CN110227534A - A kind of magnetic N doping biology Pd/carbon catalyst and preparation method thereof based on sludge - Google Patents
A kind of magnetic N doping biology Pd/carbon catalyst and preparation method thereof based on sludge Download PDFInfo
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- CN110227534A CN110227534A CN201910639362.8A CN201910639362A CN110227534A CN 110227534 A CN110227534 A CN 110227534A CN 201910639362 A CN201910639362 A CN 201910639362A CN 110227534 A CN110227534 A CN 110227534A
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- 239000010802 sludge Substances 0.000 title claims abstract description 73
- 239000003054 catalyst Substances 0.000 title claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000010865 sewage Substances 0.000 claims abstract description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- 239000002028 Biomass Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 45
- 229910052742 iron Inorganic materials 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 17
- 239000005416 organic matter Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 9
- 239000003610 charcoal Substances 0.000 claims description 8
- 230000005389 magnetism Effects 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 5
- 241001553178 Arachis glabrata Species 0.000 claims description 5
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 5
- 235000018262 Arachis monticola Nutrition 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 claims description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 5
- 235000020232 peanut Nutrition 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 229960000789 guanidine hydrochloride Drugs 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000010902 straw Substances 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 2
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 abstract description 20
- 230000015556 catabolic process Effects 0.000 abstract description 18
- 238000006731 degradation reaction Methods 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- 238000004064 recycling Methods 0.000 abstract description 10
- 239000007800 oxidant agent Substances 0.000 abstract description 8
- 230000001590 oxidative effect Effects 0.000 abstract description 8
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 4
- 238000005067 remediation Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000000498 ball milling Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 27
- 229940106691 bisphenol a Drugs 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000000975 dye Substances 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- 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 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- 238000013329 compounding Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 230000003115 biocidal effect Effects 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 230000033558 biomineral tissue development Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 229910003321 CoFe Inorganic materials 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- -1 throws sea Substances 0.000 description 2
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 1
- ZYUVGYBAPZYKSA-UHFFFAOYSA-N 5-(3-hydroxybutan-2-yl)-4-methylbenzene-1,3-diol Chemical compound CC(O)C(C)C1=CC(O)=CC(O)=C1C ZYUVGYBAPZYKSA-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910002518 CoFe2O4 Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- LSQZJLSUYDQPKJ-NJBDSQKTSA-N amoxicillin Chemical compound C1([C@@H](N)C(=O)N[C@H]2[C@H]3SC([C@@H](N3C2=O)C(O)=O)(C)C)=CC=C(O)C=C1 LSQZJLSUYDQPKJ-NJBDSQKTSA-N 0.000 description 1
- 229960003022 amoxicillin Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- NHADDZMCASKINP-HTRCEHHLSA-N decarboxydihydrocitrinin Natural products C1=C(O)C(C)=C2[C@H](C)[C@@H](C)OCC2=C1O NHADDZMCASKINP-HTRCEHHLSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- LSQZJLSUYDQPKJ-UHFFFAOYSA-N p-Hydroxyampicillin Natural products O=C1N2C(C(O)=O)C(C)(C)SC2C1NC(=O)C(N)C1=CC=C(O)C=C1 LSQZJLSUYDQPKJ-UHFFFAOYSA-N 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010801 sewage sludge Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 description 1
- 229960004306 sulfadiazine Drugs 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 239000002912 waste gas 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/39—Photocatalytic properties
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Processing Of Solid Wastes (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a kind of magnetic N doping biology Pd/carbon catalyst and preparation method thereof based on sludge belongs to recycling sludge and utilizes field and environment remediation field.The preparation method is the following steps are included: carry out ultrasonic mixing for the thickened sludge and a certain amount of nitrogen-enriched compounds and biomass castoff that city domestic sewage treatment plant, Sewage Chang Huo industrial park sewage treatment plant generate, raw material is placed in crucible after drying, ball milling and is sealed, and roasted in Muffle furnace high temperature, high catalytic activity, high stability and separation and recovery readily magnetic N doping biology Pd/carbon catalyst is finally made.The catalyst can be coupled with oxidant peroxy-monosulfate (PMS), the persistent organic pollutants in efficient degradation even mineralising water body.Preparation method provided by the invention has that raw material sources are wide, reaction condition is mild, preparation cost is low, the advantages such as environmentally protective, both the intractable sludge of sewage treatment plant and biomass castoff had been recycled, it solves the hardly degraded organic substance pollution problem in water body again, is had broad application prospects in recycling sludge using field and environment remediation field.
