CN110386711A - A kind of method of the tubular type free-radical oxidation processing of landfill leachate - Google Patents
A kind of method of the tubular type free-radical oxidation processing of landfill leachate Download PDFInfo
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- CN110386711A CN110386711A CN201910687191.6A CN201910687191A CN110386711A CN 110386711 A CN110386711 A CN 110386711A CN 201910687191 A CN201910687191 A CN 201910687191A CN 110386711 A CN110386711 A CN 110386711A
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- landfill leachate
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- tubular type
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000000149 chemical water pollutant Substances 0.000 title claims abstract description 28
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 27
- 230000003647 oxidation Effects 0.000 title claims abstract description 26
- 238000012545 processing Methods 0.000 title claims abstract description 14
- 239000010865 sewage Substances 0.000 claims abstract description 37
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 230000000694 effects Effects 0.000 claims abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 5
- 239000002638 heterogeneous catalyst Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 230000003139 buffering effect Effects 0.000 claims description 17
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 16
- 229910001868 water Inorganic materials 0.000 claims description 14
- 230000003197 catalytic effect Effects 0.000 claims description 11
- 239000012266 salt solution Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 238000009279 wet oxidation reaction Methods 0.000 claims description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- 241000196324 Embryophyta Species 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000011068 loading method Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 150000003384 small molecules Chemical class 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000005416 organic matter Substances 0.000 claims description 5
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000002525 ultrasonication Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 150000003254 radicals Chemical class 0.000 claims description 3
- 235000005979 Citrus limon Nutrition 0.000 claims description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 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
- 239000003292 glue Substances 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- 244000248349 Citrus limon Species 0.000 claims 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 claims 1
- 229910000104 sodium hydride Inorganic materials 0.000 claims 1
- 239000012312 sodium hydride Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 230000001590 oxidative effect Effects 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 239000010802 sludge Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- -1 Calcium titanate (CaTiO3) compound Chemical class 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000010813 municipal solid waste Substances 0.000 description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 4
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910002254 LaCoO3 Inorganic materials 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 238000009938 salting Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- PUKLDDOGISCFCP-JSQCKWNTSA-N 21-Deoxycortisone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)C)(O)[C@@]1(C)CC2=O PUKLDDOGISCFCP-JSQCKWNTSA-N 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- FCYKAQOGGFGCMD-UHFFFAOYSA-N Fulvic acid Natural products O1C2=CC(O)=C(O)C(C(O)=O)=C2C(=O)C2=C1CC(C)(O)OC2 FCYKAQOGGFGCMD-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 1
- 240000001085 Trapa natans Species 0.000 description 1
- 235000014364 Trapa natans Nutrition 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002306 biochemical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002509 fulvic acid Substances 0.000 description 1
- 229940095100 fulvic acid Drugs 0.000 description 1
- 239000003864 humus Substances 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000241 respiratory effect Effects 0.000 description 1
- 235000009165 saligot Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000003643 water by type Substances 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
- B01J23/84—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 arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/394—Metal dispersion value, e.g. percentage or fraction
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- 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
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The present invention provides a kind of method of the tubular type free-radical oxidation processing of landfill leachate, uses air as oxidant, occupation area of equipment is small, and longtime running is at low cost, and process safety is controllable；With the composite oxide carrier of LaMnxCo1-xO3 type perovskite feature, with the heterogeneous catalyst of nano silver active metal, catalyst reaction activity is high, it is thorough to the removal of pollutant, toxic and harmful gas is not generated in sewage disposal process, does not generate sludge, without secondary pollution, CODcr removal rate reaches as high as 92% or more, NH3-N removal rate 91% or more.
Description
Technical field
The present invention relates to sewage treatment field, in particular to the side of the tubular type free-radical oxidation processing of a kind of landfill leachate
Method.
Background technique
Garbage loading embeading is a kind of main waste treatment and disposal mode, but all can during landfill and after Closure of landfill site
Along with the generation of landfill leachate.It has been investigated that containing in percolate, there are many toxicant and carcinogens, if certainly
It degrades under the conditions of so, its COD, BOD value of 15 years time is needed to can be only achieved national emission standard, and ammonia nitrogen needs 24~26 years
Time can be only achieved national emission standard.If percolate is without processing direct emission, by serious polluted underground water, surface water
And ambient enviroment, so it is very necessary for carrying out appropriate processing to it.
