000 description 31
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 239000003795 chemical substances by application Substances 0.000 description 17
- 230000008569 process Effects 0.000 description 15
- 229910052742 iron Inorganic materials 0.000 description 11
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 8
- 239000000701 coagulant Substances 0.000 description 8
- 238000011068 loading method Methods 0.000 description 8
- 238000005345 coagulation Methods 0.000 description 7
- 230000015271 coagulation Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 7
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000010802 sludge Substances 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000006004 Quartz sand Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 235000019580 granularity Nutrition 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000004062 sedimentation Methods 0.000 description 5
- 235000011149 sulphuric acid Nutrition 0.000 description 5
- 239000001117 sulphuric acid Substances 0.000 description 5
- 239000003082 abrasive agent Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 239000010865 sewage Substances 0.000 description 4
- 229920001661 Chitosan Polymers 0.000 description 3
- 238000005352 clarification Methods 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 3
- 235000020188 drinking water Nutrition 0.000 description 3
- 239000008394 flocculating agent Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 3
- MVZXTUSAYBWAAM-UHFFFAOYSA-N iron;sulfuric acid Chemical compound [Fe].OS(O)(=O)=O MVZXTUSAYBWAAM-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920002401 polyacrylamide Polymers 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 3
- 229910052683 pyrite Inorganic materials 0.000 description 3
- 239000011028 pyrite Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003818 cinder Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
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- 238000012851 eutrophication Methods 0.000 description 2
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- 230000006698 induction Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
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- 239000002244 precipitate Substances 0.000 description 2
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- 238000004065 wastewater treatment Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- ANFIEGWCRSNVFS-UHFFFAOYSA-N [Na].OCl(=O)=O Chemical compound [Na].OCl(=O)=O ANFIEGWCRSNVFS-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229940087654 iron carbonyl Drugs 0.000 description 1
- 229910000358 iron sulfate Inorganic materials 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000006249 magnetic particle Substances 0.000 description 1
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of preparation method that magnetic separates the magnetic flocculant of water technology that is used for.It is to be that 1: 1～3 magnetic and ball-milling medium place stirring ball-milling equipment to mix with mass ratio, under 40～80r/min mixing speed, the acid droplet that sprays into atomizing in the ball milling cylindrical shell is carried out the ball milling surface reaction, the per hour sour emitted dose of 1Kg magnetic is 0.1～0.2Kg, reaction 0.5～1h, temperature rises to 40 ℃～50 ℃ by the spontaneous heat release of room temperature, the sour emitted dose of per kilogram magnetic correspondence is brought up to 0.15～0.25Kg/h, continue reaction 1.5～2h, temperature rises to 65 ℃～80 ℃, stop to spray into the acid droplet of atomizing, under 80～120r/min stirring velocity, react 0.5～1h again, cooling is sieved, and obtains having the black powder shape magnetic flocculant of nucleocapsid structure.Production technique of the present invention is simple, energy consumption is low, efficient is high.This magnetic flocculant is a nucleocapsid structure, and surfactivity is high and have good magnetic responsiveness, can directly combine with the magnetic drum separator to be used for magnetic separation method water processing technique, has expanded the range of application of magnetic field in water treatment field.
Description
Technical field
The invention belongs to the environmental chemical engineering field, particularly a kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique.
Background technology
In water pollution control, the flocculation sediment process is an important key link in the various water treatment purification process, also be most widely used general, the most general cell processing technology, the flocculation agent of widespread use at present mainly contains aluminium based flocculating agent (as aluminum chloride, Tai-Ace S 150, polymerize aluminum chloride, polyaluminium sulfate etc.) and iron-based flocculating agent (as iron(ic) chloride, ferric sulfate, poly-ferric chloride, bodied ferric sulfate etc.), pH value scope is little because the aluminium based flocculating agent is used in sewage disposal, dosage is big, settling of floccus that produce is slow, and Al
3+Residual meeting in water body works the mischief to human body, and the trend of aluminum salt flocculant appears progressively substituting in the molysite flocculation agent in recent years.