Description
Technical field
The present invention relates to one kind to prepare magnetic nitrogen by primary raw material of thickened sludge, nitrogen-enriched compounds and biomass castoff
Biological Pd/carbon catalyst and preparation method thereof is adulterated, belongs to recycling sludge and utilizes field and environment remediation field.
Background technique
With China's economic society development and sewage treatment facility it is perfect, specific resistance to filtration problem has become currently
One of most important environmental problem.Sludge, also because of the difference for the treatment of process, contains in addition to organic matter rich in, nitrogen and phosphorus element
There are the metallic elements such as a certain amount of iron, calcium, magnesium, manganese, many harmful substances are furthermore usually contained in sludge, such as microorganism, organic
The toxic heavy metals such as pollutant and arsenic, copper, mercury, chromium, if processing disposition not in time, it will made to mankind's activity, ecological environment
At significant damage.Traditional sludge processing method of disposal has very much, such as land use, burning, sanitary landfills, compost, throws sea, building
Material etc., but there is potential environmental risk to soil, underground water and air in these disposition.It is examined from angle of sustainable development
Consider, need to explore new processing method of disposal, to realize that sludge reuses and reduces poisonous and harmful residue to greatest extent.
In view of metallic elements, the organic matters such as organic matter rich in sludge and a large amount of iron, manganese can be used as biology
The raw material of charcoal, and the transition metal elements such as iron, manganese can be used for oxidant H2O2, peroxy-monosulfate (PMS) etc. activation.Therefore,
Waste gas purification or sewage treatment, which are prepared, as primary raw material using sludge has become the main trend that sludge is studied at this stage with catalyst,
It can be achieved " treatment of wastes with processes of wastes against one another ".Catalyst is prepared using sludge as primary raw material at present and is purified for persistent organic pollutants, it is main
Include the following three types preparation approach:
One, catalyst is directly used as after sludge high temperature roasting.For example, document " Sludge biochar-based
catalyst for improved pollutant degradation by activating peroxymonosulfate”
(6 (2018) 8978-8985 of J Mater Chem A): using sludge from wastewater treatment plant as raw material, through drying, different atmosphere
Lower high-temperature roasting, HCl- water successively wash and etc. be made sludge base charcoal, which couples with PMS can be used for dyestuff
The catalytic degradation of (such as rhodamine B) and phenolic comp ' ds pollution (such as phenol, bisphenol-A).
Two, using sludge or sludge base charcoal as carrier, Metal Supported sludge catalyst is made by compounding metallic element.
For example, document " Magnetic biochar catalyst derived from biological sludge and ferric
sludge using hydrothermal carbonization:Preparation,characterization and its
circulation in Fenton process for dyeing wastewater treatment”(Chemosphere
191 (2018) 64-71), document " Radical assisted iron impregnation on preparing sewage
sludge derived Fe/carbon as highly stable catalyst for heterogeneous Fenton
Reaction " (352 (2018) 837-846 of Chem Eng J) and patent " preparation method of magnetic sludge base ozone catalyst and
Using " (201310712765.3): by compounding iron containing sludge or ferro element in municipal sludge, through hydro-thermal or high-temperature roasting system
Magnetic iron containing sludge catalyst is obtained, and is used for the catalytic degradation of dyestuff.Patent " a kind of sludge carbon base type Fenton catalyst and its
Preparation method and application " (201710077309.4), " a kind of heterogeneous lightwave CATV catalyst of trielement composite material and its preparation
And application " (201810936719.4), " a kind of sludge prepare heterogeneous lightwave CATV catalyst method and catalyst and application "
(201810307989.9) and " method and catalyst and application that a kind of pyrolyzing sludge prepares lightwave CATV catalyst "
(201810307934.8): using the charcoal behind paper mill or sludge from wastewater treatment plant high-temperature roasting as carrier, with titanium,
In the metallic elements such as silver, manganese, iron, bismuth any one, be used as metal active constituent two or three, by ultrasonic mixing, dry
The treatment process such as dry, high-temperature roasting prepare Metal Supported sludge catalyst, can be used for heterogeneous lightwave CATV or Fenton-like
System handles persistent organic pollutants (such as dyestuff, o-chlorphenol).