Pollutant mainly has following three sources in percolate: great amount of soluble organic matter that rubbish itself contains, inorganic
Object rainwater, earth's surface smuggled goods underground water entrance during dissolve and enter percolate；Rubbish passes through biology, chemical physical action
The solable matter of generation enters percolate；Enter the solable matter of percolate in earthing and surrounding soil.The group of percolate
It is influenced at by factors such as component of refuse, weather, hydrogeology, garbage loading embeading time and land-fill methods.
Tubular type free-radical oxidation method is grown up on the basis of wet air oxidation.Wet air oxidation is beauty
Zimmer~man of state is in exploitation in 1994, also known as WAO method.The processing method that catalyst is added in WAO method is then referred to as
Tubular type free-radical oxidation method, abbreviation WACO method.It refers under high temperature (200~280 DEG C), high pressure (2~8MPa), with oxygen rich air
Body or oxygen are oxidant, using the catalytic action of catalyst, accelerate the respiratory reaction between useless Organic substance in water and oxidant, make
Organic matter in waste water and CO is oxidized to containing poisonous substances such as N, S2、N2、SO2、H2O reaches the purpose of purification.To high chemical oxygen content
Or the various industrial organic waste waters for the compound that cannot be degraded containing biochemical method, COD removal rate reach 99% or more, it is no longer necessary into
Row post-processing, only through single treatment i.e. up to discharge standard.
Catalyst is added in traditional wet oxidation system for handling, reduces the activation energy of reaction, thus not reducing place
In the case where managing effect, the temperature and pressure of reaction is reduced, the ability of oxygenolysis is improved, shortens the time of reaction, improved anti-
Efficiency is answered, and reduces the corrosion of equipment and reduces costs；The catalyst performance of wet oxidation effect heavy dependence catalyst
Perovskite refers to a kind of ceramic oxide, general molecular formula ABO3；This type oxide is found earliest, is to be present in perovskite
Calcium titanate (CaTiO3) compound in stone, therefore and gain the name.Since there are many characteristics on such compound structure, in condensed state
Physics aspect application and research are very wide, thus physicist and the chemistry daily life of a family with the ratio of each compound in its molecule formula (1:
1:3) come abbreviation, therefore also known as " 113 structure ".In cube crystalline form.In cubic crystal often with the striped of parallel crystal edge, it is
High temperature variant generates the result of multiple twin when being changed into low temperature variant.
Perovskite is with the naming of Russian geology Preosvik, and structure usually has simple perovskite knot
Structure, structure of double perovskite and laminated perovskite structure.The chemical general formula of simple perovskite compound is that wherein X is usually radius
It is lesser or, structure of double perovskite (Double-Perovskite) have composition general formula, laminated perovskite structure composition it is more multiple
Miscellaneous, studying more is with general formula and with superconducting property and tripartite's stratiform calcium titanium etc..Most study is that group becomes
Perovskite structure type compound.
The perovskite structure type compound that group becomes, affiliated crystallographic system mainly have it is orthogonal, cube, water chestnut side, four directions, monocline and
Anorthic system, A ion is usually the metallic element that rare earth or alkaline earth have larger ionic radius, it is coordinated with 12 oxygen,
Form most close cubic packing, the effect of main stabilization perovskite structure；The B generally lesser elements of ionic radius are (general
For transition metal element, such as Mn, Co, Fe), it is coordinated with 6 oxygen, the octahedra center in cubic closest packing is occupied, due to
The variability of its valence state makes it usually become the chief component for determining many properties of perovskite structure types of material.With it is simple
Oxide is compared, and perovskite structure can be such that some elements exist with improper valence state, the oxygen with non-stoichiometric, or is made
Active metal exists with mixed valence, makes solid that certain special natures be presented.Since the property of solid and its catalytic activity are close
The particularity of correlation, perovskite structure makes it be used widely in terms of catalysis.
Perovskite composite oxide ABO3 is a kind of non-gold of the novel inorganic with specific physical properties and chemical property
Belong to material, A are usually rare earth or alkaline earth element ion, and B are transition element ion, and A and B all can be similar in radius
Other ionic metal moieties replace and keep its crystal structure to be basically unchanged, therefore theoretically it be Study of Catalyst surface and
The ideal sample of catalytic performance.Since this kind of compound has stable crystal structure, unique electromagnetic performance and very high
Redox, hydrogenolysis, isomerization, electro-catalysis isoreactivity, as a kind of novel functional material, in environmental protection and Industrial Catalysis
Equal fields have very big potentiality to be exploited.
