CN107986382A - A kind of method of microwave irradiation high concentrated organic wastewater - Google Patents
A kind of method of microwave irradiation high concentrated organic wastewater Download PDFInfo
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- CN107986382A CN107986382A CN201711286749.7A CN201711286749A CN107986382A CN 107986382 A CN107986382 A CN 107986382A CN 201711286749 A CN201711286749 A CN 201711286749A CN 107986382 A CN107986382 A CN 107986382A
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- microwave
- activated carbon
- catalyst
- dipping
- carborundum
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- 238000000034 method Methods 0.000 title claims abstract description 63
- 239000002351 wastewater Substances 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000003054 catalyst Substances 0.000 claims abstract description 70
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 45
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 45
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 17
- 239000007800 oxidant agent Substances 0.000 claims abstract description 14
- 230000001590 oxidative effect Effects 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- 238000006722 reduction reaction Methods 0.000 claims abstract description 9
- 239000003344 environmental pollutant Substances 0.000 claims abstract description 8
- 239000005416 organic matter Substances 0.000 claims abstract description 8
- 231100000719 pollutant Toxicity 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 239000003863 metallic catalyst Substances 0.000 claims abstract description 4
- 230000009471 action Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 33
- 238000007254 oxidation reaction Methods 0.000 claims description 25
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 230000003647 oxidation Effects 0.000 claims description 24
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 18
- 239000003570 air Substances 0.000 claims description 18
- 239000002253 acid Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 229910000510 noble metal Inorganic materials 0.000 claims description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- -1 zinc transition metal Chemical class 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004155 Chlorine dioxide Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- XXVRGGCHZUCJCX-UHFFFAOYSA-N [Cl].[Rh] Chemical compound [Cl].[Rh] XXVRGGCHZUCJCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 235000019398 chlorine dioxide Nutrition 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 239000010970 precious metal Substances 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 238000007598 dipping method Methods 0.000 abstract 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000007792 addition Methods 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000004088 simulation Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000009303 advanced oxidation process reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910016874 Fe(NO3) Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/302—Treatment of water, waste water, or sewage by irradiation with microwaves
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- 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
- B01J23/72—Copper
-
- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/33—
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
Abstract
The present invention provides a kind of method of microwave irradiation high concentrated organic wastewater, this method comprises the following steps：A, activated carbon, carborundum, activated carbon fibre, carbon nanotube loaded metallic catalyst are prepared using dipping microwave, impregnation-calcination or liquid phase ethylene glycol chemical reduction method.B, the catalyst of above-mentioned gained is added in the waste water containing organic matter, under microwave action, is passed through oxidant gas or liquid, the organic matter in waste water is oxidized into inorganic molecules compound, so as to achieve the purpose that to reduce pollutant emission.The method of the present invention handles organic wastewater, selects activated carbon, carborundum, activated carbon fibre, carbon nanotubes to have the advantages that service life length, catalytic activity height, wastewater treatment condition milder as catalyst carrier.
Description
Technical field
The present invention relates to a kind of method of microwave irradiation high concentrated organic wastewater, belong to field of waste water treatment.
Background technology
The development of modern industry makes industrial wastewater species containing persistent organic pollutants and quantity increasing, this kind of useless
Water usually contains the pollutants such as difficult degradation, poisonous, harmful, organic pollution and ammonia nitrogen compound, suspended matter, the dirt to environment
Dye degree is very large, has been difficult to meet technology and economy using processing methods such as conventional biologies or physico-chemical purification
It is required that.Therefore the purified treatment problem of this kind of industrial organic waste water has become at present one of problem of field of environment protection both at home and abroad,
Have been to be concerned by more and more people.
At present, organic wastewater is mainly handled by being used in combination for Physical, chemical method and bioanalysis.At biology
Logos also has some shortcomings, is that process is slow first, and can produce a large amount of sludge, and these sludge must landfill disposal.Separately
Outside, it is not suitable for handling using biologic treating technique for the waste water that toxicity is larger, concentration is higher, above-mentioned substance is to microorganism
Growth have inhibitory action, these all limit the application of biologic treating technique.