Three, using sludge as carrier, N doping sludge catalyst is made by compounding nitrogenous compound.Document
“Activation of peroxymonosulfate by nitrogen-functionalized sludge carbon for
efficient degradation of organic pollutants in water”(Bioresour Technol 241
(2017) 244-251): sludge from wastewater treatment plant is dried first, is ground, it is small then to mix 24 at room temperature with urea liquid
When, drying, grind, in tube furnace lower 700 DEG C of nitrogen atmosphere roast 2 hours, HCl- water successively wash removal inorganic impurity etc. and walks
Suddenly, finally obtained N doping sludge base Pd/carbon catalyst, the catalyst can be coupled to organic pollutant (such as dyestuff, benzene with PMS
Phenol) catalytic degradation.Patent " the CoFe of activation persulfate advanced treatment on coking wastewater2O4/ N doping sludge-based activated carbon is urged
Agent and preparation method " (2019100341795): being first converted into sludge-based activated carbon for coke-oven plant's thickened sludge, then outer
Acrylamide is added, as precursor, to calcine using polymer-network gel method and Muffle furnace as the nitrate of nitrogen source, cobalt and iron
Method realizes the N doping and magnetism CoFe of sludge-based activated carbon simultaneously2O4Uniform load, be made can Magneto separate recycling
CoFe2O4/ N doping sludge-based activated carbon catalyst.
By discussed above as it can be seen that sludge base catalyst mainly uses recompounded metallic element or nitrogen in existing research
Method be made, magnetic sludge base catalyst mainly use the additional iron of sludge, cobalt element or iron containing sludge method be made.And with
Thickened sludge is primary raw material, realizes catalyst magnetization by carrying out Forms Transformation to ferro element own in thickened sludge, simultaneously
Compound a certain amount of nitrogen-enriched compounds and biomass castoff in sludge and magnetic N doping biology Pd/carbon catalyst be made, then there is not yet
Report.
Summary of the invention
The purpose of the present invention is to provide it is a kind of can be used for the degradation of hardly degraded organic substance in water body and mineralising based on sludge
Magnetic N doping biology Pd/carbon catalyst；Another object is to provide preparation method.
Purpose to realize the present invention, technical solution are as follows: with city domestic sewage treatment plant, Sewage factory or industry
The thickened sludge that garden sewage treatment plant generates is primary raw material, by compounding a certain amount of nitrogen-enriched compounds and biology wherein
Matter waste handles through ultrasonic mixing, drying, ball milling, high-temperature roasting etc., a kind of novel magnetic N doping charcoal is prepared
Catalyst.The catalyst can be coupled with oxidant PMS, the persistent organic pollutants in efficient degradation even mineralising water body.
Preparation method detailed process provided by the invention are as follows: (1) thickened sludge, nitrogen-enriched compounds, life are added in crucible
Physical obsolescence object is placed in ultrasonic cleaning machine and is uniformly mixed；(2) that mixture obtained by step (1) is dried to weight is constant, then
It moves into ball mill and is ground to 50 mesh or less；(3) mixture obtained by step (2) is moved into crucible, capping is placed on Muffle furnace
In, it is down to room temperature naturally after 300-700 DEG C of high-temperature roasting to get magnetic N doping biology Pd/carbon catalyst.