A or B is replaced by other metal ions or partially can synthesize various composite oxides after substitution in standard perovskite,
The position the B ion for forming anion defect or different valence state, be one kind have excellent performance, widely used new function material.
The complicated component of landfill leachate, it is however generally that, the organic matter in percolate can be divided into three: the low-quality fat of class
The fulvic acid substance of acids, Humus polymeric carbohydrate and intermediate molecular weight, although a certain spy in percolate
The concentration for determining pollutant is very low, but since pollutant kind is various, processing difficulty is larger, traditional processing method process flow
Complexity, occupation area of equipment is big, equipment investment and maintenance cost are big, design-production-installation period is long, it is difficult to it popularizes in an all-round way, because
This needs to improve its process equipment.
Summary of the invention
Object of the present invention is in view of the deficiencies of the prior art, provide a kind of tubular type free-radical oxidation processing of landfill leachate
Method, have catalytic activity high, the processing of the landfill leachate of complicated component can be effectively applicable to, CODcr removal rate exists
90% or more, it can qualified discharge after advanced treating
In order to achieve the above-mentioned object of the invention, the present invention provides a kind of processing of the tubular type free-radical oxidation of landfill leachate
Method, it is characterised in that this method uses tubular type continuous reaction apparatus, and described device includes filter, evaporator, sewage buffering
Tank, sewage pump, free-radical generator, condenser, air compressor machine, high-pressure buffering pot, high pressure knockout drum；The filter outlet with
Evaporator inlet is connected, and the entrance of sewage surge tank is connected with the outlet of evaporator, and outlet passes through sewage pump and freedom
The sewage inlet of base generator is connected；The air compressor machine is connected with the entrance of high-pressure buffering pot, the high-pressure buffering pot 8 outlet with
Free-radical generator is connected, and condenser is arranged in the free-radical generator exit, and condensate outlet is connected with high pressure knockout drum
It connects, the high pressure separation upper end is equipped with gas vent, and bottom is equipped with collection port；The catalyst is with LaMnxCo1-xO3 type
The composite oxide carrier of perovskite feature can be into one by nano-silver loaded with the heterogeneous catalyst of nano silver active metal
Step improves the catalytic activity of perovskite composite oxides, and the catalysis oxidation for making it be more suitable for the landfill leachate of complicated component is anti-
It answers；It is described that there is LaMnxCo1-xO3The composite oxides of type perovskite feature, wherein the range of doping (x value) be x=0~
0.2。
In use, catalyst is pre-loaded in free-radical generator, landfill leachate is removed by filter big first
Solid particle, then since the concentration of landfill leachate is lower, thus filter after import evaporator in be concentrated after imported into again
In sewage surge tank, the treatment sewage in cesspool is pumped by free-radical generator by sewage pump, passes through sky at the same time
Press conveying high-pressure air into high-pressure buffering pot conveys after pressure is stable and reaches preset value into free-radical generator
Pressure-air, treatment sewage is sent out under the effect of the catalyst with the air from high-pressure buffering pot in free-radical generator 5
Raw wet oxidation reaction, larger molecular organics under the conditions of certain pressure and temperature in free-radical generator in sewage are strong
Oxidizing decomposition, the double bond fracture in organic constitution, is oxidized to small molecule by macromolecular, small molecule is further oxidized to
Carbon dioxide and water, the sewage of purification enter high pressure knockout drum after flowing into condenser cooling by free-radical generator water outlet,
Uncooled gas point is vented by gas vent, and liquid is collected by collection port.
Preferably, 130~210 DEG C, 2.2~3.5MPa of reaction pressure of the reaction temperature, liquid air speed 0.7~
3.6h-1, 50~400ml/min of oxygen or air velocity.