Abiotic processing method includes Physical and chemical method.Physical（Including absorption method, salting out method, solvent extraction,
The air lift way of distillation, ion-exchange and membrane technology etc.）It is by common phase detachment technique, concentrates pollutant.Then, if any
Necessity, then using chemical Treatment pollutant.The chemical Treatment of pollutant mainly aoxidizes, first commercialized oxidation skill
Art is exactly to burn.In this process, aoxidized in gas phase of the pollutant more than 1000 DEG C.In fact, burn require it is organic
Thing concentration is sufficiently high, to ensure whole process autothermal equilibrium, otherwise will need big energy, therefore incineration technology is needed in waste water
COD reach 300g/L.In addition, burning disposal chlorine-bearing compound is that to produce bioxin be also merit attention the problem of.
Another processing method different with gaseous oxidation is liquid phase oxidation, according to the difference of oxidant, is broadly divided into two
Class：First, wet process oxidation technology（WAO）, second, advanced oxidation processes（AOP）.WAO is usually under 0.5-20MPa and 400-700K
The shortcomings that operation, it is maximum is cost of investment height, and at high temperature and pressure, oxidation product has higher corrosivity, it is necessary to make
With special alloy material.
Microwave irradiation technology（MICOP）It is to focus on the radiation of high intensity short pulse microwave containing some " quick
On the solid catalyst bed surface of agent ", by the strong interaction of surface point position and microwave energy, microwave energy is changed into heat
Can, so as to optionally raise the temperature of some surface point positions, it is anti-chemical catalysis may to occur when reactant is in contact with it
Should.The strong wave absorbtion of activated carbon makes it to be used as " sensitizer ", is widely used in microwave method and curbs environmental pollution in thing.Microwave lures
Lead activated carbon catalysis oxidation technology has become one of research hotspot of processing high concentration hard-degraded organic waste water both at home and abroad.
In the Chinese patent of Application No. 02118708.8, a kind of microwave catalysis oxidation processing used water difficult to degradate is disclosed
Technique and device, the technique can be reacted under low-temperature atmosphere-pressure, technique is simple, it can be achieved that automation.But its oxidant is main
It is big there are security risk using hydrogen peroxide or pure oxygen, it is of high cost the shortcomings that.
In the Chinese patent of Application No. 200410013583.8, disclose a kind of for microwave-induced oxidation process
The preparation method of modified alumina catalyst.The catalyst can be rapidly and efficiently microwave is converted into thermal energy, but embodiment
In only with simulated wastewater, compare removal abilities of index such as the removing of waste water pigment, actual waste water COD and indefinite.
In the Chinese patent of Application No. 200610115836.1, disclose one kind and be used for microwave induced ClO2Oxidation is urged
Change the CuO- γ Al of oxidation technology2O3Preparation method.The catalyst can accelerate oxidation rate, reduce ClO2Dosage, realize
In efficient quick processing wastewater the problem of persistent organic pollutants.But its oxidant cost is high, and security risk is big, handles at the same time
Waste strength is relatively low（200mg/L or so）
In the Chinese patent of Application No. 201310430879.9, disclose a kind of one kind in containing iron, manganese and nickel or
The surface of the oxidant of several absorbing materials, is that oxidant surface produces higher temperature, so that oxygen occur using microwave effect
Change reaction, organic matter is degraded, so as to achieve the purpose that treated sewage.But the program is complicated there are catalyst preparation, use
The shortcomings that amount is big, and the rate of recovery is low.
The content of the invention
It is an object of the present invention to provide a kind of method of new microwave radiation technology oxidation processes organic high strength wastewater, leads to
Organic matter in waste water can effectively be removed by crossing this method.
The present invention provides a kind of method of new microwave radiation technology oxidation processes organic high strength wastewater, this method include with
Lower step：
A prepares activated carbon, carborundum, active carbon fibre using dipping-microwave, dipping-roasting or liquid phase ethylene glycol chemical reduction method
Dimension, carbon nanotube loaded metallic catalyst.
B adds the catalyst of above-mentioned gained in the waste water containing organic matter, under microwave action, is passed through gas or liquid
Body oxidant, makes the organic matter in waste water be oxidized into inorganic molecules compound, and pollutant emission is reduced so as to reach
Purpose.
