CN107879583A - Sludge pyrohydrolysis and anaerobic digestion integrated treatment process system - Google Patents
Sludge pyrohydrolysis and anaerobic digestion integrated treatment process system Download PDFInfo
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- CN107879583A CN107879583A CN201711411044.3A CN201711411044A CN107879583A CN 107879583 A CN107879583 A CN 107879583A CN 201711411044 A CN201711411044 A CN 201711411044A CN 107879583 A CN107879583 A CN 107879583A
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- 239000010802 sludge Substances 0.000 title claims abstract description 193
- 238000000034 method Methods 0.000 title claims abstract description 56
- 230000029087 digestion Effects 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 72
- 239000007789 gas Substances 0.000 claims abstract description 44
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 43
- 230000003647 oxidation Effects 0.000 claims abstract description 37
- 238000003860 storage Methods 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 230000003197 catalytic effect Effects 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims description 125
- OMOVVBIIQSXZSZ-UHFFFAOYSA-N [6-(4-acetyloxy-5,9a-dimethyl-2,7-dioxo-4,5a,6,9-tetrahydro-3h-pyrano[3,4-b]oxepin-5-yl)-5-formyloxy-3-(furan-3-yl)-3a-methyl-7-methylidene-1a,2,3,4,5,6-hexahydroindeno[1,7a-b]oxiren-4-yl] 2-hydroxy-3-methylpentanoate Chemical compound CC12C(OC(=O)C(O)C(C)CC)C(OC=O)C(C3(C)C(CC(=O)OC4(C)COC(=O)CC43)OC(C)=O)C(=C)C32OC3CC1C=1C=COC=1 OMOVVBIIQSXZSZ-UHFFFAOYSA-N 0.000 claims description 108
- 239000000463 material Substances 0.000 claims description 90
- 239000007788 liquid Substances 0.000 claims description 84
- 238000001035 drying Methods 0.000 claims description 77
- 229910052799 carbon Inorganic materials 0.000 claims description 64
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 62
- 235000019441 ethanol Nutrition 0.000 claims description 38
- 238000005406 washing Methods 0.000 claims description 30
- -1 3,3'- dihydroxybiphenyl amine Chemical class 0.000 claims description 22
- 229910052708 sodium Inorganic materials 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 18
- NQSMEZJWJJVYOI-UHFFFAOYSA-N Methyl 2-benzoylbenzoate Chemical class COC(=O)C1=CC=CC=C1C(=O)C1=CC=CC=C1 NQSMEZJWJJVYOI-UHFFFAOYSA-N 0.000 claims description 15
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 15
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical class [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims description 15
- 125000005498 phthalate group Chemical class 0.000 claims description 15
- 229910052700 potassium Inorganic materials 0.000 claims description 15
- 239000011591 potassium Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 14
- IRSIKJPEFMMRHD-UHFFFAOYSA-N 2-butyl-3-methylpyrazine Chemical class CCCCC1=NC=CN=C1C IRSIKJPEFMMRHD-UHFFFAOYSA-N 0.000 claims description 12
- 239000003643 water by type Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 6
- 239000006260 foam Substances 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 4
- SKDNDSLDRLEELJ-UHFFFAOYSA-N 2,3,5-tribromothiophene Chemical class BrC1=CC(Br)=C(Br)S1 SKDNDSLDRLEELJ-UHFFFAOYSA-N 0.000 claims description 3
- OTZUKTGQTUYRCH-UHFFFAOYSA-N 2-bromo-3-chloropyrazine Chemical class ClC1=NC=CN=C1Br OTZUKTGQTUYRCH-UHFFFAOYSA-N 0.000 claims description 3
- BOGKTBKWDIUAGK-UHFFFAOYSA-N 2-fluoro-4-nitropyridine Chemical class [O-][N+](=O)C1=CC=NC(F)=C1 BOGKTBKWDIUAGK-UHFFFAOYSA-N 0.000 claims description 3
- FJZRUSFQHBBTCC-UHFFFAOYSA-N 2-oxo-1h-pyrazine-3-carboxylic acid Chemical class OC(=O)C1=NC=CNC1=O FJZRUSFQHBBTCC-UHFFFAOYSA-N 0.000 claims description 3
- BXEAAHIHFFIMIE-UHFFFAOYSA-N 3-chlorothiophene-2-carboxylic acid Chemical class OC(=O)C=1SC=CC=1Cl BXEAAHIHFFIMIE-UHFFFAOYSA-N 0.000 claims description 3
- VGJLGPCXUGIXRQ-UHFFFAOYSA-N 3-methylpyridin-4-amine Chemical class CC1=CN=CC=C1N VGJLGPCXUGIXRQ-UHFFFAOYSA-N 0.000 claims description 3
- NDPKVJZZCMFBIO-UHFFFAOYSA-N 5-methylpyridazin-3-amine Chemical compound CC1=CN=NC(N)=C1 NDPKVJZZCMFBIO-UHFFFAOYSA-N 0.000 claims description 3
- QGWZOYKTNMWCJG-UHFFFAOYSA-N COC(=O)C=1SC=CC1.CC=1C=CC=CC1 Chemical class COC(=O)C=1SC=CC1.CC=1C=CC=CC1 QGWZOYKTNMWCJG-UHFFFAOYSA-N 0.000 claims description 3
- PESZCXUNMKAYME-UHFFFAOYSA-N Citroflex A-4 Chemical class CCCCOC(=O)CC(O)(C(=O)OCCCC)C(C(C)=O)C(=O)OCCCC PESZCXUNMKAYME-UHFFFAOYSA-N 0.000 claims description 3
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 3
- DNSISZSEWVHGLH-UHFFFAOYSA-N butanamide Chemical class CCCC(N)=O DNSISZSEWVHGLH-UHFFFAOYSA-N 0.000 claims description 3
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- VNFXNPFSTYYFCZ-UHFFFAOYSA-N methyl 6-oxo-1h-pyrazine-3-carboxylate Chemical class COC(=O)C1=CN=C(O)C=N1 VNFXNPFSTYYFCZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 239000011344 liquid material Substances 0.000 claims 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 2
- 238000007654 immersion Methods 0.000 claims 2
- 229910052760 oxygen Inorganic materials 0.000 claims 2
- 239000001301 oxygen Substances 0.000 claims 2
- 239000000203 mixture Substances 0.000 abstract description 13
- 238000012545 processing Methods 0.000 abstract description 6
- 239000010865 sewage Substances 0.000 abstract description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 2
- 239000002585 base Substances 0.000 description 18
- 239000005416 organic matter Substances 0.000 description 15
- 230000007062 hydrolysis Effects 0.000 description 14
- 238000006460 hydrolysis reaction Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 8
- 102000004169 proteins and genes Human genes 0.000 description 7
- 108090000623 proteins and genes Proteins 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 244000005700 microbiome Species 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 150000001413 amino acids Chemical class 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 238000005189 flocculation Methods 0.000 description 4
- 230000016615 flocculation Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000001720 carbohydrates Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000004676 glycans Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 108010016626 Dipeptides Proteins 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical group 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 230000003834 intracellular effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 244000052769 pathogen Species 0.000 description 2
- 230000001717 pathogenic effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920001184 polypeptide Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 108090000765 processed proteins & peptides Proteins 0.000 description 2
- 102000004196 processed proteins & peptides Human genes 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- WWLFISHRFXUAOE-UHFFFAOYSA-N 4-bromopyridazine-3,6-dione Chemical class BrC1=CC(=O)N=NC1=O WWLFISHRFXUAOE-UHFFFAOYSA-N 0.000 description 1
- WRVHQEYBCDPZEU-UHFFFAOYSA-N 4-chloro-6,7-dimethoxyquinoline Chemical class C1=CC(Cl)=C2C=C(OC)C(OC)=CC2=N1 WRVHQEYBCDPZEU-UHFFFAOYSA-N 0.000 description 1
- 108091028026 C-DNA Proteins 0.000 description 1
- 241000256113 Culicidae Species 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 238000009412 basement excavation Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
