CN118045599A - Preparation method of modified micro-sand and chemical wastewater hardness-reducing TOC-removing and phosphorus-removing treatment method - Google Patents
Preparation method of modified micro-sand and chemical wastewater hardness-reducing TOC-removing and phosphorus-removing treatment method Download PDFInfo
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- 239000004576 sand Substances 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000002351 wastewater Substances 0.000 title claims abstract description 38
- 239000000126 substance Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000003245 coal Substances 0.000 claims abstract description 36
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 24
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 claims abstract description 23
- 239000003818 cinder Substances 0.000 claims abstract description 17
- 230000005484 gravity Effects 0.000 claims abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 13
- 239000011574 phosphorus Substances 0.000 claims abstract description 13
- 238000011068 loading method Methods 0.000 claims description 96
- 239000010802 sludge Substances 0.000 claims description 57
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- 238000005345 coagulation Methods 0.000 claims description 44
- 230000015271 coagulation Effects 0.000 claims description 44
- 239000003795 chemical substances by application Substances 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 238000004062 sedimentation Methods 0.000 claims description 32
- 239000002893 slag Substances 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 24
- 238000005189 flocculation Methods 0.000 claims description 21
- 230000016615 flocculation Effects 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 11
- 239000002002 slurry Substances 0.000 claims description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 239000000701 coagulant Substances 0.000 claims description 3
- 239000002223 garnet Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 230000003139 buffering effect Effects 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000013618 particulate matter Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 230000002378 acidificating effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 238000005868 electrolysis reaction Methods 0.000 abstract description 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 19
- 230000000694 effects Effects 0.000 description 14
- 238000007254 oxidation reaction Methods 0.000 description 14
- 229920002401 polyacrylamide Polymers 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000001914 filtration Methods 0.000 description 10
- 238000002156 mixing Methods 0.000 description 10
- 238000009210 therapy by ultrasound Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 238000003825 pressing Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 229940037003 alum Drugs 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910017108 Fe—Fe Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003851 biochemical process Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- -1 hydroxyl free radical Chemical group 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- PVGBHEUCHKGFQP-UHFFFAOYSA-N sodium;n-[5-amino-2-(4-aminophenyl)sulfonylphenyl]sulfonylacetamide Chemical compound [Na+].CC(=O)NS(=O)(=O)C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 PVGBHEUCHKGFQP-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46176—Galvanic cells
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/05—Conductivity or salinity
- C02F2209/055—Hardness
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a preparation method of modified micro sand and a treatment method for removing TOC and phosphorus from chemical wastewater by reducing hardness. The preparation raw materials of the modified micro sand comprise fine sand, coal cinder fine materials, cerium oxide and zero-valent nano iron, and the modified micro sand has the advantages of high specific gravity, strong adsorption performance, micro-electrolysis removal of organic matters and cyclic utilization, and has higher catalytic activity under acidic and alkaline conditions. The treatment method for removing TOC and phosphorus from the chemical wastewater by reducing the hardness has the synergistic capability of removing TOC, reducing the hardness and removing TP, and has the advantages of simple operation, low running cost and no secondary pollution.
Description
Technical Field
The invention belongs to the technical field of chemical wastewater treatment, and particularly relates to a flocculant loading and precipitation process for hard-falling TOC and phosphorus removal of chemical wastewater.
Background
The wastewater coagulating sedimentation technology is mainly used for reducing hardness, such as the hardness removal of circulating water sewage, the hardness removal of gasified ash water and the like; at present, the TOC removal technology of the wastewater mainly comprises oxidation processes, such as hydrogen peroxide oxidation, ozone oxidation and the like and combined related processes; adsorption processes such as activated carbon adsorption, resin adsorption, etc.; biochemical processes, such as activated sludge processes, biological filter bed processes, and the like. The dephosphorization process mainly comprises biological dephosphorization and chemical dephosphorization. Compared with the traditional coagulating sedimentation, the conventional high-density pond has the advantages of high sedimentation efficiency, stable water outlet, small occupied area and the like, and the micro-sand flocculating sedimentation process is usually added with sea sand or a sedimentation aid with larger specific gravity, or adopts a magnetic carrier, so that the aim of recycling is fulfilled by utilizing a magnetic separation technology. The synergistic process for reducing hardness, removing TOC and removing phosphorus has few difficulties in the current market, and the method has the advantages that the Fe-C-CeO 3 micro-battery can be formed, the modified micro-sand with the multivalent oxidation-reduction effect is used for loading the flocculation precipitation process, and the effects are achieved by screening the compound coagulant and the flocculant.