Such as the step A, activated carbon of the present invention, carborundum, activated carbon fibre, carbon nanotube loaded metal are urged
Agent preparation method mainly has three kinds：
（One）Dipping-roasting method
Prepare the metal salt solution of certain molar concentration, under stirring condition, constant weight is added according to the ratio of liquor capacity
Activated carbon, carborundum, activated carbon fibre, carbon nanotubes are impregnated, and are then roasted.
（Two）Dipping-microwave method
Prepare the metal salt solution of certain molar concentration, under stirring condition, constant weight is added according to the ratio of liquor capacity
Activated carbon, carborundum, activated carbon fibre, carbon nanotubes are impregnated, and carry out microwave treatment.
（Three）Liquid phase ethylene glycol chemical reduction method
The inorganic noble metal acid solution of certain molar concentration is prepared, ethylene glycol is added by noble metal acid solution certain proportion.Stirring
Under the conditions of by liquid volume certain proportion add activated carbon, carborundum, activated carbon fibre, carbon nanotubes, adjust pH after microwave
Processing.
Preferably, in the step A, catalyst is prepared using dipping-microwave method, wherein coming for noble metal catalyst
Say, it is preferred to select liquid phase ethylene glycol chemical reduction method to prepare catalyst.
Preferably, in the step A, carrier used is activated carbon, carborundum, activated carbon fibre, carbon nanotubes, metal
Using iron, cobalt, nickel, manganese, cadmium, vanadium, copper, zinc transition metal and gold, platinum, palladium, rhodium noble metal oxide or composite oxides, its
In more preferably iron, copper, platinum.
Inorganic noble metal acid in the present invention refers to the inorganic acid for including precious metal element, such as gold chloride, chloroplatinic acid, chlorine
Palladium acid and chlorine rhodium acid.
Metal salt solution in the present invention, refer to above-mentioned metal soluble-salt prepare aqueous solution, including its hydrochloride,
Nitrate, sulfate.
Preferably, the method（One）With（Two）In, salting liquid molar concentration used is 0.1-1.0M, more preferably
0.5M.Preferably, activated carbon, carborundum, activated carbon fibre, the amount of carbon nanotubes are added（g）For liquid volume（ml）'s
0.5-5%, more preferably 1-2%.
Preferably, the method（One）In, calcination temperature is 300 ~ 600 DEG C, when roasting time is 1-4 small, it is furthermore preferred that
Calcination temperature is 400 DEG C, when roasting time is 2 small.
Preferably, the method（Two）In, microwave power is 400 ~ 700W, and the microwave time is 1-10min, it is furthermore preferred that
Microwave power is 700W, and the microwave time is 2min.
Preferably, the method（Three）In, the molar concentration of inorganic noble metal acid solution is 0.01-0.2M, more preferably
For 0.05M.Preferably, ethylene glycol addition is 200-600 times of inorganic noble metal acid solution, is more preferably 500 times.It is preferred that
Add activated carbon, carborundum, activated carbon fibre, the amount of carbon nanotubes（g）For liquid volume（ml）0.1% ~ 1%, it is more excellent
Choosing for 0.2%.
Preferably, the method（Three）In, microwave power is 100 ~ 1000W, and the microwave time is 1-10min, it is furthermore preferred that
Microwave power is 700W, and the microwave time is 1.5min.
Preferably, in the step B, oxidant used includes air, oxygen, ozone, hydrogen peroxide, chlorine dioxide etc. can
To produce the gas of oxygen radical or solution, air, oxygen and hydrogen peroxide are more preferably selected.
Preferably, in the step B, the waste water COD concentration of processing is 100-20000mg/L.
Preferably, in the step B, catalyst charge（g）Relative to COD total amounts in waste water（mg）Percentage be
0.01% ~ 1%, more preferably 0.04% ~ 0.2%.
Preferably, in the step B, reaction temperature is 40 ~ 200 DEG C；When oxidant is gas, more preferably 90 ~ 100
℃；When oxidant is liquid, more preferably 150-180 DEG C.