- 238000011026 diafiltration Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000001079 digestive effect Effects 0.000 description 1
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- 239000012895 dilution Substances 0.000 description 1
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- 230000005611 electricity Effects 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 210000004681 ovum Anatomy 0.000 description 1
- 244000045947 parasite Species 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000009790 rate-determining step (RDS) Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000010801 sewage sludge Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000003516 soil conditioner Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003911 water pollution Methods 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
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/02—Biological treatment
- C02F11/04—Anaerobic treatment; Production of methane by such processes
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/36—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of vanadium, niobium or tantalum
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/06—Treatment of sludge; Devices therefor by oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/122—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using filter presses
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/06—Sludge reduction, e.g. by lysis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Molecular Biology (AREA)
- Health & Medical Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a kind of sludge pyrohydrolysis and anaerobic digestion integrated treatment process system, the process system is by entering mud sump, sludge pipe, enter dredge pump, sludge concentrator, pulp tank, stirring vane, agitating shaft, temperature sensor, stirring motor, pressure sensor, pyrohydrolysis retort, it is filled with the pyrohydrolysis catalysing tube of nickel-base catalyst, steam generator, pressure release tank, steam storage tank, advanced oxidation retort, ozonizer, it is filled with the ozone catalytic pipe of Ti-base catalyst, ozone generator, digester, plate and frame filter press, go out mud sump, methane gas connecting tube and methane gas storage tank composition.The invention has the advantages that the processing that the sludge pyrohydrolysis and anaerobic digestion integrated treatment process system are applied to sludge had into the advantages such as energy consumption is low, killing germ ability is strong, dewatering performance of sludge is good, dewatered sludge yield is few, methane in sewage gas gas content is high, hydrogen sulfide content is low.
Description
Technical field
The invention belongs to technical field of sludge treatment, more particularly to sludge pyrohydrolysis and anaerobic digestion integrated treatment process system
System.
Background technology
Sludge is the accessory substance in sewage disposal process, has the characteristics that moisture content is high, particle is relatively thin, proportion is lighter, its
In contain the material such as a large amount of organic matters, nitrogen phosphorus, pathogenic microorganism, parasitic ovum and virus, heavy metal ion.Organic matter in sludge
It is perishable and produce stench, the easy raw mosquitos and flies of evil；The nutriments such as nitrogen, phosphorus can flow into earth's surface or underground under rainwash
Water body, cause water pollution；When sludge untreated or that processing is not up to standard is used as agricultural fertilizer or landfill, pathogen and parasite etc. enter
Enter soil, and it is direct or indirect contacted with human or animal, harmful to human and animal health；Heavy metal ion and difficult degradation have
Easily diafiltration comes out or volatilized malicious harmful substance, causes the secondary pollution of water body, soil and air.
The target of specific resistance to filtration is to realize the minimizing of sludge, innoxious, stabilisation and recycling.Municipal sludge contains
Water rate is universal higher, typically more than 95%, causes sludge volume very big, is unfavorable for storing and transports, therefore minimizing ten
It is point important, moisture percentage in sewage sludge can be reduced by the mode such as concentrating, being dehydrated, sludge volume is effectively reduced, is readily transported and digests,
Reduce the expense of specific resistance to filtration；Contain a large amount of harmful substances in sludge, by processing, the organic matter in sludge of degrading, go
Removing heavy metals, suppressing or kill pathogen etc., sludge quality is stable, safe and healthy after final disposal, does not decompose further,
So as to avoid producing secondary pollution；Contain nutriment in a fertilizer, soil conditioner and the micro member needed for the plants such as abundant nitrogen, phosphorus in sludge
Element etc., while the organic substance in sludge, are potential regenerative resource materials, and cleaning energy can be converted into by anaerobic digestion
Source --- biogas.Therefore, if can be dealt carefully with sludge and rationally utilized, it will reaching turns waste into wealth, comprehensively utilizes, protecting
The purpose in retaining ring border.
Most of organic matter of sludge exists in solid form, is concentrated mainly in microbial cell, because microorganism is thin
The natural cover for defense effect of cell wall (film), hydrolase is very low to the hydrolysis rate of organic matter, therefore hydrolysis is the biochemical drop of sludge anaerobic
The rate-determining steps of solution.Hydrolysis rate slowly causes that anaerobic digestion hydraulic detention time is very long, and reactor volume is too big.Last 100 yearses
Come, anaerobic sludge digestion technology is constantly ripe, technological process gradual perfection, however, the low property of sludge hydrolytic speed is from basic
On fettered the further excavations of anaerobic digestion potentiality.Therefore, anaerobic sludge digestion efficiency is improved, it is necessary to improve complicated organic
The hydrolysis rate of thing.To solve this problem, people, which begin one's study, can effectively crush sludge flco and cyto-architectural physics
Chemical pretreatment techniques, the hydrolysis rate of complicated organic matter is improved by these preconditioning techniques, improve the property of sludge, and then
Subsequent anaerobic digestion efficiency and biogas output are improved, realizes minimizing and the recycling of sludge, thus it is more and more each by the world
The attention of state.Studying more sludge pre-treatment techniques at present has pyrohydrolysis pretreatment, Mechanical Crushing pretreatment, alkali process, super
Sound wave pretreatment, ozone pretreatment, ferment treatment, Microwave Pretreatment etc..Before the 1980s, pyrohydrolysis is mainly used
In the dewatering for improving sludge；The eighties rise, and pyrohydrolysis is used for the anaerobic digestion performance for improving sludge；After the nineties,
Pyrohydrolysis is used to obtain the carbon source needed for denitrification and the mud decrement based on recessive growth.With not being broken into for pyrohydrolysis technology
Ripe and development, present pyrohydrolysis have developed into a kind of efficient sludge pre-treatment techniques.