CeO 2 as a transition metal oxide is a hot spot material in the catalytic field due to the characteristics of rich oxygen vacancy defects, flexible conversion between Ce 3+ and Ce 4+ states and the like. However, due to the poor conductivity of the single-component CeO 2, the development of the single-component CeO 2 in the field of electrocatalysis is limited to a large extent.
The effect of the existing inventive sedimentation agent is mainly focused on increasing the floc sedimentation, and the sedimentation speed is increased and the hydraulic load, such as CN103232102A, is improved through the co-sedimentation effect of the sedimentation agent with larger specific gravity and the floc; for the catalyst with the organic matter degradation effect, metals such as Fe/Ce/Cu and the like are loaded conventionally, and hydroxyl free radical chain-breaking organic matters such as CN113083364A are generated by catalyzing hydrogen peroxide; some of the sedimentation aids can be recycled, magnetic substances such as ferroferric oxide and the like are added in the carrier, the effect of recycling is achieved through magnetic separation, meanwhile, part of the sedimentation aids have a large specific surface area/porous structure, and organic substances such as CN113058555A are removed through adsorption; the above-mentioned sedimentation aid/catalyst can not reach the effect of degrading organic matters/raising sedimentation property at the same time under the same process, so that the invention can integrate the advantages of the invention, through taking coal slag as a carrier, modifying by nano iron and simultaneously loading cerium oxide, carbon and nano iron in the coal slag raise the conductivity of cerium oxide, degrade organic matters, have larger specific surface area/larger specific gravity, adsorb/degrade organic matters, and raise sedimentation rate.
Disclosure of Invention
The invention aims to provide a preparation method of modified micro sand, which has the advantages of high specific gravity, strong adsorption performance, micro electrolysis removal of organic matters and recycling, and has higher catalytic activity under acidic and alkaline conditions.
The invention also aims to provide a treatment method for removing TOC and phosphorus from chemical wastewater by reducing hardness, which has the synergistic capability of removing TOC, reducing hardness and removing TP, and has the advantages of simple operation, low running cost and no secondary pollution.
In order to solve the technical problems, the invention adopts the following technical scheme:
The preparation method of the modified micro sand comprises the following steps:
(1) The fine sand, the coal slag fines, the cerium oxide, the zero-valent nano iron and the water are mixed according to the mass ratio of 5 (0.1-5) (0.01-1): (50-500), heating to 40-80deg.C to obtain slurry, granulating, and drying to obtain granular material;
(2) Introducing steam into the granular material, reacting at 120-280 deg.c, preferably 150-200 deg.c for 5-12 hr, preferably 6-8 hr, cooling, washing and drying to obtain modified micro sand.
The coal cinder fine material is obtained by crushing coal cinder and filtering the crushed coal cinder by adopting a 10-100-mesh screen.
Preferably, in the step (1) of the present invention, the mixing is performed by ultrasonic treatment for 60-120min.
Preferably, in the step (1) of the present invention, the heating time is 2 to 8 hours.
Preferably, the drying in step (1) is carried out at 100-110℃for 2-3 hours.
Preferably, the amount of steam introduced in step (2) is from 5 to 20mL/g, based on the mass of particulate matter.
Preferably, the washing in step (2) comprises the steps of: washing with deionized water for 3-5 times, and washing with absolute ethanol for 3-5 times.
Preferably, the drying in step (2) is at 100-110 ℃ for 2-3 hours.
Preferably, the average particle size of the zero-valent nano iron is 10-50nm, the purity is more than 99.9%, and the specific surface area is 20-100m 2/g, preferably spherical crystal form.
Preferably, the cinder contains SiO2 40-50wt％、Al2O3 30-50wt％、Fe2O3 4-20wt％、CaO 1-5wt％、C 1-5wt％.
Preferably, the fine sand is garnet, the grain diameter is 80-120 meshes, the density is 3.8-4.1 g/cm 3, and the bulk specific gravity is 2.3-2.4.
Preferably, the specific surface area of the modified micro sand is 50-200m 2/g.