The beneficial effects of the present invention are：The method of the present invention handles organic wastewater, selects activated carbon, carborundum, activated carbon
Fiber, carbon nanotubes are as catalyst carrier, and larger using its adsorption capacity, adsorptive selectivity is good, and equilibration time is short, high-strength
Degree, regenerates easier advantage, is more effective adsorbent.Additionally, due to its high conductivity, high intensity and adsorption capacity, so as to keep away
Exempted from it is conventional use activated carbon for carrier easily occur by oxidation and duct block etc. deactivation phenomenom, have service life length,
The advantages that catalytic activity is high, wastewater treatment condition milder.
Embodiment
Embodiment 1
The preparation of Carbon Nanotubes Supported Platinum Catalysts
Carbon nanotubes 0.4g is weighed, adds 200ml ethylene glycol, stirs lower chloroplatinic acid 0.4ml, the ultrasonic 10min for adding 0.05M,
Stirring be slowly added dropwise NaOH saturated solutions to PH be 12.It is put under microwave 700W power and stablizes 75s, taking-up is cooled to room temperature, and is taken out
Filter, acetone foam washing is three times.Obtained solid is finally put into 85 DEG C of dryings of air dry oven, gained sample is as carbon nanotube loaded
Platinum catalyst.
Carbon Nanotubes Supported Platinum Catalysts catalytic air oxidation laboratory simulation organic wastewater
Prepare 2000mg/L phenol solutions（COD is 5000mg/L or so）As simulative organic wastewater, take in solution 30ml additions
Catalyst 0.12g is stated, ultrasonic 5min, is filtered after stirring at normal temperature absorption.Above-mentioned solid is separately added into phenol solution 30ml, is placed in
In microwave reactor, air is passed through, adjusts 100 DEG C of microwave power controlling reaction temperature.React 2.5 it is small when after, reaction was completed, survey
Determine solution C OD values, it is 71% to calculate COD removal rates.
Embodiment 2
The preparation of carbon nanotube loaded copper catalyst
Nitrate trihydrate copper 8.5g is weighed, adds water 70ml wiring solution-formings, adds carbon nanotubes 1.0g, stirring at normal temperature, filters, and filter cake is used
Filtered after washing, be put into air dry oven drying.Above-mentioned solid is taken out and is put into there-necked flask, is placed in microwave reactor, nitrogen
Under air-flow, stablize 2min under microwave power 700W, up to carbon nanotube loaded copper catalyst.
Carbon nanotube loaded copper catalyst catalytic air oxidation laboratory simulation waste water
Prepare 2000mg/L phenol solutions（COD is 5000mg/L or so）As simulative organic wastewater, take in solution 30ml additions
Catalyst 0.12g is stated, ultrasonic 5min, is filtered after stirring at normal temperature absorption.Above-mentioned solid separately is added to phenol solution 30ml, is placed in micro-
In ripple reactor, air is passed through, adjusts 100 DEG C of microwave power controlling reaction temperature.React 2.5 it is small when after, reaction was completed, measure
Solution C OD values, it is 64% to calculate COD removal rates.
Embodiment 3
The preparation of carbon nanotube loaded iron catalyst
Take 65% concentrated nitric acid solution 43.7ml to add water 70ml wiring solution-formings, weigh Fe(NO3)39H2O 14.14g and be put into solution and stir
Dissolving is mixed, adds carbon nanotubes 1.0g, is stirred, filtering.Filtered after filter cake washing.It is put into air dry oven drying.Taken above-mentioned
Go out to be put into there-necked flask, be placed in microwave reactor, under nitrogen stream, stablize 2min under microwave power 700W, up to carbon nanotubes
The iron catalyst of load.
Carbon nanotube loaded iron catalyst catalytic air oxidation laboratory simulation waste water
Prepare 2000mg/L phenol solutions（COD is 5000mg/L or so）As simulative organic wastewater, take in solution 30ml additions
Catalyst 0.12g is stated, ultrasonic 5min, is filtered after stirring at normal temperature absorption.It is another to take phenol solution 30ml to add above-mentioned solid, it is placed in micro-
In ripple reactor, air is passed through, adjusts 100 DEG C of microwave power controlling reaction temperature.React 2.5 it is small when after, reaction was completed, measure
Solution C OD values, it is 55% to calculate COD removal rates.