Along with the aggravation of water pollution and the raising of water quality standard, traditional coagulation-settlement process highlights it and handles the deficiency that the structures floor space is big, reagent cost is high and variation water quality is big.Quicken to use on the clarification technique basis flocculation morphology theory at contact flocculation in recent years and developed the loading flocculation process, by when mixing pit adds flocculation agent, additionally adding the gravitational settling thing, realize the high-speed separation of solid-liquid with the density that improves flco as closely knit mud, quartz sand etc., it is advantageous that the suspension liquid concentration of may command flocculation reaction, its flocculation sediment residence time is short, and the shock resistance compound ability is strong and water outlet is effective.The problem that exists mainly is because the relative proportion of closely knit mud is less, can not play preferably the precipitating action that increases the weight of as the gravitational settling thing of settling pond to tiny suspended particle in the water, and the sludge yield of settling pond is big, water ratio is high, has increased the cost of follow-up sludge treatment.Quartz sand is poor as the consistency of the flco that the gravitational settling thing of clarification process mixed reaction pond and flocculation agent produce, it is comparatively loose to combine, and swirler can only reach 90% as the retrieving arrangement of quartz sand to the rate of recovery of quartz sand in the employing water, it is bigger to cause loading settling pond consumption quartz sand amount, and working cost is higher.
It is from the development of mineral magnetic separation technology that magnetic separates water technology, have technology simple, efficiently, the characteristics of non-secondary pollution, obtained significant progress in recent years.Be widely used in the wastewater treatment that steel wastewater etc. contains the ferromagnetism medium, at the water body that does not generally contain magnetic medium, someone studies by additionally adding magnetic and inoculates the magnetic kind, dosing coagulant and flocculation agent then, together form the magnetic floc sedimentation with pollutent, utilize magnetic separator to carry out magnetic with this and filter to hold back and contain the magnetic flco.As Granted publication number for the patent of invention of CN 1187274C discloses a kind of high-gradient magnetically separating handle the method and apparatus of drinking water with secondary pollution, by in drinking water with secondary pollution, adding magnetic iron powder, after the high-gradient magnetic separation unit processing, turbidity, colourity, bacterium, algae and organism in the water all there are removal preferably, have reached requirement the drinking water with secondary pollution advanced treatment.Patent of invention as U.S.Pat.NO 6099738 discloses a kind of by premagnetization strengthens dissolved organic matter by the method for coagulating agent precipitation removal ability to water body, make colloidal solid take off surely by dosing coagulant, and and then add magnetic kind and flocculation agent, after the precipitate and separate, supernatant liquor is utilized the electromagnetic filter residual contaminants floc sedimentation in the water that dams efficiently, and with the magnetic drum separator magnetic kind is reclaimed cycling and reutilization after treatment.Publication number is that the patent of invention of CN1864211A discloses magnetic is dispersed in the natural organic floculant chitosan solution and makes chitosan magnetic solution, utilize the adsorption bridging of chitosan and electrically the magnetic responsiveness of neutralization and magnetic remove the method that the water body algal tufa pollutes.In the foregoing invention patent, the magnetic kind only plays the effect that adds reprecipitation and magnetic medium is provided, the flco that coagulating agent produces can only part coated magnetic particle, and the effect of this parcel is loose, thereby the magnetic responsiveness of flco is poor, and usually, the dosage of magnetic and coagulating agent is relatively large, the processing cost height fails the magnetic responsiveness of magnetic flco and the advantage of magnetic separating apparatus are combined.
The chemical constitution of magnetite powder is with Fe
2O
3And Fe
3O
4Be main, mohs hardness 5.5～6, proportion 4.8～5.3g/cm
3, be the strongest mineral of occurring in nature magnetic, it is mainly used in ironmaking, coal separation, also can be used as the raw materials for production of ferric sulfate.At present commercially available solid iron salt flocculation agent is generally two-step approach production, and steps such as acid such as iron ore, pyrite cinder or ferrous sulfate is molten, filtration, oxidation make the liquid flocculation agent, make solid phase prod by the moisture eliminator drying again.As application number is that 200810069644.0 patent of invention discloses the method for utilizing preparing iron sulfate with iron ore, powdered iron ore is being heated under 100 ℃ of constant temperatures at the industrial sulphuric acid solution of calcining back under the 750-900 ℃ of condition and 36%-40% reacting 2-3h, then through overcooling, filter the ferrum sulfuricum oxydatum solutum that obtains.Application number is that 200610105070.9 patent of invention discloses a kind of microwave technology and is used for preparing polymeric ferric sulfate from pyrite burned slag pickling liquid technology, this technology is by microwave induced partial reduction and oxypolymerization process, with 60～70 ℃ of acid solution and pyrite cinder control reaction temperature, add oxygenant chloric acid sodium, prepared in reaction obtains liquid polymeric ferric sulfate product under microwave radiation.Because the fluid sulphuric acid iron product is not easy to transport and store, and needs further fluid sulphuric acid iron drying is obtained solid sulphuric acid iron, the drying process energy consumption is big, cost is high, simultaneously, can cause the water body jaundice after the molysite flocculation agent uses, and own its has stronger corrodibility.