A method for removing TOC and phosphorus from chemical wastewater by reducing hardness comprises the following steps:
a) And (3) a coagulation stage: the wastewater enters a primary loading coagulation tank, and a coagulant PAC (polyaluminium chloride) is added into the primary loading coagulation tank; then the mixture enters a secondary loading coagulation tank, sodium hydroxide solution is added into the secondary loading coagulation tank, and the mixture is stirred at a speed gradient G=500-800S -1, and the residence time is 5-10min; then, the wastewater enters a three-stage loading coagulation tank, sodium carbonate is added into the three-stage loading coagulation tank, and calcium-magnesium floc sediment is formed;
b) Loading flocculation stage: the product of the step a) enters a loading flocculation tank, and PAM (anionic polyacrylamide) and modified micro sand are added into the loading flocculation tank;
c) Precipitation: the product of the step b) enters an inclined plate sedimentation tank for sedimentation, clear liquid overflows to water, and sludge containing modified micro sand flocs is sedimented to the bottom of the inclined plate sedimentation tank;
d) And (3) a sludge centrifugation stage: the modified micro sand-containing flocculated sludge is discharged from the bottom of the inclined plate sedimentation tank to the loading agent separator, the modified micro sand is separated from the flocculated sludge through centrifugal separation, the modified micro sand with high specific gravity is radially downward and enters the loading flocculation tank, the flocculated sludge with low specific gravity is radially upward and enters the sludge buffering tank, part of the sludge flows back to the first-stage loading coagulation tank, and the rest part of the sludge enters the sludge storage tank.
The product of the step a) comprises PAC micro organic flocs, calcium hydroxide, calcium carbonate and other inorganic flocs.
The method of the invention adopts modified micro sand loading flocculation technology to increase the specific gravity of the flocs, reduce the sedimentation time, and also utilizes the porous structure of the modified carrier to improve the removal efficiency of organic matters, thereby improving the pretreatment effect on chemical wastewater.
Preferably, the PAC dosage in the primary loading coagulation tank in the step a) is 10-500mg/L, based on the wastewater volume of the primary loading coagulation tank.
Preferably, in the step a), the adding amount of sodium hydroxide in the primary loading coagulation tank is controlled to be 7.5-9.5 according to the pH value.
Preferably, in the step a), in the three-stage loading coagulation tank, the molar ratio of sodium carbonate to the sum of calcium and magnesium elements in the wastewater is 1: (0.5-1).
Preferably, PAM in step b) is an anion, the number average molecular weight is 800-2000 ten thousand, the adding amount is 0.5-2mg/L, and the PAM is based on the volume of wastewater of the primary loading coagulation tank.
Preferably, in the step b), the modified micro sand is added to ensure that the content of the modified micro sand in the wastewater is 10-500mg/L.
Preferably, step b) is stirred with a velocity gradient g=500-800S -1, residence time 5-10min.
Preferably, the settling stage residence time of step c) is from 0.5 to 10 hours.
Preferably, in the step d), the sludge centrifugation stage, the modified micro sand-containing floccule sludge contains modified micro sand and floccule sludge, and the density of the modified micro sand-containing floccule sludge is 1.1% -1.5% g/cm 3.
Preferably, in the step d) of the sludge centrifugation, the proportion of the sludge flowing back to the primary loading coagulation tank is 10-50%.
Preferably, in step d) the sludge centrifugation stage, the loss rate of the micro sand is 0.1-0.5g/t water.
The wastewater mainly comprises biochemical water production or circulating water for discharging, the water quantity of the wastewater is 1000-1500t/h, the hardness is 200-600mg/L, the TOC is 15-55mg/L, and the TP is 0.1-5.5mg/L; through the process treatment, the wastewater index can be reduced to be less than 60mg/L in hardness, 15mg/L in TOC and 0.1mg/L in TP; the modified loading agent has obvious advantages in loss and addition of less than 0.5g/t of wastewater.
The invention has the beneficial effects that:
(1) The modified micro sand has high specific gravity (3.8-4.1 g/cm 3) so as to ensure that the sedimentation speed is high, and the overall process load is improved by more than 30 percent; the specific surface area is large (50-200 m 2/g), so that the adsorption performance is greatly enhanced; fe-C in the modified micro sand forms a miniature primary cell, so that organic matters can be broken and degraded;
(2) The nano-iron modified micro sand contains Fe/Fe 2+/Fe3+,Fe→Fe2+, so that weak oxidants S/I 2/Cu2+ and the like in water can be eliminated in the oxidation process, and strong oxidants Cl 2/Br2/HNO3 and the like in water can be eliminated in the oxidation process of Fe-Fe 3+ and Fe 2+→Fe3+; in the reduction process of Fe 3+ -Fe, reducing agents H 2/CO/Zn and the like in water can be eliminated; in the reduction process of Fe 3+→Fe2+, the reducing agent S 2-/HS-/SO3 2-/HSO3- and the like in water can be eliminated.