Pyrohydrolysis is that pending sludge is placed in closed container tank, makes sludge under certain temperature and pressure environment
In part cell body expanded by heating and rupture, destroy the cell membrane (film) of microorganism, intracellular protein and colloid etc. is organic
Thing discharges, and promotes the dissolving and hydrolysis of organic matter：Fat splitting is into glycerine and aliphatic acid；Carbohydrate inversion Cheng little Fen
The polysaccharide of son, or even monose；Protein is hydrolyzed into polypeptide, dipeptides, amino acid, and it is organic that amino acid is further hydrolyzed to low molecule
Acid, ammonia and carbon dioxide.Sludge is after pyrohydrolysis pretreatment, and the microorganism flco in sludge disintegrates, and microbial cell is broken
Broken, the inclusion in cell discharges an one-step hydrolysis of going forward side by side so that the organic removal rate of anaerobic sludge digestion improves, methane production
Increase, the dewatering of sludge improve.
Sludge pyrohydrolysis process includes the dissolving of solid matter and the hydrolysis of organic matter.Following 4 can be specifically subdivided into
Process：Plum occurs for disintegration, sludge clasmatosis and the release of organic matter of sludge flocculation structure, the hydrolysis of organic matter and organic matter
Maillard reaction.(1) sludge flocculation structure disintegrates：After sludge is heated, the hydrogen bond in the extracellular polymeric structure on its flco and surface
It is destroyed, cause flocculation structure to disintegrate, organic matter is dissolved and is transferred in liquid phase, while the Interstitial Water in flocculation structure is released
Out, free water is turned into.(2) sludge clasmatosis and organic matter release：With the rise of temperature and pressure, microorganism in sludge
Eucaryotic cell structure be destroyed, and then the organic compound such as clasmatosis, protein, carbohydrate and the lipid of intracellular is released
Out, and it is converted into dissolved matter.(3) hydrolysis of organic matter：The organic matter being dissolved out from sludge flco and into the cell,
Hydrolyzed in pyrohydrolysis process, generate dissolubility intermediate product：Fat splitting is into glycerine and aliphatic acid；Carbohydrate inversion
Into the polysaccharide of small molecule, or even monose；Protein is hydrolyzed into polypeptide, dipeptides, amino acid, and amino acid is further hydrolyzed to low molecule
Organic acid, ammonia and carbon dioxide.(4) mailland reaction：It is the condensation reaction between amino-compound and carbonyls, generation
A kind of intermediate product (Melanoidins) for being difficult to biochemical degradation, when pyrohydrolysis temperature is more than 190 DEG C, mailland reaction starts
Existing, temperature is higher, and reaction is more violent.The generation of Melanoidins weakens the treatment effect of pyrohydrolysis to a certain extent, causes dirt
Mud digestic property declines.
Sludge pyrohydrolysis pretreatment can be divided into Cold pretreatment (<100 DEG C) and high temperature pretreatment (>100 DEG C), temperature
Difference can cause the difference at cytoclasis position, and microorganism extracellular polymeric can dissolve in heat treatment process, protein and
Nucleic acid equimolecular also can be denatured and destroy, and at 45~65 DEG C, cell membrane can rupture, and rRNA goes to pot；At 50~70 DEG C
DNA is destroyed；The cell wall rupture at 65~90 DEG C；Protein will be denatured at 70~95 DEG C.Pyrohydrolysis temperature is from 80 DEG C
When being increased to 100 DEG C, the burst size of polysaccharide and total organic carbon increases, and the burst size of protein is reduced.Can be by carefully during heating
The material that born of the same parents discharge is divided into two classes：Dissolved organic carbon and carboxylic acid fragment, biology can be broken using the carboxylic acid of small-molecular-weight quickly
Piece, and the former degradation property is then much lower.Discovery is compared to the pyrohydrolysis pretreating effect of 135 DEG C and 190 DEG C, no matter
It is the dissolution of total COD or lipid etc., pretreating effect at 190 DEG C is considerably better than effect at 135 DEG C.
The major influence factors of pyrohydrolysis pretreating effect contain including reaction temperature, reaction pressure, processing time and sludge
Gu rate etc., wherein temperature are conclusive influence factor, within the specific limits, temperature rise, reaction rate is accelerated.Reaction pressure
Indirect influence factor, but the additive factor under the conditions of high-temperature closed, are mainly made up of, it is ensured that sludge exists saturated vapour pressure
Reacted in liquid phase.Reaction time belongs to minor effect factor, related to temperature.Temperature then needs longer reaction when reducing
Time.In general, when pyrohydrolysis reaction temperature is 170 DEG C or so, the reaction time is shorter, between 30~60 minutes.So
And under the high temperature conditions, because mailland reaction is also easy to produce the material of some difficult degradations.Sludge is pre-processed through pyrohydrolysis simultaneously
Afterwards, the experiment of biological methane gesture is carried out to it to find, when pyrohydrolysis temperature is increased to 190 DEG C, the anaerobic digestion performance of sludge declines.
Illustrate under the high temperature conditions, there may also be while sludge hydrolytic and be difficult to biodegradable material generation, while find with heat
The rise of hydrolysis temperature, sludge SCOD final removal efficiency reduce.
Two kinds of sludge hot hydrolysis process of Veolia research and development, it is the Biothelys techniques and continous way of batch-type respectively
ExelysTM techniques.Biothelys techniques are sludge hot hydrolysis process and mesophilic anaerobic digestion technique under special reaction condition
Combination.Service condition is：150 DEG C~170 DEG C of high temperature, high pressure (<Under conditions of 12.5bar), 20~60min is reacted.Hot water
Sludge after solution enters digester, carries out mesophilic anaerobic digestion.Biogas caused by the technique disclosure satisfy that the energy of its own system
Demand, can be for civilian use after biogas more than needed is purified or generates electricity, and realizes the self-balancing and energy yield maximization of energy requirement.