Thereby, exploitation can be played the magnetic medicament of the nucleocapsid structure of the dual function that loads flocculation agent in the flocculation water treatment process and load precipitation agent, and combine the circulation of high efficiente callback magnetic nuclear part with corresponding magnetic separating apparatus and add in mixed reaction pond as the gravitational settling agent, can strengthen the flocculate and clarify process that loads, make up and load the isolating novel water treatment clarification process of flocculation magnetic, the floor space of water treatment deposition facility be can save greatly, precipitate and separate efficient and effluent quality improved.Can be widely used in that water supply purification, eutrophication river improvement, sewage work carry that mark is transformed and water treatment field such as trade effluent flocculation precipitation pretreatment.
Summary of the invention
The objective of the invention is provides a kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique in order to overcome the deficiencies in the prior art.
The preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique is: with mass ratio is that 1: 1～3 magnetic and ball-milling medium place stirring ball-milling equipment to mix, under 40～80r/min mixing speed, the acid droplet that sprays into atomizing in the ball milling cylindrical shell is reacted, the per hour sour emitted dose of 1Kg magnetic is 0.1～0.2Kg, reaction 0.5～1h, temperature rises to 40 ℃～50 ℃ by the spontaneous heat release of room temperature, the sour emitted dose of per kilogram magnetic correspondence is brought up to 0.15～0.25Kg, continue reaction 1.5～2h, temperature rises to 65 ℃～80 ℃, stop to spray into the acid droplet of atomizing, under 80～120r/min stirring velocity, react 0.5～1h again, cooling is sieved, and obtains having the black powder shape magnetic flocculant of nucleocapsid structure.
Described stirring ball-milling equipment is horizontal, cylindrical shell is by monosymmetric roller bearings on the stir shaft, be fixed on the support by dismountable tack bolt, cylindrical shell is provided with discharging flange port and acid mist injector, stir shaft connects the adjustable speed transmission mechanism, and the blade on the stir shaft is staggered bar type.Magnetic is a ferrous grade at 55%～70% magnetite powder, and granularity of magnet powder is at 380 orders～500 orders, and ball-milling medium is granulated glass sphere, agate ball or the zircon ball of 3～5mm, and acid is that mass percent concentration is 93%～98% sulfuric acid.
Technological process of the present invention is simple, and the surface reaction of " single stage method " solid-liquid prepares the solid powdery magnetic flocculant, keeps reaction by reaction self heat release and carries out, and the production process energy consumption is low, efficient is high.
Magnetic flocculant of the present invention has good Coagulation and Adsorption effect to pollutent in the water and colloidal substances do, itself is for nucleocapsid structure and have magnetic responsiveness, after the reaction tank hybrid reaction, produce the magnetic flco, can examine part by the magnetic that the magnetic drum separator reclaims in the magnetic flco, and circulation is added to the reaction tank of loading settling pond as the gravitational settling agent, to increase concentration of suspension in the flocculation tank, increase the number of times of contaminant particle effective collision, improve the density and the particle size of pollutent flco, time and reduction structures floor space to shorten flocculation sediment also can reduce added amount of chemical and working cost.The loading flocculate and clarify technology of utilization magnetic flocculant can be used for that propose mark transformation and tertiary treatment, give water treatment the municipal sewage plant, eutrophication water is administered and field such as trade effluent pre-treatment.
Description of drawings
Fig. 1 (a) is a magnetic flocculant stirring ball-milling device structure front view;
Fig. 1 (b) is a magnetic flocculant stirring ball-milling device structure vertical view.