Embodiment 4
Carbon nanotube loaded metallic catalyst is catalyzed hydrogen peroxide oxidation laboratory simulation waste water
Prepare 2000mg/L phenol solutions（COD is 5000mg/L or so）As simulative organic wastewater, solution 100ml is taken to add carbon
Nano tube supported platinum catalyst 100mg, ultrasonic 5min, are filtered after stirring at normal temperature absorption.It is another to take phenol solution 100ml additions above-mentioned
Solid, is placed in microwave reactor, adds hydrogen peroxide 3ml, adjusts 120 DEG C of microwave power controlling reaction temperature.React 1.5 it is small when
Afterwards, reaction was completed, measures solution C OD and TOC value, and it is that 97%, TOC removal rates are 82% to calculate COD removal rates.
Identical with above-mentioned test operation, using carbon nanotube loaded iron catalyst, COD removal rates are 99%, TOC removal rates
For 91%.
Identical with above-mentioned test operation, using carbon nanotube loaded copper catalyst, COD removal rates are 100%, TOC removal rates
For 97%.
Embodiment 5
Investigate under different condition, the optimum condition of microwave radiation technology air catalytic oxidation treatment of laboratory simulated wastewater.Carbon is selected to receive
Mitron load platinum catalyst, to it under different technology conditions（Reaction temperature, catalyst proportion and waste water COD concentration）Catalysis
Activity is studied.
Reaction temperature mainly selects 100 DEG C, 80 DEG C and 60 DEG C, catalyst amount（g）Selection processing wastewater flow rate（ml）'s
0.4%th, 0.8% and 0.2%, waste water COD concentration mainly selects 10000mg/L, 5000mg/L and 2500mg/L.Operated by embodiment 1
Method is tested.Result of the test is seen the above table.
As can be seen from the above table, reaction temperature influences maximum for catalyst activity, secondly catalyst amount, reacts bottom
Thing concentration influences minimum for catalytic reaction.Compare differential responses temperature（100℃、80℃、60℃）Under, as temperature raises,
The removal amount of COD and phenol is bigger.Reaction temperature is high, illustrate that microwave energy is big, the oxidation of phenol will be more prone to thoroughly.But
With the rise of temperature, the removal rate increasing degree of COD and phenol diminishes.
Under the same reaction conditions, 0.2%, 0.4% and 0.8% is investigated respectively（w/v）Catalyst amount, can be with from upper table
Find out, with the increase of catalyst amount, catalytic capability strengthens, but when catalyst amount increases to 0.8% from 0.4%, COD
Do not increase with phenol removal rate, this 0.4% catalyst amount of explanation is optimal selection.
Under the same reaction conditions, the phenol solution different to COD concentration respectively（2500mg/L, 5000mg/L and
10000mg/L）Catalytic oxidation treatment is carried out, the COD removal rates of wherein low concentration and middle concentration are suitable（71% and 69%）, high concentration
The COD removal rates of substrate are relatively low（66%）, but for reaction temperature and catalyst proportion, different concentration of substrate are for urging
It is smaller to change activity influence.
By result above as it can be seen that when reaction temperature is 100 DEG C, and catalyst amount is 0.1%, processing COD concentration is
The waste water effect of 5000mg/L or so is best, and COD removal rates can reach more than 70%.
Embodiment 6
Investigate under different condition, the optimum condition of microwave radiation technology hydrogen peroxide catalytic oxidation treatment of laboratory simulated wastewater.Select carbon
Nano tube supported iron catalyst, to it under different technology conditions（Reaction temperature, catalyst proportion）Catalytic activity carries out
Research.
Using hydrogen peroxide as oxidant, the initial COD value of phenol synthetic water is 5000mg/ml or so, and carbon nanotubes is born
The dosage of supported ferric catalyst（The grams of catalyst amount accounts for 0.2%, 0.1% and the 0.05% of wastewater volume milliliter number）Not equality of temperature
Under degree（180℃、120℃、100℃）The removal rate of the COD and TOC of phenol synthetic water are studied.Using hydrogen peroxide as
Catalyst, can significantly improve treatment effeciency, COD removal rates highest, which can reach 100%, TOC removal rates highest, can reach 97%.