(3) The invention utilizes the carbon in the nano iron and the cinder to improve the conductivity of cerium oxide, and forms Ce 3+ and Ce 4+ under the high temperature condition, thereby improving the oxygen vacancy and leading the cerium oxide to have higher catalytic activity under the acidic and alkaline conditions.
(4) The modified micro-sand loading flocculation precipitation process has the synergistic capability of removing TOC, reducing hardness and removing TP, and has the advantages of simple operation, low running cost and no secondary pollution.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention:
Wherein 1, waste water pipeline, 2, PAC pipeline, 3, sodium hydroxide pipeline, 4, sodium carbonate pipeline, 5, PAM pipeline, 6, loading agent pipeline, 7, sediment reflux pipeline, 8, sludge separation pipeline, 9, sludge reflux pipeline, 10, sludge discharge pipeline, 11, hydrochloric acid pipeline, 12, discharge water pipeline, 13, sludge tank discharge pipeline, 14, primary loading coagulation tank, 15, secondary loading coagulation tank, 16, tertiary loading coagulation tank, 17, loading flocculation tank, 18, inclined plate sedimentation tank, 19, sludge storage tank, 20, loading agent separator, 21 and sludge buffer tank
Detailed Description
The technical scheme and effects of the invention are further described by the following specific examples. The following examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. Simple modifications of the invention using the inventive concept are within the scope of the invention as claimed.
The high-efficiency loading flocculation precipitation pretreatment device for reuse water comprises a reagent feeding system (PAC pipeline 2, PAM pipeline 5, sodium hydroxide pipeline 3, sodium carbonate pipeline 4 and hydrochloric acid pipeline 11), a loading flocculation precipitation system (a primary loading coagulation tank 14, a secondary loading coagulation tank 15, a tertiary loading coagulation tank 16, a loading flocculation tank 17 and an inclined plate sedimentation tank 18), a loading agent utilization system (a loading agent pipeline 6, a sediment reflux pipeline 7, a sludge separation pipeline 8 and a loading agent separator 20), and a sludge treatment system (a sludge reflux pipeline 9, a sludge external discharge pipeline 10, a sludge buffer tank 21 and a sludge storage tank 19);
The chemical adding system is characterized in that the concentration of the chemical in the PAC pipeline 2 is 10 percent, and the chemical is added into the primary loading coagulation tank 14; the concentration of the agent in the sodium hydroxide pipeline 3 is 32%, and the agent is added into the secondary loading coagulation tank 15; the concentration of the agent in the sodium carbonate pipeline 4 is 10 percent, and the agent is added into the three-stage loading coagulation tank 16; the PAM pipeline 5 has the concentration of 0.1 percent and is added into the loading flocculation tank 17; the concentration of the reagent in the HCI pipeline 11 is 30 percent and the reagent is added into the external drainage pipeline 12;
The wastewater in the wastewater pipeline 1 enters a primary loading coagulation tank 14, and PAC reagent is added and mixed uniformly; enters a secondary loading coagulation tank 15 and is uniformly mixed with sodium hydroxide; enters a three-stage loading coagulation tank 16 and is uniformly mixed with sodium carbonate; enters a loading flocculation sedimentation tank 17, is uniformly mixed with PAM to generate alum blossom, and enters an inclined plate sedimentation tank 18; the flocculated sludge containing the loading agent is discharged through a sediment return pipeline 7, and the supernatant overflows through an inclined plate and is mixed with HCI and then is discharged through an external water discharge pipeline 12;
The loading agent utilization system is characterized in that flocculated sludge containing the loading agent is discharged to a loading agent separation system 20 through a sediment return pipeline 7, and supernatant and sludge are discharged to a sludge buffer tank 21 from a sludge separation pipeline 8 under the action of centrifugal force and gravity; the loader is discharged from the loader line 6 to the load flocculation tank 17;
In the sludge treatment system, part of sludge in a sludge buffer tank 21 is discharged to a primary loading coagulation tank 14 through a sludge backflow pipeline 9, and the rest is discharged to a sludge storage tank 19 through a sludge discharge pipeline 10, and is subjected to secondary sedimentation and concentration and is discharged through a sludge tank discharge pipeline 13;