Embodiment
The present invention is according to the essential characteristic that loads the flocculate and clarify water technology, advantage in conjunction with the magnetic separating apparatus high efficiency separation, the functional type medicament that is applicable to loading flocculation magnetic separation water treatment from exploitation is started with, proposed to adopt mechanical force and chemical surface modification and acid to modify the bonded novel process and prepared magnetic flocculant magnetic, itself utilize the heat release of material id reaction, need not extraneous heating driving a reaction, directly prepare solid magnetic flocculation agent by stirring ball-milling solid-liquid phase surface reaction " single stage method " with nucleocapsid structure, the iron a large amount of energy consumptions that are equipped with process heating and drying process of conventional solid sulphuric acid have been avoided, magnetic flocculant can play and load flocculation agent and the dual function that loads precipitation agent in the flocculation water treatment process, and combine with corresponding magnetic separating apparatus to strengthen and load coagulation process, make up and load the isolating novel water technology of coagulation magnetic.
The preparation principle of magnetic flocculant of the present invention is the mechanical force and chemical effect that selected magnetite powder is combined by ball milling mixing and sour modification of surfaces modification, because magnetite powder can produce the intensive viscous deformation in mechanical milling process, reduce the intensity of activation of Elements Diffusion, and in intergranular extruding, formed a large amount of defectives and nanometer crystal boundary and produced unsaturated link(age), free ion and electronics etc., thereby make granule surface activity improve greatly, simultaneously under the effect of strong acid atmosphere, can excite a series of surface chemical reaction of magnetite powder, the intensive Mechanochemical Effect takes place, thereby makes the magnetite powder of surface modification have stronger surfactivity and adsorptive power.Thereby change magnetic surface composition structure and electrical, enhanced granule surface dissolution and wettability are to improve Coagulation and Adsorption ability and the loading capacity to water pollutant and colloidal substances do.
Shown in Fig. 1 (a) and Fig. 1 (b), being used to prepare the stirring ball-milling equipment of magnetic flocculant is made up of stir shaft 6, step-down gear 8 and cylinder stent more than 5 major parts of cylindrical shell 10, band blade 2, cylindrical shell 10 is provided with discharge opening 11, with flange 12 sealings, cylindrical shell top centre is provided with sour atomizer 13, and cylindrical shell 10 both sides blind flanges are provided with thermopair socket 1; Blade 2 on the stir shaft is a bar type, staggered vertical distribution, and the vertical range of stirring rod end and barrel 10 is 10～15mm; Reducing motor 8 rotating speeds that link to each other with stir shaft 6 are adjustable, and rotating speed is at 40-200r/min; Cylindrical shell 10 supports by the rolling bearing 3 of stir shaft, and cylindrical shell 10 can relatively rotate with stir shaft 6, and when the material stirring reaction, cylindrical shell 10 adopts hinged bolt 9 to be fixed on the support, after reaction finishes, unscrews bolt 9, and upset cylindrical shell 10 carries out discharging.
Magnetite powder mechanical force and chemical surface modification is being prepared in the magnetic flocculant process, evenly add continuously into stirring ball-milling equipment after the concentrated acid atomizing, the dosage of acid is not enough than the amount of magnetite powder, be 1/8～1/4 of the required theoretical acid amount of magnetite powder complete reaction, thereby the magnetic carrier for preparing is a nucleocapsid structure, there is active higher transition state iron carbonyl compound in the top layer, inner magnetic nuclear structure is not destroyed, can keep the good magnetic responsiveness of magnetic carrier for preparing, in addition, the technical grade vitriol oil of concentrated acid mass concentration 93%～98% and the reaction of the solid-liquid phase surface of magnetic are spontaneous thermopositive reaction, need not to add the heating driving a reaction and carry out.
Embodiment 1:
At first in 20L volumetrical stirring ball-milling equipment barrel, add 10 kilograms of granularities about 500 orders, iron content is sampled the selected magnetite powder 55%, the compound abrasive that adds 10 kilograms of 5mm granulated glass spherees and 10 kilograms of 3mm granulated glass spherees then, start the adjustable speed transmission mechanism, low whipping speed is that 40r/min mixes 5min, begin speed with 18g/min then and evenly spray into 96% industrial sulphuric acid, after half an hour, temperature of charge progressively is raised to 45 ℃ by room temperature, the speed that adds that increases acid is to 30g/min, and improve stirring velocity to 100r/min, temperature of charge progressively rises to 65 ℃ in the cylindrical shell, continue to stop to add acid behind the stirring ball-milling reaction 1.5h, the confined reaction device, unclamp the cylindrical shell tack bolt, cylindrical shell is differential motion relatively under stir shaft drives, and the Powdered magnetic flocculant that obtains black behind the abrasive material is sieved out in discharging after half an hour behind the naturally cooling.