ExelysTMTechnique is a kind of sludge hot hydrolysis process continuously run, can handle the sludge that solid content is up to 25%.With height
The dewatered sludge of solid content is continuously pumped into tubular reactor under stress, while high-temperature steam is also injected into reactor to dirt
Mud is heated.Sludge is in plunger stream mode in tubular reactor, under 165 DEG C and 9bar of pressure, is at least reacted
30min.Pyrohydrolysis sludge, which first passes through heat exchanger recovery heat, reduces temperature, adds water dilution, further reduces temperature, drop simultaneously
Low solid content, allows it to be fed directly into anaerobic digestion process.Both techniques existing Britain, France, Italy etc. are multinational
More sewage plants use this technique.CambiTM techniques are at present in the world using the most pyrohydrolysis technique of achievement, the technique system
System is by pulp tank, pyrohydrolysis tank, and the three parts such as release tank composition.Part I is pulp tank, the dirt being pumped into by sludge storage tank
Mud mixes with the steam waste heat of reuse in follow-up two tanks, reaches about 97 degrees Celsius；Part II is pyrohydrolysis retort, the portion
Dividing is handled using batch-type, is typically made up of 6 tanks, is formed the effect continuously run, pressure steam is provided with by steam boiler,
Sludge is heated to 155-170 degrees Celsius, and is kept for 30 minutes, the sludge after aquathermolysis passes through pressure relief blow to release tank；3rd
Part is release tank, and sludge is after release, and temperature is reduced to 102 degrees Celsius, and the particle diameter of mud granule further reduces, after increase
Continuous digestive efficiency.Compared to Biothelys techniques, CambiTMThe retort gas-phase space ratio of technique is smaller, and capacity utilization is more
It is high；When handling the sludge of same size, CambiTMThe production line negligible amounts of technique, steam consumption quantity guarantee value are lower.It is domestic
The more units using Tsing-Hua University as representative are also studied pyrohydrolysis technique, but technical matters is current and immature, anxious
The sludge pyrohydrolysis for possessing independent intellectual property right and anaerobic digestion integrated treatment process system need to be researched and developed.
The content of the invention
It is an object of the invention to provide a kind of sludge pyrohydrolysis and anaerobic digestion integrated treatment process system, the process system
By enter mud sump 1, sludge pipe 2, enter dredge pump 3, sludge concentrator 4, pulp tank 5, pulp tank sludge inlet flange 6, stirring vane 7,
Agitating shaft 8, temperature sensor 9, stirring motor 10, pressure sensor 11, pulp tank steam inlet flange 12, pulp tank steam stream
Measure valve 13, pulp tank sludge outlet flange 14, pyrohydrolysis retort 15, pyrohydrolysis retort steam (vapor) outlet flange 16, pyrohydrolysis
Retort sludge outlet flange 17, pyrohydrolysis retort sludge inlet flange 18, the pyrohydrolysis catalysis for being filled with nickel-base catalyst
Pipe 19, pyrohydrolysis retort steam inlet flange 20, steam pipe 21, pyrohydrolysis retort steam flow valve 22, steam generator
23rd, pyrohydrolysis retort trip bolt 24, pressure release tank steam flow valve 25, pressure release tank steam inlet flange 26, pressure release tank sludge
It is outlet(discharge) flange 27, pressure release tank sludge inlet flange 28, pressure release tank 29, pressure release tank steam (vapor) outlet flange 30, steam storage tank 31, advanced
Oxidation reaction tank sludge inlet flange 32, advanced oxidation retort 33, advanced oxidation retort sludge outlet flange 34, ozonizer
35th, ozone flow valve 36, ozonizer inlet flange 37, the ozone catalytic pipe 38 for being filled with Ti-base catalyst, ozone generator 39,
Advanced oxidation retort trip bolt 40, digester sludge inlet flange 41, digester 42, digester sludge outlet flange 43,
Plate and frame filter press 44, go out mud sump 45, methane gas outlet(discharge) flange 46, methane gas connecting tube 47, methane gas storage tank 48 and go out
Gas port valve 49 forms.
By sludge pipe 2 and enter dredge pump 3 and will enter mud sump 1 and be connected with sludge concentrator 4, in pulp tank sludge inlet flange 6
Sludge concentrator 4 is connected by place by sludge pipe with pulp tank 5；Passed in the top mounting temperature sensor 9 and pressure of pulp tank 5
Sensor 11, stirring motor 10 is installed in the central upper portion position of pulp tank 5, stirring vane 7 is arranged on agitating shaft 8, agitating shaft 8
It is connected with stirring motor 10；By steam pipe and pulp tank steam flow valve 13 by steam at pulp tank steam inlet flange 12
Storage tank 31 is connected with pulp tank 5；
By sludge pipe by pulp at pulp tank sludge outlet flange 14 and pyrohydrolysis retort sludge inlet flange 18
Tank 5 is connected with pyrohydrolysis retort 15；It is anti-by steam pipe 21 and pyrohydrolysis at pyrohydrolysis retort steam inlet flange 20
Answer tank steam flow valve 22 that pyrohydrolysis retort 15 is connected with steam generator 23；In pyrohydrolysis retort steam (vapor) outlet flange
Pyrohydrolysis retort 15 is connected with steam storage tank 31 by steam pipe at 16；It is filled with the pyrohydrolysis catalysing tube of nickel-base catalyst
19 are arranged in pyrohydrolysis retort 15 by pyrohydrolysis retort trip bolt 24, the position of pyrohydrolysis retort trip bolt 24
Put at the bottom centre of pyrohydrolysis retort 15；
By sludge pipe by hot water at pyrohydrolysis retort sludge outlet flange 17 and pressure release tank sludge inlet flange 28
Solution retort 15 is connected with pressure release tank 29；Pass through steam pipe and pressure release tank steam flow valve at pressure release tank steam inlet flange 26
25 are connected pressure release tank 29 with steam generator 23；At pressure release tank steam (vapor) outlet flange 30 by steam pipe by pressure release tank 29 with
Steam storage tank 31 is connected；
It will be let out by sludge pipe at pressure release tank sludge outlet flange 27 and advanced oxidation retort sludge inlet flange 32
Pressure tank 29 is connected with advanced oxidation retort 33；The ozone catalytic pipe 38 for being filled with Ti-base catalyst passes through advanced oxidation retort
Trip bolt 40 is arranged in advanced oxidation retort 33, and the position of advanced oxidation retort trip bolt 40 is anti-in advanced oxidation
At the bottom centre of Ying Guan 33；Titanium-based will be filled with ozonizer inlet flange 37 by ozonizer 35 and ozone flow valve 36 to urge
The ozone catalytic pipe 38 of agent is connected with ozone generator 39；
By sludge pipe by height at advanced oxidation retort sludge outlet flange 34 and digester sludge inlet flange 41
Level oxidation reaction tank 33 is connected with digester 42；It will be disappeared by sludge pipe at the digester sludge outlet flange 43 of digester 42
Change tank 42 with plate and frame filter press 44 to be connected；Plate and frame filter press 44 is connected by sludge pipe with mud sump 45 is gone out；
By methane gas connecting tube 47 by digester 42 and methane gas storage tank 48 at methane gas outlet(discharge) flange 46