Method for preparing catalyst of the invention includes the following steps:
Method for preparing catalyst of the present invention includes the following steps:
1) soluble-salt of the soluble-salt of lanthanum, the soluble-salt of manganese and cobalt is stoichiometrically weighed, and is dissolved in certain
In the deionized water of amount, configure mixed salt solution, be then added a certain amount of citric acid, stirring to be completely dissolved to be formed it is molten
Glue；
2) colloidal sol is dried into moisture, be cooled to room temperature, be fully ground sieving；
3) powder after sieving is added in calciner plant, under air atmosphere, carries out microwave heating calcining to get having
The composite oxide carrier of LaMnxCo1-xO3 type perovskite feature；
4) soluble-salt for weighing a certain amount of silver is dissolved in a certain amount of deionized water, is configured to silver salt solution；It weighs
A certain amount of polyvinylpyrrolidone is dissolved in deionized water, is configured to PVP solution；
5) it under agitation by PVP solution, is added dropwise in anion solutions, obtains mixed solution, step is then added
The composite oxide carrier of rapid 3) the middle LaMnxCo1-xO3 type perovskite feature prepared, ultrasonication 10~after twenty minutes,
Sodium borohydride solution is added, after reaction 1~3 hour, filtering, deionized water are washed till neutrality, are drying to obtain composite catalyst.
Preferably, the molar ratio of lemon mangaic acid and metal ion in mixed salt solution is 2-3:1 in step 1).
Preferably, the drying temperature in step 2) be 80~110 DEG C, be sieved for 80 meshes.
Preferably, in step 3), the power of microwave is in 1500w~2000w, and heating temperature is at 900~1100 DEG C, heating
Between be 2~5 minutes.
Preferably, the concentration of silver ion is 0.02~0.1mol/L in step 4), the concentration of PVP solution is 0.01~
0.05g/mL, PVP additional amount are the 1%~2% of carrier quality.
Preferably, the additional amount of sodium borohydride is 1.1 to 1.5 times of silver ion mole in step 5).
Preferably, the drying process of step 5) is, in a vacuum drying oven, 3~5 hours dry at 100~120 DEG C.
The effect of tubular type free-radical oxidation depends primarily on the activity of catalyst, and perovskite type oxide class is urged
For the activity of agent, the catalyst of the important influence factor of synthesis technology, different preparation method preparations usually has difference
Structure, form, granularity, specific surface area and catalytic activity, and the perovskite type catalyst being prepared using the present invention, catalysis
The partial size of agent is smaller, disperses more uniform, and specific surface area is bigger, and performance is more stable, and catalytic activity is into one after loading nano silvery
Step is promoted so that catalyst prepared by the present invention has better catalytic activity to the landfill leachate of complicated component, can compared with
Low temperature, compared under the conditions of low oxygen partial pressure realize complicated component landfill leachate wet oxidation.
Compared with prior art, beneficial effects of the present invention:
1) technique of the invention uses air as oxidant, and occupation area of equipment is small, and longtime running is at low cost, process peace
It is complete controllable；Convenient and practical, catalyst reaction activity is high, thorough to the removal of pollutant, does not generate in sewage disposal process toxic
Pernicious gas does not generate sludge, without secondary pollution.
2) composite catalyst of the invention during the preparation process, prepares LaMnxCo1-xO3 type perovskite using microwave sintering
The composite oxides of feature are smaller as the partial size of carried catalyst, and dispersion is more uniform, and specific surface area is bigger, and performance is more steady
It is fixed, synergistic effect is produced by loading nano silvery ion and carrier and substantially increases catalytic performance.The present invention is efficient, stable
Catalyst changes the course of wet oxidation reaction, and temperature and pressure needed for greatly reducing oxidation reaction simultaneously improves processing
Effect improves oxidation efficiency, and COD of waste leachate cr removal rate is in 90% or more, NH3-N removal rate 91% or more.
Detailed description of the invention
Fig. 1 is tubular type continuous reaction apparatus of the present invention
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
It is as shown in Figure 1 tubular type free-radical oxidation processing unit of the invention, described device includes filter 1, evaporator
2, sewage surge tank 3, sewage pump 4, free-radical generator 5, condenser 6, air compressor machine 7, high-pressure buffering pot 8, high pressure knockout drum 9；
The outlet of filter 1 is connected with 2 entrance of evaporator, the outlet phase of the entrance and evaporator 2 of the sewage surge tank 4
Even, outlet is connected by sewage pump 4 with the sewage inlet of free-radical generator 5；The air compressor machine 7 enters with high-pressure buffering pot 8
Mouth is connected, and the outlet of high-pressure buffering pot 8 is connected with free-radical generator 5, and 5 exit of the free-radical generator setting is cold
Condenser 6, condensate outlet are connected with high pressure knockout drum 9, and 9 top of high pressure knockout drum is equipped with gas vent, and bottom, which is equipped with, collects
Mouthful.