During operation, wastewater enters a primary loading coagulation tank 14 through a wastewater pipeline 1, PAC concentration is 100mg/L according to water quantity, sodium hydroxide is added into a secondary loading coagulation tank 15 until pH is 9, so that macromolecular organic matters, phosphate and PAC form flocs; adding 200mg/L sodium carbonate into the three-stage loading coagulation tank 16 to form calcium carbonate precipitate by calcium ions; when the wastewater enters the loading flocculation tank 17, the loading agent separated by the loading agent separator is added to the loading flocculation tank, the concentration of 50mg/L is maintained, and meanwhile, 2mg/L of PAM is added, so that small flocs are changed into alum flowers with larger specific gravity, and the alum flowers and the wastewater enter the inclined plate sedimentation tank 18 together, and at the moment, the alum flowers with larger specific gravity are quickly settled, discharged from the bottom and recycled; overflowing the clear liquid and discharging;
The separation efficiency of the loading agent separation system is generally more than 99%, but a small amount of loading agent is discharged along with the sludge, when the concentration of the loading agent at the loading flocculation tank 17 is lower than 20mg/L, about 50kg of loading agent is added according to the volume 720m 3 of the system, and the adding period is about 3-6 months;
after being separated by the loading agent separator 20, the flocculated sludge is conveyed to a sludge buffer tank 21 through a sludge separation pipeline 8, a small amount of agents such as loading agent and PAM still exist, and the agents are added to the primary loading coagulation tank 14 through a sludge return pipeline 9 according to the flow rate of the sediment return pipeline 7 by 10% -30%, so that the effects of improving the particle size of flocculated particles and reducing the use amount of the agents are achieved.
The TOC of the wastewater was 35mg/L, TP (total phosphorus) was 1.5mg/L, hardness was 460mg/L, and SS (suspended solids) was 18mg/L.
Comparative example 1:1# loader (fine sand):
garnet, particle size: 80-120 mesh, density: 3.8 to 4.1g/cm 3, bulk specific gravity: 2.3 to 2.4.
Comparative example 2: preparation of No. 2 loading agent (fine sand+cinder+nano iron):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, zero-valent nano iron and deionized water according to a mass ratio of 5:5:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, granulating, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Comparative example 3:3# loader preparation (fine sand + cinder + cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide and deionized water according to a mass ratio of 5:5:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, granulating, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Example 4: preparation of No. 4 loading agent (fine sand, cinder, nano iron and cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 5:5:1:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Example 5: preparation of No. 5 loading agent (fine sand, cinder, nano iron and cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 5:5:0.01:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Example 6: preparation of 6# loading agent (fine sand + cinder + nano iron + cerium oxide):
crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 5:5:1:0.01:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Example 7: preparation of No. 7 loading agent (fine sand+cinder+nano iron+cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 5:0.1:1:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Comparative example 8:8# preparation of loading agent (fine sand + cinder + nano iron + cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 1:5:1:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Example 9: preparation of No.9 loading agent (fine sand+cinder+nano iron+cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 5:5:1:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing 10mL/min of water vapor, controlling the reaction temperature to be 150 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
Example 10: preparation of No. 10 loading agent (fine sand+cinder+nano iron+cerium oxide):
Crushing coal slag, and filtering by adopting a 100-mesh screen to obtain coal slag fines; mixing fine sand, coal slag fines, cerium oxide, zero-valent nano iron and deionized water according to a mass ratio of 5:5:1:1:200, performing ultrasonic treatment for 120min, heating to 80 ℃, stirring for 6h to obtain slurry, pressing particles, and drying to obtain granular substances; placing the granular substances in an oxidation reaction tube, introducing water vapor for 5mL/min, controlling the reaction temperature to be 200 ℃ for reaction for 6 hours, cooling to room temperature, washing and drying to obtain the modified micro sand.
TABLE 1 Effect of wastewater treatment
From the table, the 4# loading agent has the optimal effects of removing TOC, phosphorus and hard and SS, and mutual verification of the comparative example (1/2/3) and the example (4/5/6/7/9/10) shows that the loading agent prepared by modifying nano iron and cerium oxide by taking the mixture of fine sand and cinder as a carrier has better sedimentation assisting effect and reduces the produced water SS and TP; secondly, the conductivity of the carrier is improved to form Ce 3+ and Ce 4+, so that oxygen vacancies are improved, and the catalyst has higher catalytic activity in the process of removing TOC and organic phosphorus from wastewater; and finally, the retired loading agent can be repeatedly processed, and the recycling effect is achieved.