For turbidity is 15.2NTU, SS is the river of 45mg/L, utilize and load the flocculation sediment performance that magnetic flocculant has been examined or check by flocculation magnetic separation pilot plant test system, at mixing pit magnetic flocculation carrier dosage is 50mg/L, the PAM dosage is 1mg/L in the flocculation basin, when the magnetic nuclear CYCLIC LOADING amount that reclaims reaches 3g/L, total system has reached the ideal treatment effect, delivery turbidity is less than 1.5NTU, SS is less than 10mg/L, the vertical sedimentation tank surface load reaches 10～15m/h upflow velocity, and by permanent magnetism magnetic drum separator, the rate of recovery of magnetic nuclear can reach more than 95% in the precipitating sludge.Than traditional coagulation-settlement process, the loading flocculation magnetic separating technology of utilization magnetic flocculation carrier can be saved about 60% floor space and save running cost about 20%.
Embodiment 2:
At first in 20L volumetrical stirring ball-milling equipment barrel, add 10 kilograms of granularities about 380 orders, iron content is sampled the magnetite powder 70%, the compound abrasive that adds 20 kilograms of 5mm granulated glass spherees and 10 kilograms of 3mm granulated glass spherees then, start the adjustable speed transmission mechanism, low whipping speed is that 60r/min mixes 5min, begin speed with 20g/min then and evenly spray into 93% the vitriol oil, after 1 hour, the spontaneous heat release of temperature of charge is raised to 55 ℃ by room temperature, increase vitriolic and add speed to 30g/min, and improve stirring velocity to 120r/min, temperature of charge progressively rises to 70 ℃ in the cylindrical shell, continue to stop to add acid behind the stirring ball-milling reaction 2h, the confined reaction device, unclamp the cylindrical shell tack bolt, cylindrical shell is differential motion relatively under stir shaft drives, and the Powdered magnetic flocculant that obtains black behind the abrasive material is sieved out in discharging after half an hour behind the naturally cooling.
For turbidity at 16.8NTU, total phosphorus is the municipal wastewater treatment plant water inlet of 2.46mg/L, traditional coagulant polymeric aluminium chloride (PAC), bodied ferric sulfate (PFS) and magnetic flocculant are all under the 80mg/L dosage, opposing than test under the same hydraulics on the six coagulation test stirrers, precipitating sludge behind the PAC coagulation is canescence, the mud of PFS is pale brown look, and primary water obviously has residual light yellow of iron ion, the mud of magnetic flocculant post precipitation is grey black, and primary water does not almost have residual faint yellow of iron ion.In addition, the lowering speed of the mud liquid level that the magnetic coagulating agent produces is obviously faster than PAC and PFS, and the mud flco is closely knit, and the sludge quantity that magnetic flocculant produces obviously is less than PAC and PFS, and its sludge quantity is half of PFS approximately, 1/4th of PAC.Polymerize aluminum chloride, bodied ferric sulfate and magnetic flocculant are respectively 95.1%, 92.7% and 94.8% to the clearance of turbidity, are respectively 87.1%, 86.7% and 92.1% to the clearance of total phosphorus.
Embodiment 3:
At first in 20L volumetrical stirring ball-milling equipment barrel, add 10 kilograms of granularities about 350 orders, iron content is sampled the selected magnetite powder 69%, the compound abrasive that adds 20 kilograms of 5mm granulated glass spherees and 10 kilograms of 3mm granulated glass spherees then, start the adjustable speed transmission mechanism, low whipping speed is that 50r/min mixes 5min, begin speed with 30g/min then and evenly spray into 98% industrial sulphuric acid, after 1 hour, temperature of charge is warmed up to 60 ℃ by the spontaneous heat release of room temperature, the speed that adds that increases acid is to 40g/min, and improve stirring velocity to 120r/min, temperature of charge progressively rises to 80 ℃ in the cylindrical shell, continue to stop to add acid behind the stirring ball-milling reaction 2h, the confined reaction device, unclamp the cylindrical shell tack bolt, cylindrical shell is differential motion relatively under stir shaft drives, and the Powdered magnetic flocculant that obtains black behind the abrasive material is sieved out in discharging after half an hour behind the naturally cooling.