It is connected；The top of methane gas storage tank 48 is provided with gas outlet valve 49；
In the central upper portion position of pyrohydrolysis retort 15, pressure release tank 29, advanced oxidation retort 33 and digester 42 point
Stirring motor is not installed, then connects upper agitating shaft and stirring vane；In pyrohydrolysis retort 15, pressure release tank 29 and digester 42
Top difference mounting temperature sensor and pressure sensor；Pacify respectively on the top of steam storage tank 31 and methane gas storage tank 48
Fill pressure sensor；
Wherein, the nickel-base catalyst is prepared by the following method：
(1) by 89.3 gram particle footpaths be 3-5mm foam nickel particle it is molten in the ethanol that 500mL mass percent concentrations are 40%
Soaked 0.5 hour in liquid, be filtered to remove liquid and obtain substance A 1, substance A 1 is dry at 105 DEG C after the washing of 500mL deionized waters
Placed 1.5 hours in dry case, obtain substance A；
(2) by 3.93 grams of PbCl2, 1.89 grams of CuCl2With 3.68 grams of ZnCl2It is added in 1500mL deionized waters,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed
Close liquid H4, mixed liquor H5；
(3) 1.29 grams of ammonium formates and 3.29 grams of potassium borohydrides are added in mixed liquor H1, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 1, and substance B 1 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance B 2；
(5) 1.24 grams of ammonium formates and 3.25 grams of potassium borohydrides are added in mixed liquor H2, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance B 4；
(7) 1.19 grams of ammonium formates and 3.21 grams of potassium borohydrides are added in mixed liquor H3, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance B 6；
(9) 1.14 grams of ammonium formates and 3.17 grams of potassium borohydrides are added in mixed liquor H4, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, shakes 25 minutes, be filtered to remove in the shaking table that temperature is 35 DEG C
Liquid obtains substance B 7, and substance B 7 is after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Place 40 minutes, obtain substance B 8；
(11) 1.09 grams of ammonium formates and 3.13 grams of potassium borohydrides are added in mixed liquor H5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, shakes 25 minutes, be filtered to remove in the shaking table that temperature is 35 DEG C
Liquid obtains substance B 9, and substance B 9 is after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Place 40 minutes, obtain substance C；
(13) by the chloro- 5- trifluoromethyls pyrazines of 12.7 grams of 2- and 22.6 grams of tributyl 2-acetylcitrates be added to 1500mL without
In water-ethanol, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor K1, mixed liquor
K2, mixed liquor K3, mixed liquor K4, mixed liquor K5；
(14) 8.7 grams of methyl o-benzoylbenzoates and 4.6 grams of 4,4'- dioctyl diphenylamines are added to mixed liquor K1
In, shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L1；
(15) 4.6 grams of diisooctyl phthalates are added in mixed liquor L1, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor M1；
(16) substance C is added in mixed liquor M1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 2；
(17) 8.3 grams of methyl o-benzoylbenzoates and 4.2 grams of 4,4'- dioctyl diphenylamines are added to mixed liquor K2
In, shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L2；
(18) 4.1 grams of diisooctyl phthalates are added in mixed liquor L2, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor M2；
(19) substance C 2 is added in mixed liquor M2, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 3, and substance C 3 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 4；
(20) 7.9 grams of methyl o-benzoylbenzoates and 3.8 grams of 4,4'- dioctyl diphenylamines are added to mixed liquor K3
In, shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L3；
(21) 3.6 grams of diisooctyl phthalates are added in mixed liquor L3, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor M3；
(22) substance C 4 is added in mixed liquor M3, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 5, and substance C 5 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 6；
(23) 7.5 grams of methyl o-benzoylbenzoates and 3.4 grams of 4,4'- dioctyl diphenylamines are added to mixed liquor K4
In, shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L4；
(24) 3.1 grams of diisooctyl phthalates are added in mixed liquor L4, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor M4；
(25) substance C 6 is added in mixed liquor M4, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 7, and substance C 7 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 8；
(26) 7.1 grams of methyl o-benzoylbenzoates and 3.0 grams of 4,4'- dioctyl diphenylamines are added to mixed liquor K5
In, shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L5；
(27) 2.6 grams of diisooctyl phthalates are added in mixed liquor L5, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor M5；
(28) substance C 8 is added in mixed liquor M5, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 9, and substance C 9 is placed 125 minutes in 75 DEG C of drying box, obtains material D；
(29) 4.2 grams of 5- methyl pyridazine -3- amine and the fluoro- 4- nitropyridines of 3.6 grams of 3- are added to 1200mL absolute ethyl alcohols
In, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 3 parts of equivalent is divided into after shaking up, obtained mixed liquor N1, mixed liquor N2, mix
Close liquid N3；
(30) by 2.2 gram 2,3,5- tri- bromothiophenes are added in mixed liquor N1, and 35 are shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor P1；
(31) material D is added in mixed liquor P1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D1, and material D1 is placed 125 minutes in 75 DEG C of drying box, obtains material D2；
(32) 3.7 grams of 3,3'- dihydroxybiphenyl amine are added in mixed liquor N2, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor P2；
(33) material D2 is added in mixed liquor P2, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material D3, and material D3 is placed 125 minutes in 75 DEG C of drying box, obtains material D4；
(34) 4.8 grams of 3- methylbenzene thiophene-2-carboxylic acid methyl esters are added in mixed liquor N3, in the shaking table that temperature is 30 DEG C
It is middle to shake 35 minutes, obtain mixed liquor P3；
(35) material D4 is added in mixed liquor P3, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material D5, material D5 is placed 125 minutes in 75 DEG C of drying box, obtained material is nickel-base catalyst；
The Ti-base catalyst is prepared by the following method：
(1) by 79.6 gram particle footpaths be 3-5mm titanium foam particle it is molten in the ethanol that 500mL mass percent concentrations are 40%
Soaked 0.5 hour in liquid, be filtered to remove liquid and obtain substance A 1, substance A 1 is dry at 105 DEG C after the washing of 500mL deionized waters
Placed 1.5 hours in dry case, obtain substance A；
(2) by 3.6 grams of 3- hydroxyl -2- pyrazine carboxylic acids and 4.4 grams of 5- HYDROXYPYRAZINE -2- carboxylate methyl esters be added to 1500mL without
In water-ethanol, shaken 40 minutes in the shaking table that temperature is 35 DEG C, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor H1, mixed liquor