In the continuous operation process, the pH is controlled to be 8.5-9, the PAC dosage is 100-150mg/L, the PAM dosage is 1-2mg/L, the loading agent is 30-50mg/L, the sodium carbonate is 350-400mg/L, the TOC removal rate of effluent is more than 50%, the TP removal rate is more than 90%, and the hardness removal rate is more than 85%, so that the method is suitable for the pretreatment and deep treatment process of a double-membrane system.
Claims (10)
1. The preparation method of the modified micro sand comprises the following steps:
(1) Fine sand, coal slag fines, cerium oxide, zero-valent nano iron and water are mixed according to the mass ratio of 5 (0.1-5):
(0.01-1): (0.01-1): (50-500), heating to 40-80deg.C to obtain slurry, granulating, and drying to obtain granular material;
(2) Introducing steam into the granular material, reacting at 120-280 deg.c, preferably 150-200 deg.c for 5-12 hr, preferably 6-8 hr, cooling, washing and drying to obtain modified micro sand.
2. The method of claim 1, wherein in step (1), the heating time is 2 to 8 hours.
3. The process according to claim 1 or 2, wherein the amount of steam introduced in step (2) is 5-20mL/g based on the mass of particulate matter.
4. A method according to any one of claims 1-3, characterized in that the zero-valent nano iron has an average particle size of 10-50nm, a purity of more than 99.9%, a specific surface area of 20-100m 2/g, preferably a spheroidal crystal form.
5. The method of any one of claims 1-4, wherein the coal cinder comprises SiO240-50wt％、Al2O3 30-50wt％、Fe2O3 4-20wt％、CaO 1-5wt％、C 1-5wt％.
6. The method of any one of claims 1-5, wherein the fine sand is garnet, has a particle size of 80-120 mesh, a density of 3.8-4.1 g/cm 3, and a bulk specific gravity of 2.3-2.4.
7. A method for removing TOC and phosphorus from chemical wastewater by reducing hardness comprises the following steps:
a) And (3) a coagulation stage: the wastewater enters a primary loading coagulation tank, and a coagulant PAC is added into the primary loading coagulation tank; then the mixture enters a secondary loading coagulation tank, sodium hydroxide solution is added into the secondary loading coagulation tank, and the mixture is stirred at a speed gradient G=500-800S -1, and the residence time is 5-10min; then, the wastewater enters a three-stage loading coagulation tank, sodium carbonate is added into the three-stage loading coagulation tank, and calcium-magnesium floc sediment is formed;
b) Loading flocculation stage: feeding the product of the step a) into a loading flocculation tank, and adding PAM and the modified micro sand prepared by the method of any one of claims 1-6 into the loading flocculation tank;
c) Precipitation: the product of the step b) enters an inclined plate sedimentation tank for sedimentation, clear liquid overflows to water, and sludge containing modified micro sand flocs is sedimented to the bottom of the inclined plate sedimentation tank;
d) And (3) a sludge centrifugation stage: the modified micro sand-containing flocculated sludge is discharged from the bottom of the inclined plate sedimentation tank to the loading agent separator, the modified micro sand is separated from the flocculated sludge through centrifugal separation, the modified micro sand with high specific gravity is radially downward and enters the loading flocculation tank, the flocculated sludge with low specific gravity is radially upward and enters the sludge buffering tank, part of the sludge flows back to the first-stage loading coagulation tank, and the rest part of the sludge enters the sludge storage tank.
8. The method for removing TOC and phosphorus from chemical wastewater by reducing hardness according to claim 7, wherein PAC addition amount in the primary loading coagulation tank in the step a) is 10-500mg/L, and the method is based on the wastewater volume of the primary loading coagulation tank; the adding amount of sodium hydroxide in the primary loading coagulation tank is controlled to be 7.5-9.5 according to the pH value; in the three-stage loading coagulation tank, the molar ratio of sodium carbonate to the sum of calcium and magnesium elements in the wastewater is 1: (0.5-1).
9. The method for removing TOC and phosphorus from chemical wastewater according to claim 7 or 8, wherein in the step b), modified micro sand is added to make the content of the modified micro sand in the wastewater be 10-500mg/L.
10. The process for the precipitation of TOC and phosphorus removal from chemical wastewater according to any of claims 7 to 9, characterized in that in step d) the sludge centrifugation stage, the proportion of the sludge returned to the primary loading coagulation basin is between 10% and 50%.
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