In use, catalyst is pre-loaded in free-radical generator 5, landfill leachate is removed by filter big first
Solid particle, thus filter after import evaporator 2 in be concentrated after imported into sewage surge tank 3 again, will be dirty by sewage pump 4
Treatment sewage in pond is pumped into free-radical generator 5, passes through air compressor machine conveying high-pressure into high-pressure buffering pot 8 at the same time
Air, after pressure is stable and reaches preset value, the conveying high-pressure air into free-radical generator 5, in free-radical generator 5
Wet oxidation reaction occurs under the effect of the catalyst for treatment sewage and the air from high-pressure buffering pot 8, in certain pressure
With the larger molecular organics under the conditions of temperature in free-radical generator 1 in sewage by strong oxidizer oxygenolysis, organic matter knot
Double bond fracture in structure, is oxidized to small molecule by macromolecular, small molecule is further oxidized to carbon dioxide and water, makes COD substantially
It spends decline BOD/COD value to improve, the sewage of purification enters height after flowing into the cooling of condenser 6 by 5 water outlet of free-radical generator
Knockout drum 7 is pressed, uncooled gas point is vented by gas vent, and liquid is collected by collection port.
[embodiment 1]
1) 1mol lanthanum nitrate, 0.2mol manganese nitrate and 0.8mol cobalt nitrate are stoichiometrically weighed, and be dissolved in 5L go from
In sub- water, mixed salt solution is configured, 2.5mol citric acid is then added, stirring to form colloidal sol to being completely dissolved；
2) colloidal sol is dried into moisture at 100 DEG C, be cooled to room temperature, be fully ground 80 meshes；
3) powder after sieving is added in calciner plant, under air atmosphere, carries out microwave heating calcining, the power of microwave
In 1500ww, for heating temperature at 900 DEG C, heating time is 5 minutes to get with LaMn0.2Co0.8O3 type perovskite feature
Composite oxide carrier；
4) nitric acid for weighing 0.1mol is dissolved in 500mL deionized water, is configured to silver salt solution；Weigh 0.5g polyethylene pyrrole
Pyrrolidone is dissolved in 10mL deionized water, is configured to PVP solution；
5) it under agitation by PVP solution, is added dropwise in anion solutions, obtains mixed solution, 50g is then added
The composite oxide carrier of the LaMn0.2Co0.8O3 type perovskite feature prepared in step 3), ultrasonication after ten minutes,
The sodium borohydride of 0.12mol is added, after reaction 2 hours, filtering, deionized water is washed till neutrality, is then placed in vacuum oven,
At 120 DEG C, dry 5 hours up to composite catalyst A1.
[embodiment 2]
1) 1mol lanthanum nitrate, 0.1mol manganese nitrate and 0.9mol cobalt nitrate are stoichiometrically weighed, and be dissolved in 5L go from
In sub- water, mixed salt solution is configured, 2.2mol citric acid is then added, stirring to form colloidal sol to being completely dissolved；
2) colloidal sol is dried into moisture at 100 DEG C, be cooled to room temperature, be fully ground 80 meshes；
3) powder after sieving is added in calciner plant, under air atmosphere, carries out microwave heating calcining, the power of microwave
In 2000ww, for heating temperature at 1100 DEG C, heating time is 3 minutes to get with LaMn0.1Co0.9O3 type perovskite feature
Composite oxide carrier；
4) nitric acid for weighing 0.1mol is dissolved in 500mL deionized water, is configured to silver salt solution；Weigh 1.0g polyethylene pyrrole
Pyrrolidone is dissolved in 15mL deionized water, is configured to PVP solution；
5) it under agitation by PVP solution, is added dropwise in anion solutions, obtains mixed solution, 50g is then added
The composite oxide carrier of the LaMn0.1Co0.9O3 type perovskite feature prepared in step 3), after ultrasonication 15 minutes,
The sodium borohydride of 0.15mol is added, after reaction 2 hours, filtering, deionized water are washed till neutrality, are then placed in vacuum oven,
At 120 DEG C, dry 3 hours up to composite catalyst A2.