H2, mixed liquor H3, mixed liquor H4, mixed liquor H5；
(3) the bromo- 3- chloropyrazines -2- amine of 1.6 grams of 5- is added in mixed liquor H1, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 1, and substance B 1 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 2；
(5) chloro- 6, the 7- dimethoxy-quinolines of 2.8 grams of 4- are added in mixed liquor H2, in the shaking table that temperature is 30 DEG C
Shake 35 minutes, obtain mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 4；
(7) 1.1 grams of 3- methyl -4-aminopyridines are added in mixed liquor H3, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 6；
(9) 3.2 grams of chloro- thenoic acids of 2- are added in mixed liquor H4,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, shakes 40 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance B 7, and substance B 7 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 8；
(11) bromo- 3, the 6- Pyridazindiones of 1.9 grams of 4- are added in mixed liquor H5, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, shakes 40 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance B 9, and substance B 9 is placed 125 minutes in 75 DEG C of drying box, obtains substance C；
(13) by 2.38 grams of CdCl2, 2.22 grams of MgCl2With 4.41 grams of PbCl2It is added in 1200mL deionized waters,
Stirred 5 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mixed liquor K3；
(14) 2.6 grams of sodium vanadates and 3.1 grams of sodium aluminates are added in mixed liquor K1,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor L1；
(15) substance C is added in mixed liquor L1, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance C 2；
(16) 2.3 grams of sodium vanadates and 2.8 grams of sodium aluminates are added in mixed liquor K2,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor L2；
(17) substance C 2 is added in mixed liquor L2, shakes 25 minutes, be filtered to remove in the shaking table that temperature is 35 DEG C
Liquid obtains substance C 3, and substance C 3 is after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Place 40 minutes, obtain substance C 4；
(18) 2.0 grams of sodium vanadates and 2.5 grams of sodium aluminates are added in mixed liquor K3,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor L3；
(19) substance C 4 is added in mixed liquor L3, shakes 25 minutes, be filtered to remove in the shaking table that temperature is 35 DEG C
Liquid obtains substance C 5, and substance C 5 is after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Place 40 minutes, obtain material D；
(20) the fluoro- 3- nitros -5- chloropyridines of 11.3 grams of 2- and 14.5 grams of N- (the chloro- 3- pyridazinyls of 6-) butyramides are added to
In 1200mL absolute ethyl alcohols, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor
M1, mixed liquor M2, mixed liquor M3, mixed liquor M4；
(21) 4.2 grams of 2- butyl -3- methylpyrazines and 2.6 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M1,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N1；
(22) the chloro- 7- Trifluoromethylquinocarboxylics of 3.3 grams of 4- are added in mixed liquor N1, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O1；
(23) material D is added in mixed liquor O1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D1, and material D1 is placed 145 minutes in 75 DEG C of drying box, obtains material D2；
(24) 3.9 grams of 2- butyl -3- methylpyrazines and 2.3 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M2,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N2；
(25) the chloro- 7- Trifluoromethylquinocarboxylics of 3.0 grams of 4- are added in mixed liquor N2, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O2；
(26) material D2 is added in mixed liquor O2, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material D3, and material D3 is placed 145 minutes in 75 DEG C of drying box, obtains material D4；
(27) 3.6 grams of 2- butyl -3- methylpyrazines and 2.0 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M3,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N3；
(28) the chloro- 7- Trifluoromethylquinocarboxylics of 2.7 grams of 4- are added in mixed liquor N3, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O3；
(29) material D4 is added in mixed liquor O3, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material D5, and material D5 is placed 145 minutes in 75 DEG C of drying box, obtains material D6；
(30) 3.3 grams of 2- butyl -3- methylpyrazines and 1.7 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M4,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N4；
(31) the chloro- 7- Trifluoromethylquinocarboxylics of 2.4 grams of 4- are added in mixed liquor N4, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O4；
(32) material D6 is added in mixed liquor O4, shakes 45 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material D7, material D7 is placed 145 minutes in 75 DEG C of drying box, obtained material is Ti-base catalyst.
The invention has the advantages that the sludge pyrohydrolysis and anaerobic digestion integrated treatment process system are applied to sludge
Processing have energy consumption it is low, kill germ ability it is strong, dewatering performance of sludge is good, dewatered sludge yield is few, methane in sewage gas gas
The advantages such as content is high, hydrogen sulfide content is low.
Brief description of the drawings
Accompanying drawing 1 is sludge pyrohydrolysis and the schematic diagram of anaerobic digestion integrated treatment process system.In accompanying drawing 11 be into mud sump,
2 be sludge pipe, 3 be into dredge pump, 4 be sludge concentrator, 5 be pulp tank, 6 be pulp tank sludge inlet flange, 7 be paddle
Piece, 8 be agitating shaft, 9 be temperature sensor, 10 be stirring motor, 11 be pressure sensor, 12 be pulp tank steam inlet method
It is blue, 13 be pulp tank steam flow valve, 14 be pulp tank sludge outlet flange, 15 be pyrohydrolysis retort, 16 be that pyrohydrolysis is anti-
Answer tank steam (vapor) outlet flange, 17 be pyrohydrolysis retort sludge outlet flange, 18 be pyrohydrolysis retort sludge inlet flange, 19
For be filled with the pyrohydrolysis catalysing tube of nickel-base catalyst, 20 be pyrohydrolysis retort steam inlet flange, 21 be steam pipe, 22 be
Pyrohydrolysis retort steam flow valve, 23 be steam generator, 24 be pyrohydrolysis retort trip bolt, 25 be pressure release tank steam
Flow valve, 26 be pressure release tank steam inlet flange, 27 be pressure release tank sludge outlet flange, 28 be pressure release tank sludge inlet flange,
29 it is pressure release tank, 30 be pressure release tank steam (vapor) outlet flange, 31 be steam storage tank, 32 is advanced oxidation retort sludge inlet method
It is blue, 33 be advanced oxidation retort, 34 be advanced oxidation retort sludge outlet flange, 35 be ozonizer, 36 be ozone flow
Valve, 37 be ozonizer inlet flange, 38 for be filled with the ozone catalytic pipe of Ti-base catalyst, 39 be ozone generator, 40 be high
Level oxidation reaction tank trip bolt, 41 be digester sludge inlet flange, 42 be digester, 43 be digester sludge outlet method
It is blue, 44 be plate and frame filter press, 45 be mud sump, 46 be methane gas outlet(discharge) flange, 47 be methane gas connecting tube, 48 be methane
Gas reservoir, 49 are gas outlet valve.