PH value for sanitary sewage is 7.15, COD is 422mg/L, total phosphorus is 4.78mg/L, at the magnetic flocculant dosage is 150mg/L, and coagulation stirs 3min, behind the generation magnetic flco, the flocculation agent polyacrylamide that adds 1mg/L again stirs 2min, after forming big and closely knit and having the floc sedimentation of good magnetic responsiveness, be adding under the permanent magnetic field behind the precipitation 3min of 3000 Gausses, the clearance of COD and total phosphorus is reached 81% and 92.3% respectively through magnetic induction density.
Embodiment 4:
At first in 20L volumetrical stirring ball-milling equipment barrel, add 10 kilograms of granularities about 350 orders, iron content is sampled the selected magnetite powder 68%, the compound abrasive that adds 20 kilograms of 5mm granulated glass spherees and 10 kilograms of 3mm granulated glass spherees then, start the adjustable speed transmission mechanism, low whipping speed is that 40r/min mixes 5min, begin speed with 20g/min then and evenly spray into 98% industrial sulphuric acid, after 2 hours, temperature of charge progressively is raised to 50 ℃ by the spontaneous heat release of room temperature, the speed that adds that increases acid is to 35g/min, and improve stirring velocity to 100r/min, temperature of charge progressively rises to 70 ℃ in the cylindrical shell, continue to stop to add acid behind the stirring ball-milling reaction 1h, the confined reaction device, unclamp the cylindrical shell tack bolt, cylindrical shell is differential motion relatively under stir shaft drives, and the Powdered magnetic flocculant that obtains black behind the abrasive material is sieved out in discharging after half an hour behind the naturally cooling.
For turbidity at 56NTU, total phosphorus is the simulated water sample of 8.1mg/L, the magnetic flocculant dosage is 200mg/L, after stirring 3min generation magnetic flco, the polyacrylamide coagulant aids that adds 2mg/L again stirs 2min, after forming big and closely knit and having the floc sedimentation of good magnetic responsiveness, being 5000 Gausses' permanent-magnet high gradient magnetic filter through magnetic induction density, is to reach 98% and 92.8% respectively with the interior clearance of river turbidity and total phosphorus that can make in 4 seconds in the residence time.
Than the coagulation-precipitation of conventional coagulant-filtered water treatment process, adopt magnetic flocculant and then Directly the water treatment technology of magnetic filtration can improve the efficient of water treatment procedure to a great extent, saves structures Floor space, in addition, magnetic flocculant itself can reclaim the magnetic nuclear part that accounts for its quality 50%-60% and add With recycling, reached simultaneously the sludge reduction purpose, help to save operating cost, as seen, will The water treatment technology of magnetic flocculant and magnetic separating device associating has broad prospect of application.
Claims (5)
1. preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique, it is characterized in that: with mass ratio is that 1: 1～3 magnetic and ball-milling medium place stirring ball-milling equipment to mix, under 40～80r/min mixing speed, the acid droplet that sprays into atomizing in the ball milling cylindrical shell is carried out the ball milling surface reaction, the per hour sour emitted dose of 1Kg magnetic is 0.1～0.2Kg, reaction 0.5～1h, temperature rises to 40 ℃～50 ℃ by the spontaneous heat release of room temperature, the sour emitted dose of per kilogram magnetic correspondence is brought up to 0.15～0.25Kg/h, continue reaction 1.5～2h, temperature rises to 65 ℃～80 ℃, stop to spray into the acid droplet of atomizing, under 80～120r/min stirring velocity, react 0.5～1h again, cooling, sieve, obtain having the black powder shape magnetic flocculant of nucleocapsid structure.
2. a kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique according to claim 1, it is characterized in that described stirring ball-milling equipment is horizontal, cylindrical shell is by monosymmetric roller bearings on the stir shaft, and be fixed on the support by dismountable tack bolt, cylindrical shell is provided with discharging flange port and acid mist injector, stir shaft connects the adjustable speed transmission mechanism, and the blade on the stir shaft is staggered bar type.
3. a kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique according to claim 1 is characterized in that described magnetic is a ferrous grade at 55%～70% magnetite powder, and granularity of magnet powder is at 380 orders～500 orders.
4. a kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique according to claim 1 is characterized in that described ball-milling medium is granulated glass sphere, agate ball or the zircon ball of 3～5mm.
5. a kind of preparation method who is used for the magnetic flocculant of magnetic separation method water processing technique according to claim 1 is characterized in that described acid is that mass percent concentration is 93%～98% sulfuric acid.
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