Primary raw material used is sludge, from city domestic sewage treatment plant, the industry park Sewage Chang Huo
The thickened sludge that sewage treatment plant, area generates, solid content 1-10%, the content of organic matter is 35-55%, inorganic ash in solid
Divide and be mainly made of elements such as calcium, iron, aluminium, silicon, manganese, wherein iron content is 2-10%；Auxiliary material is nitrogen-enriched compounds
And biomass castoff, wherein nitrogen-enriched compounds are any one in urea, dicyandiamide, melamine, thiocarbamide, guanidine hydrochloride
Kind, any one of biomass castoff in sawdust, straw, stalk, bark, peanut shell；Thickened sludge (in terms of solid),
The weight ratio of nitrogen-enriched compounds and biomass castoff is 1:0.05-2:0.05-2.
Application method detailed process provided by the invention are as follows: add magnetic N doping biology Pd/carbon catalyst in containing difficult to degrade
In the water body of organic matter, a certain amount of oxidant peroxy-monosulfate (PMS) is added, catalytic degradation and mineralising are carried out to organic matter, so
The recycling of catalyst can be realized by simple Magneto separate afterwards.The hardly degraded organic substance be dyestuff (such as methylene blue,
Rhodamine), phenols (such as phenol, bisphenol-A), one of antibiotic (such as sulphadiazine, Amoxicillin) or a variety of.Described urges
Agent additional amount is 0.1-1g/L, and hardly degraded organic substance concentration is 0.001-0.5mmol/L, and PMS additional amount is difficult to degrade organic
1-20 times of object concentration, solution ph 1-13.
The beneficial effects of the present invention are: (1) with city domestic sewage treatment plant, Sewage Chang Huo industrial park
The thickened sludge that sewage treatment plant generates is primary raw material, by compounding a certain amount of inexpensive, the nitrogen-enriched compounds and biology that are easy to get
Matter waste prepares the catalyst of efficient stable through simple process such as mixing, drying, grinding, high-temperature roastings, effectively solves dirty
Mud handles handling problems, reaches " turning waste into wealth "；(2) catalyst provided by the invention can be coupled with oxidant PMS, efficient degradation
The persistent organic pollutants such as dyestuff, phenols and antibiotic even in mineralising water body, and can be realized by simple Magneto separate
The recycling of catalyst efficiently solves the problems, such as organic pollution water body purification, reaches " treatment of wastes with processes of wastes against one another "；(3) present invention mentions
The preparation method of confession has that raw material sources are wide, reaction condition is mild, preparation cost is low, the advantages such as environmentally protective, both recycles
The intractable sludge of sewage treatment plant and biomass castoff, and solve the hardly degraded organic substance pollution problem in water body,
It is had broad application prospects in recycling sludge using field and environment remediation field.
Detailed description of the invention
Figure 1A figure be in 5 degradations-recycling circulation NBC-2 made from embodiment 2 to the catalytic degradation effect of bisphenol-A (with
BPA removal rate indicates) and remineralization efficacy (being indicated with TOC removal rate), the Magneto separate recycling photo that B figure is NBC-2.
Specific embodiment
It is as follows for embodiment for preferably the present invention is described in detail:
Embodiment 1
In crucible be added the municipal sewage plant 50mL thickened sludge (moisture content 97.6%, the content of organic matter 50.4%,
Inorganic ash content is mainly made of elements such as calcium, iron, aluminium, silicon, manganese, wherein iron content be 2%) with 0.06g melamine and
0.06g stalk (over dry sludge, melamine, stalk weight ratio be 1:0.05:0.05), be placed in ultrasonic cleaning machine and mix
Uniformly, it dries, be ground to 50 mesh hereinafter, mixture is placed in crucible for 105 DEG C, capping is placed in Muffle furnace, through 300 DEG C of height
Temperature roasting is down to room temperature naturally after 6 hours to get NBC-1.