Embodiment
Embodiment
(1) preparation process of sludge pyrohydrolysis and anaerobic digestion integrated treatment process system is as follows：
Sludge pyrohydrolysis and anaerobic digestion integrated treatment process system are by entering mud sump 1, sludge pipe 2, to enter dredge pump 3, sludge dense
Contracting machine 4, pulp tank 5, pulp tank sludge inlet flange 6, stirring vane 7, agitating shaft 8, temperature sensor 9, stirring motor 10, pressure
Force snesor 11, pulp tank steam inlet flange 12, pulp tank steam flow valve 13, pulp tank sludge outlet flange 14, hot water
Solve retort 15, pyrohydrolysis retort steam (vapor) outlet flange 16, pyrohydrolysis retort sludge outlet flange 17, pyrohydrolysis retort
Sludge inlet flange 18, the pyrohydrolysis catalysing tube 19 for being filled with nickel-base catalyst, pyrohydrolysis retort steam inlet flange 20, steaming
Steam pipe 21, pyrohydrolysis retort steam flow valve 22, steam generator 23, pyrohydrolysis retort trip bolt 24, pressure release tank steam
Vapour flow valve 25, pressure release tank steam inlet flange 26, pressure release tank sludge outlet flange 27, pressure release tank sludge inlet flange 28, let out
Press tank 29, pressure release tank steam (vapor) outlet flange 30, steam storage tank 31, advanced oxidation retort sludge inlet flange 32, advanced oxidation
Retort 33, advanced oxidation retort sludge outlet flange 34, ozonizer 35, ozone flow valve 36, ozonizer inlet flange 37,
Ozone catalytic pipe 38, ozone generator 39, advanced oxidation retort trip bolt 40, the digester for being filled with Ti-base catalyst are dirty
Mud inlet flange 41, digester 42, digester sludge outlet flange 43, plate and frame filter press 44, go out mud sump 45, methane gas outlet
Flange 46, methane gas connecting tube 47, methane gas storage tank 48, gas outlet valve 49 form.
The volume for entering mud sump is 4.5m3, sludge pipe is the pvc pipe that internal diameter is 10cm, and steam pipe is that internal diameter is the stainless of 8cm
Steel pipe, methane gas connecting tube be internal diameter be 9cm stainless steel tube, pulp tank, pyrohydrolysis retort, pressure release tank, advanced oxidation
The volume of retort and digester is 1.5m3, the volume of steam storage tank is 7.5m3, the volume of methane gas storage tank is 5.5m3,
The volume for going out mud sump is 8.5m3.Pyrohydrolysis catalysing tube is the stainless steel tube that internal diameter is 10cm, and being covered with pore size on tube wall is
2mm aperture.Ozone catalytic pipe is the stainless steel tube that internal diameter is 10cm, and the aperture that pore size is 2mm is covered with tube wall.
By sludge pipe 2 and enter dredge pump 3 and will enter mud sump 1 and be connected with sludge concentrator 4, in pulp tank sludge inlet flange 6
Sludge concentrator 4 is connected by place by sludge pipe with pulp tank 5；Passed in the top mounting temperature sensor 9 and pressure of pulp tank 5
Sensor 11, stirring motor 10 is installed in the central upper portion position of pulp tank 5, stirring vane 7 is arranged on agitating shaft 8, agitating shaft 8
It is connected with stirring motor 10；By steam pipe and pulp tank steam flow valve 13 by steam at pulp tank steam inlet flange 12
Storage tank 31 is connected with pulp tank 5.
By sludge pipe by pulp at pulp tank sludge outlet flange 14 and pyrohydrolysis retort sludge inlet flange 18
Tank 5 is connected with pyrohydrolysis retort 15；It is anti-by steam pipe 21 and pyrohydrolysis at pyrohydrolysis retort steam inlet flange 20
Answer tank steam flow valve 22 that pyrohydrolysis retort 15 is connected with steam generator 23；In pyrohydrolysis retort steam (vapor) outlet flange
Pyrohydrolysis retort 15 is connected with steam storage tank 31 by steam pipe at 16；It is filled with the pyrohydrolysis catalysing tube of nickel-base catalyst
19 are arranged in pyrohydrolysis retort 15 by pyrohydrolysis retort trip bolt 24, the position of pyrohydrolysis retort trip bolt 24
Put at the bottom centre of pyrohydrolysis retort 15.
By sludge pipe by hot water at pyrohydrolysis retort sludge outlet flange 17 and pressure release tank sludge inlet flange 28
Solution retort 15 is connected with pressure release tank 29；Pass through steam pipe and pressure release tank steam flow valve at pressure release tank steam inlet flange 26
25 are connected pressure release tank 29 with steam generator 23；At pressure release tank steam (vapor) outlet flange 30 by steam pipe by pressure release tank 29 with
Steam storage tank 31 is connected.
It will be let out by sludge pipe at pressure release tank sludge outlet flange 27 and advanced oxidation retort sludge inlet flange 32
Pressure tank 29 is connected with advanced oxidation retort 33；The ozone catalytic pipe 38 for being filled with Ti-base catalyst passes through advanced oxidation retort
Trip bolt 40 is arranged in advanced oxidation retort 33, and the position of advanced oxidation retort trip bolt 40 is anti-in advanced oxidation
At the bottom centre of Ying Guan 33；Titanium-based will be filled with ozonizer inlet flange 37 by ozonizer 35 and ozone flow valve 36 to urge
The ozone catalytic pipe 38 of agent is connected with ozone generator 39.
By sludge pipe by height at advanced oxidation retort sludge outlet flange 34 and digester sludge inlet flange 41
Level oxidation reaction tank 33 is connected with digester 42；It will be disappeared by sludge pipe at the digester sludge outlet flange 43 of digester 42
Change tank 42 with plate and frame filter press 44 to be connected；Plate and frame filter press 44 is connected by sludge pipe with mud sump 45 is gone out.