[comparative example 1]
1) 1mol lanthanum nitrate, 1mol cobalt nitrate are stoichiometrically weighed, and is dissolved in 5L deionized water, configuration mixing gold
Belong to salting liquid, 2.5mol citric acid is then added, stirring to form colloidal sol to being completely dissolved；
2) colloidal sol is dried into moisture at 100 DEG C, be cooled to room temperature, be fully ground 80 meshes；
3) powder after sieving is added in calciner plant, under air atmosphere, carries out microwave heating calcining, the power of microwave
In 1500ww, for heating temperature at 900 DEG C, heating time is 5 minutes to get the combined oxidation with LaCoO3 type perovskite feature
Object carrier；
4) nitric acid for weighing 0.1mol is dissolved in 500mL deionized water, is configured to silver salt solution；Weigh 0.5g polyethylene pyrrole
Pyrrolidone is dissolved in 10mL deionized water, is configured to PVP solution；
5) it under agitation by PVP solution, is added dropwise in anion solutions, obtains mixed solution, 50g is then added
The composite oxide carrier of the LaCoO3 type perovskite feature prepared in step 3), ultrasonication after ten minutes, are added
The sodium borohydride of 0.12mol, after reaction 2 hours, filtering, deionized water is washed till neutrality, is then placed in vacuum oven, and 120
At DEG C, dry 5 hours up to composite catalyst B1.
[comparative example 2]
1) 1mol lanthanum nitrate, 1mol cobalt nitrate are stoichiometrically weighed, and is dissolved in 5L deionized water, configuration mixing gold
Belong to salting liquid, 2.5mol citric acid is then added, stirring to form colloidal sol to being completely dissolved；
2) colloidal sol is dried into moisture at 100 DEG C, be cooled to room temperature, be fully ground 80 meshes；
3) powder after sieving is added in calciner plant, under air atmosphere, carries out microwave heating calcining, the power of microwave
In 1500ww, for heating temperature at 900 DEG C, heating time is 5 minutes to get the combined oxidation with LaCoO3 type perovskite feature
Object C1.
[embodiment 3]
The processing of sample sewage:
Sample sewage is garbage loading embeading factory landfill leachate, as follows through detection main indicator:
Color: black；PH value is 4.2；COD main component is piperidines ketone compounds, and CODcr is in 45220mg/L；Coloration
9000 times；Organic acid 2120mg/L；NH3-N is 4320mg/L.
Device as shown in Figure 1, the beaded catalyst that embodiment 1-2 and comparative example 1-2 are prepared are packed into free radical hair
In catalyst bed in raw device 1, the pressure for adjusting air compressor machine and high-pressure buffering pot reaches setting pressure 3.5Mpa, heating
It rises to 250 DEG C with free-radical generator, and air and sample sewage are fed into free-radical generator together, from reaction after 3 hours
Liquid, carries out COD test analysis, and the removal rate of COD is shown in Table 1.
Table 1
Above description sufficiently discloses a specific embodiment of the invention.It should be pointed out that being familiar with the field
Range of any change that technical staff does a specific embodiment of the invention all without departing from claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (8)
1. the method that a kind of tubular type free-radical oxidation of landfill leachate is handled, which is characterized in that a kind of pipe of landfill leachate
The method of formula free-radical oxidation processing, it is characterised in that this method uses tubular type continuous reaction apparatus, and described device includes filtering
Device, evaporator, sewage surge tank, sewage pump, free-radical generator, condenser, air compressor machine, high-pressure buffering pot, high pressure knockout drum；
The filter outlet is connected with evaporator inlet, and the entrance of sewage surge tank is connected with the outlet of evaporator, out
Mouth is connected by sewage pump with the sewage inlet of free-radical generator；The air compressor machine is connected with the entrance of high-pressure buffering pot, institute
It states high-pressure buffering pot outlet to be connected with free-radical generator, condenser is arranged in the free-radical generator exit, is condensed out
Mouth is connected with high pressure knockout drum, and the high pressure separation upper end is equipped with gas vent, and bottom is equipped with collection port；The free radical
Loading catalyst is with LaMn in generatorxCo1-xO3The composite oxide carrier of type perovskite feature, with nano silver active metal
Heterogeneous catalyst, can further improve the catalytic activity of perovskite composite oxides by nano-silver loaded, keep it more applicable
In the catalytic oxidation of the landfill leachate of complicated component, wherein the range of x value is x=0~0.2.