20mg NBC-1 is added in methylene blue, methyl orange or rhodamine B containing 0.01-1mmol/L, is adsorbed
After balance, a certain amount of oxidant PMS is added, catalytic degradation and mineralising are carried out to organic matter.Result of study shows NBC-1 to three
The removal rate of kind dyestuff is 90% or more.
Embodiment 2
50mL papermaking sewage processing unit thickened sludge (moisture content 92.7%, the content of organic matter are added in crucible
40.8%, inorganic ash content is mainly made of elements such as calcium, iron, aluminium, silicon, manganese, and wherein iron content is 5%；) urinated with 1.825g
Element and 1.825g sawdust (over dry sludge, urea, sawdust weight ratio be 1:0.5:0.5), be placed in ultrasonic cleaning machine and mix
Uniformly, it dries, be ground to 50 mesh hereinafter, mixture is placed in crucible for 105 DEG C, capping is placed in Muffle furnace, through 550 DEG C of height
Temperature roasting is down to room temperature naturally after 3 hours to get NBC-2.
2-40mg NBC-2 is added in phenol or bisphenol-A waste water containing 0.1mmol/L, after adsorption equilibrium, is added
0.05-2mmol/L oxidant PMS carries out catalytic degradation and mineralising to organic matter.Result of study shows NBC-2 Pyrogentisinic Acid and double
The removal rate of phenol A rises with the increase of NBC-2 and PMS additional amount, and optimal N BC-2 additional amount is 0.5g/L, and optimal PMS adds
Entering amount is 1mmol/L, and the removal rate of phenol and bisphenol-A is close to 100% under optimal conditions, mineralization rate (i.e. TOC removal rate)
70% or more；In very wide ph range (pH 1-13), the efficient removal to bisphenol-A is can be achieved in NBC-2, and in solution simultaneously
The leaching of ferro element is not detected, illustrates that NBC-2 has stronger stability in very wide ph range, to solution ph
Adaptability is much better than existing Fenton or type Fenton catalyst.
Catalyst is recycled using Magneto separate, is then used further to the catalytic degradation of bisphenol-A.Result of study shows i.e.
Make through 5 degradations-recycling circulation, NBC-2 95% and 65% or more is still up to the catalysis degradation modulus and mineralization rate of bisphenol-A (see
Attached drawing 1), illustrate that magnetic N doping biology Pd/carbon catalyst provided by the invention can be used for persistent organic pollutants to stability and high efficiency
Removal.
Embodiment 3
The industrial park 50mL sewage treatment plant thickened sludge (moisture content 97.1%, the content of organic matter are added in crucible
42.2%, inorganic ash content is mainly made of elements such as calcium, iron, aluminium, silicon, manganese, wherein iron content be 7%) with 2.9g hydrochloric acid
Guanidine and 2.9g peanut shell (over dry sludge, guanidine hydrochloride, peanut shell weight ratio be 1:2:2), be placed in ultrasonic cleaning machine and mix
Uniformly, it dries, be ground to 50 mesh hereinafter, mixture is placed in crucible for 105 DEG C, capping is placed in Muffle furnace, through 700 DEG C of height
Temperature roasting is down to room temperature naturally after 1 hour to get NBC-3.
20mg NBC-3 is added in the antibiotic waste water containing 0.1mmol/L, after adsorption equilibrium, 1mmol/L oxygen is added
Agent PMS carries out catalytic degradation and mineralising to organic matter.Result of study shows NBC-3 to the removal rate of antibiotic 50%
More than.
Comparative example 1
Nitrogen-enriched compounds (urea) is not added, BC is made using preparation method same as Example 2.
20mg BC is added in the bisphenol-A waste water containing 0.1mmol/L, after adsorption equilibrium, 1mmol/L oxidant is added
PMS carries out catalytic degradation and mineralising to organic matter.Result of study shows that BC is 73% to the removal rate of bisphenol-A, and mineralization rate is (i.e.
TOC removal rate) it is 40%, far below NBC-2 to the removal effect of bisphenol-A, illustrate that N doping is remarkably improved urging for catalyst
Change activity.