Similar with air oxidation, influence of the reaction temperature for catalyst treatment is very big.Temperature is higher, and COD and TOC are gone
Except rate is higher（At 180 DEG C, TOC removal rates are 97%, and 55% is reduced at 100 DEG C；At 180 DEG C, COD removal rates are 100%, 100
76% is reduced at DEG C）.The influence that catalyst amount is removed for COD and TOC is investigated, with the increase of catalyst amount, COD
Also increase therewith with TOC removal rates.
By result above as it can be seen that when reaction temperature is 180 DEG C, and catalyst amount is 0.05%, COD removal rates can reach
It can reach more than 97% to 100%, TOC removal rates.
Embodiment 7
Carbon Nanotubes Supported Platinum Catalysts catalytic air oxidation factory pharmacy waste water
Certain pharmacy corporation is taken to produce waste water, COD 16100mg/L.Solution 300ml is taken to add Carbon Nanotubes Supported Platinum Catalysts
4g, ultrasonic 5min, are filtered after stirring at normal temperature absorption.Above-mentioned solid separately is added into above-mentioned waste water solution 300ml, it is anti-to be placed in microwave
Answer in device, blowing air, adjust 100 DEG C of microwave power controlling reaction temperature.React 2.5 it is small when after, reaction was completed, measure solution
COD value, it is 67% to calculate COD removal rates.
Comparative example 1
Except catalyst to be replaced with to carbon nanotubes, activated carbon, activated carbon supported copper catalyst respectively, catalyst amount is adjusted
Whole outer, other experimental methods and condition are same as Example 1.（Specific data see the table below）
As can be seen from the above table, carbon nanotube loaded copper catalyst activity is significantly larger than other catalyst.
Except catalyst to replace with to carbon nanotubes, activated carbon, activated carbon supported copper catalyst respectively, catalyst amount into
Row adjustment is outer, other experimental methods and condition are same as Example 4.（Specific data see the table below）
As can be seen from the above table, carbon nanotube loaded copper catalyst activity is significantly larger than other catalyst.
Comparative example 2
According to the operating condition of embodiment 1, the COD of more carbon nanotube loaded copper catalyst and activated carbon supported copper catalyst
Removal rate.（Data such as following table）
After above-mentioned data can be seen that carbon nanotube loaded catalyst is reused 7 times, under catalytic capability is not obvious
Drop, and after activated carbon supported catalyst is reused 3 times, catalytic capability is just decreased obviously.Illustrate carbon nanotube loaded
Catalyst service life is longer.
Applicant states that the present invention illustrates the method detailed of the present invention, but this hair by above-described embodiment and comparative example
It is bright to be not limited to above-mentioned method detailed, that is, do not mean that the present invention has to rely on above-mentioned method detailed and could implement.Affiliated skill
The technical staff in art field should be understood that any improvement in the present invention, including the replacement of each raw material, the addition of auxiliary element,
Selection of concrete mode etc., is within the scope of the present invention.
Claims (6)
1. a kind of method of microwave irradiation high concentrated organic wastewater, this method comprise the following steps：
A prepares activated carbon, carborundum, active carbon fibre using dipping-microwave, dipping-roasting or liquid phase ethylene glycol chemical reduction method
Dimension, carbon nanotube loaded metallic catalyst；
B adds the catalyst of above-mentioned gained in the waste water containing organic matter, under microwave action, is passed through gas or liquid oxygen
Agent, makes the organic matter in waste water be oxidized into inorganic molecules compound, so as to achieve the purpose that to reduce pollutant emission.