2. the method that the tubular type free-radical oxidation of landfill leachate according to claim 1 is handled, which is characterized in that catalysis
Agent is pre-loaded in free-radical generator, and landfill leachate passes through filter first and removes big solid particle, then due to
The concentration of landfill leachate is lower, thus imports after filtering in evaporator and imported into sewage surge tank again after concentration, passes through dirt
Treatment sewage in cesspool is pumped into free-radical generator by water pump, defeated into high-pressure buffering pot by air compressor machine at the same time
Pressure-air is sent, after pressure is stable and reaches preset value, the conveying high-pressure air into free-radical generator occurs in free radical
Wet oxidation reaction occurs under the effect of the catalyst for treatment sewage and the air from high-pressure buffering pot in device 5, certain
Larger molecular organics under the conditions of pressure and temperature in free-radical generator in sewage are by strong oxidizer oxygenolysis, organic matter
Double bond fracture in structure, is oxidized to small molecule by macromolecular, small molecule is further oxidized to carbon dioxide and water, the dirt of purification
Water is flowed into after condenser cooling by free-radical generator water outlet enters high pressure knockout drum, and uncooled gas point is by gas vent
Emptying, liquid are collected by collection port.
3. the method that the tubular type free-radical oxidation of landfill leachate according to claim 1 is handled, which is characterized in that described
130~210 DEG C of reaction temperature, 2.2~3.5MPa of reaction pressure, liquid 0.7~3.6h-1 of air speed, oxygen or air velocity 50
~400ml/min.
4. the method that the tubular type free-radical oxidation of landfill leachate according to claim 1 is handled, which is characterized in that described
Method for preparing catalyst include the following steps:
1) soluble-salt of the soluble-salt of lanthanum, the soluble-salt of manganese and cobalt is stoichiometrically weighed, and is dissolved in a certain amount of
In deionized water, configure mixed salt solution, be then added a certain amount of citric acid, stirring to be completely dissolved to be formed it is molten
Glue；
2) colloidal sol is dried into moisture, be cooled to room temperature, be fully ground sieving；
3) powder after sieving is added in calciner plant, under air atmosphere, carries out microwave heating calcining to get having
LaMnxCo1-xO3The composite oxide carrier of type perovskite feature；
4) soluble-salt for weighing a certain amount of silver is dissolved in a certain amount of deionized water, is configured to silver salt solution；It weighs certain
The polyvinylpyrrolidone of amount is dissolved in deionized water, is configured to PVP solution；
5) it under agitation by PVP solution, is added dropwise in anion solutions, obtains mixed solution, step 3) is then added
The LaMn of middle preparationxCo1-xO3The composite oxide carrier of type perovskite feature, ultrasonication 10~after twenty minutes, boron is added
Sodium hydride solution, after reaction 1~3 hour, filtering, deionized water are washed till neutrality, are drying to obtain composite catalyst.
5. the method that the tubular type free-radical oxidation of landfill leachate according to claim 4 is handled, which is characterized in that step
1) molar ratio of lemon mangaic acid and metal ion in mixed salt solution is 2-3:1 in；Drying temperature in step 2) is 80
~110 DEG C, be sieved for 80 meshes.
6. the method that the tubular type free-radical oxidation of landfill leachate according to claim 4 is handled, which is characterized in that step
3) in, the power of microwave is in 1500w~2000w, and for heating temperature at 900~1100 DEG C, heating time is 2~5 minutes.
7. the method that the tubular type free-radical oxidation of landfill leachate according to claim 4 is handled, which is characterized in that step
4) concentration of silver ion is 0.02~0.1mol/L in, and the concentration of PVP solution is 0.01~0.05g/mL, and PVP additional amount is to carry
The 1%~2% of weight.
8. the method that the tubular type free-radical oxidation of landfill leachate according to claim 4 is handled, which is characterized in that step
5) additional amount of sodium borohydride is 1.1 to 1.5 times of silver ion mole in；The drying process of step 5) are as follows: be dried in vacuo
It is 3~5 hours dry at 100~120 DEG C in case.
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