Comparative example 2
600 DEG C aerobic roasting 2 hours in Muffle furnace NBC-2 prepared by embodiment 2, to remove the N doping in sample
Charcoal obtains corresponding ash content, is denoted as NBC-2-A.
20mg NBC-2-A is added in the bisphenol-A waste water containing 0.1mmol/L, after adsorption equilibrium, 1mmol/L oxygen is added
Agent PMS carries out catalytic degradation and mineralising to organic matter.Result of study shows NBC-2-A to bisphenol-A substantially without removal effect
(BPA removal rate is 15%, TOC removal rate is 6%), and sample loses magnetism after ashing, illustrates that N doping charcoal is NBC-2
Main catalytic active site, and sample magnetic (existing forms for being controlled by iron) is closely related with preparation condition.
Claims (6)
1. a kind of magnetism N doping biology Pd/carbon catalyst, which is characterized in that be prepared via a method which: (1) in crucible
Thickened sludge, nitrogen-enriched compounds and biomass castoff is added, is placed in ultrasonic cleaning machine and is uniformly mixed；(2) by step (1)
Drying to constant weight for gained mixture, then moves into ball mill and is ground to 50 mesh or less；(3) mixture obtained by step (2) is moved
Enter in crucible, capping is placed in Muffle furnace, is down to room temperature naturally after high-temperature roasting and is catalyzed to get magnetic N doping charcoal
Agent；Thickened sludge described in step (1) is originated from sewage treatment plants, Sewage Chang Huo industrial park sewage treatment
Factory, solid content 1-10%, the content of organic matter is 35-55% in solid, contains calcium, iron, aluminium, silicon, manganese element in inorganic ash content,
Wherein iron content is 2-10%；The nitrogen-enriched compounds are urea, dicyandiamide, melamine, thiocarbamide, appointing in guanidine hydrochloride
It anticipates one kind；The biomass castoff is sawdust, straw, stalk, bark, any one in peanut shell.
2. magnetism N doping biology Pd/carbon catalyst according to claim 1, which is characterized in that dense described in step (1)
Contracting sludge is in terms of solid, the weight ratio of nitrogen-enriched compounds and biomass castoff is 1:0.05-2:0.05-2.
3. magnetism N doping biology Pd/carbon catalyst according to claim 1 or 2, which is characterized in that described in step (3)
High-temperature roasting temperature is 300-700 DEG C, and calcining time is 1-6 hours.
4. preparing the preparation method of magnetic N doping biology Pd/carbon catalyst described in claim 1, which is characterized in that by such as
Lower step is realized: (1) thickened sludge, nitrogen-enriched compounds and biomass castoff being added in crucible, is placed in ultrasonic cleaning machine
It is uniformly mixed；(2) by mixture obtained by step (1), drying to constant weight, then moves into ball mill and is ground to 50 mesh or less；(3)
Mixture obtained by step (2) is moved into crucible, capping is placed in Muffle furnace, is down to room temperature naturally after high-temperature roasting, i.e.,
Obtain magnetic N doping biology Pd/carbon catalyst；Thickened sludge described in step (1) is originated from sewage treatment plants, Sewage
The industrial park Chang Huo sewage treatment plant, solid content 1-10%, the content of organic matter is 35-55%, iron in inorganic ash content in solid
Constituent content is 2-10%；The nitrogen-enriched compounds are urea, dicyandiamide, melamine, thiocarbamide, any one in guanidine hydrochloride；
The biomass castoff is sawdust, straw, stalk, bark, any one in peanut shell.
5. the preparation method of magnetism N doping biology Pd/carbon catalyst according to claim 4, which is characterized in that step (1)
Described in thickened sludge in terms of solid, the weight ratio of nitrogen-enriched compounds and biomass castoff be 1:0.05-2:0.05-2.
6. the preparation method of magnetism N doping biology Pd/carbon catalyst according to claim 4 or 5, which is characterized in that step
(3) the high-temperature roasting temperature described in is 300-700 DEG C, and calcining time is 1-6 hours.
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