2. according to the method described in claim 1, it is characterized in that, in the step A, method for preparing catalyst is used such as
Under：
Dipping-roasting method：Prepare the metal salt solution of certain molar concentration, under stirring condition, add according to the ratio of liquor capacity
Enter the activated carbon of constant weight, carborundum, activated carbon fibre, carbon nanotubes to be impregnated, then roasted；
Dipping-microwave method：Prepare the metal salt solution of certain molar concentration, under stirring condition, add according to the ratio of liquor capacity
Enter the activated carbon of constant weight, carborundum, activated carbon fibre, carbon nanotubes to be impregnated, carry out microwave treatment；
Liquid phase ethylene glycol chemical reduction method：The inorganic noble metal acid solution of certain molar concentration is prepared, by noble metal acid solution one
Certainty ratio adds ethylene glycol；Under stirring condition by liquid volume certain proportion add activated carbon, carborundum, activated carbon fibre,
Carbon nanotubes, adjusts microwave treatment after pH；
Preferably, catalyst is prepared using dipping-microwave method, wherein for noble metal catalyst, more preferably selects second
Glycol solution phase chemical reduction prepares catalyst.
3. according to the method described in claim 2, it is characterized in that, carrier used is activated carbon, carborundum, active carbon fibre
Dimension, carbon nanotubes, metal is using iron, cobalt, nickel, manganese, cadmium, vanadium, copper, zinc transition metal and gold, the oxidation of platinum, palladium, rhodium noble metal
Thing or composite oxides.
4. according to the method described in claim 2, it is characterized in that, inorganic noble metal acid used refers to include precious metal element
Inorganic acid, including gold chloride, chloroplatinic acid, chlorine palladium acid and chlorine rhodium acid；Metal salt solution used, refers to carry in claim 3
And metal the aqueous solution for preparing of soluble-salt, including its hydrochloride, nitrate, sulfate.
5. dipping-roasting method according to claim 2 and dipping-microwave method, it is characterised in that salting liquid mole used
Concentration is 0.1-1.0M, more preferably 0.5M；Preferably, activated carbon, carborundum, activated carbon fibre, carbon nanotubes are added
Amount（g）For liquid volume（ml）0.5-5%, more preferably 1-2%；
Preferably, in the dipping-roasting method, calcination temperature is 300 ~ 600 DEG C, when roasting time is 1-4 small, it is furthermore preferred that
Calcination temperature is 400 DEG C, when roasting time is 2 small；
Preferably, in the dipping-microwave method, microwave power is 400 ~ 700W, and the microwave time is 1-10min, it is furthermore preferred that micro-
Wave power is 700W, and the microwave time is 2min；
Preferably, in the liquid phase ethylene glycol chemical reduction method, the molar concentration of inorganic noble metal acid solution is 0.01-0.2M,
More preferably 0.05M；
Preferably, ethylene glycol addition is 200-600 times of inorganic noble metal acid solution, is more preferably 500 times；
Preferably add activated carbon, carborundum, activated carbon fibre, the amount of carbon nanotubes（g）For liquid volume（ml）0.1% ~
1%, more preferably 0.2%；
Preferably, in the liquid phase ethylene glycol chemical reduction method, microwave power is 400 ~ 700W, and the microwave time is 1-10min, more
Preferably, microwave power 700W, microwave time are 1.5min.
6. according to the method described in claim 1, it is characterized in that, in the step B, oxidant used includes air, oxygen
Gas, ozone, hydrogen peroxide, chlorine dioxide etc. can produce the gas or solution of oxygen radical, more preferably select air, oxygen and
Hydrogen peroxide；
Preferably, in the step B, the waste water COD concentration of processing is 100-20000mg/L；
Preferably, in the step B, catalyst charge（g）Relative to COD total amounts in waste water（mg）Percentage be
0.01% ~ 1%, more preferably 0.04% ~ 0.2%；
Preferably, in the step B, reaction temperature is 40 ~ 200 DEG C；When oxidant is gas, more preferably 90 ~ 100 DEG C；
When oxidant is liquid, more preferably 150-180 DEG C.
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| CN110975854B (en) * | 2019-12-19 | 2022-08-05 | 万华化学集团股份有限公司 | Catalyst for treating sulfur-containing waste alkali and preparation method and application thereof |
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| CN112076756A (en) * | 2020-10-21 | 2020-12-15 | 山东祥桓环境科技有限公司 | Preparation and application of composite metal water treatment microwave advanced oxidation catalyst |
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