By methane gas connecting tube 47 by digester 42 and methane gas storage tank 48 at methane gas outlet(discharge) flange 46
It is connected；The top of methane gas storage tank 48 is provided with gas outlet valve 49.
In the central upper portion position of pyrohydrolysis retort 15, pressure release tank 29, advanced oxidation retort 33 and digester 42 point
Stirring motor is not installed, then connects upper agitating shaft and stirring vane；In pyrohydrolysis retort 15, pressure release tank 29 and digester 42
Top difference mounting temperature sensor and pressure sensor；Pacify respectively on the top of steam storage tank 31 and methane gas storage tank 48
Fill pressure sensor.
(2) nickel-base catalyst is prepared by the following method：
1) by 89.3 gram particle footpaths be 3-5mm foam nickel particle it is molten in the ethanol that 500mL mass percent concentrations are 40%
Soaked 0.5 hour in liquid, be filtered to remove liquid and obtain substance A 1, substance A 1 is dry at 105 DEG C after the washing of 500mL deionized waters
Placed 1.5 hours in dry case, obtain substance A；
2) by 3.93 grams of PbCl2, 1.89 grams of CuCl2With 3.68 grams of ZnCl2It is added in 1500mL deionized waters,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed
Close liquid H4, mixed liquor H5；
3) 1.29 grams of ammonium formates and 3.29 grams of potassium borohydrides are added in mixed liquor H1, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J1；
4) substance A is added in mixed liquor J1, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Substance B 1 is obtained, substance B 1 is placed after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
40 minutes, obtain substance B 2；
5) 1.24 grams of ammonium formates and 3.25 grams of potassium borohydrides are added in mixed liquor H2, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J2；
6) substance B 2 is added in mixed liquor J2, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance B 4；
7) 1.19 grams of ammonium formates and 3.21 grams of potassium borohydrides are added in mixed liquor H3, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J3；
8) substance B 4 is added in mixed liquor J3, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance B 6；
9) 1.14 grams of ammonium formates and 3.17 grams of potassium borohydrides are added in mixed liquor H4, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J4；
10) substance B 6 is added in mixed liquor J4, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 7, and substance B 7 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance B 8；
11) 1.09 grams of ammonium formates and 3.13 grams of potassium borohydrides are added in mixed liquor H5, stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor J5；
12) substance B 8 is added in mixed liquor J5, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance B 9, and substance B 9 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance C；
13) by the chloro- 5- trifluoromethyls pyrazines of 12.7 grams of 2- and 22.6 grams of tributyl 2-acetylcitrates be added to 1500mL without
In water-ethanol, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor K1, mixed liquor
K2, mixed liquor K3, mixed liquor K4, mixed liquor K5；
14) 8.7 grams of methyl o-benzoylbenzoates and 4.6 gram 4,4'- dioctyl diphenylamines are added in mixed liquor K1,
Shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L1；
15) 4.6 grams of diisooctyl phthalates are added in mixed liquor L1, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor M1；
16) substance C is added in mixed liquor M1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 2；
17) 8.3 grams of methyl o-benzoylbenzoates and 4.2 gram 4,4'- dioctyl diphenylamines are added in mixed liquor K2,
Shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L2；
18) 4.1 grams of diisooctyl phthalates are added in mixed liquor L2, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor M2；
19) substance C 2 is added in mixed liquor M2, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 3, and substance C 3 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 4；
20) 7.9 grams of methyl o-benzoylbenzoates and 3.8 gram 4,4'- dioctyl diphenylamines are added in mixed liquor K3,
Shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L3；
21) 3.6 grams of diisooctyl phthalates are added in mixed liquor L3, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor M3；
22) substance C 4 is added in mixed liquor M3, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 5, and substance C 5 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 6；
23) 7.5 grams of methyl o-benzoylbenzoates and 3.4 gram 4,4'- dioctyl diphenylamines are added in mixed liquor K4,
Shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L4；
24) 3.1 grams of diisooctyl phthalates are added in mixed liquor L4, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor M4；
25) substance C 6 is added in mixed liquor M4, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 7, and substance C 7 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 8；
26) 7.1 grams of methyl o-benzoylbenzoates and 3.0 gram 4,4'- dioctyl diphenylamines are added in mixed liquor K5,
Shaken 35 minutes in the shaking table that temperature is 30 DEG C, obtain mixed liquor L5；
27) 2.6 grams of diisooctyl phthalates are added in mixed liquor L5, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor M5；
28) substance C 8 is added in mixed liquor M5, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 9, and substance C 9 is placed 125 minutes in 75 DEG C of drying box, obtains material D；
29) 4.2 grams of 5- methyl pyridazine -3- amine and the fluoro- 4- nitropyridines of 3.6 grams of 3- are added to 1200mL absolute ethyl alcohols
In, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 3 parts of equivalent is divided into after shaking up, obtained mixed liquor N1, mixed liquor N2, mix
Close liquid N3；
30) by 2.2 gram 2,3,5- tri- bromothiophenes are added in mixed liquor N1, and 35 points are shaken in the shaking table that temperature is 30 DEG C
Clock, obtain mixed liquor P1；
31) material D is added in mixed liquor P1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D1, and material D1 is placed 125 minutes in 75 DEG C of drying box, obtains material D2；
32) by 3.7 gram 3,3'- dihydroxybiphenyl amine is added in mixed liquor N2, is shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor P2；
33) material D2 is added in mixed liquor P2, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D3, and material D3 is placed 125 minutes in 75 DEG C of drying box, obtains material D4；
34) 4.8 grams of 3- methylbenzene thiophene-2-carboxylic acid methyl esters are added in mixed liquor N3, in the shaking table that temperature is 30 DEG C
It is middle to shake 35 minutes, obtain mixed liquor P3；
35) material D4 is added in mixed liquor P3, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D5, material D5 is placed 125 minutes in 75 DEG C of drying box, obtained material is nickel-base catalyst；
(3) Ti-base catalyst is prepared by the following method：
1) by 79.6 gram particle footpaths be 3-5mm titanium foam particle it is molten in the ethanol that 500mL mass percent concentrations are 40%
Soaked 0.5 hour in liquid, be filtered to remove liquid and obtain substance A 1, substance A 1 is dry at 105 DEG C after the washing of 500mL deionized waters
Placed 1.5 hours in dry case, obtain substance A；
2) by 3.6 grams of 3- hydroxyl -2- pyrazine carboxylic acids and 4.4 grams of 5- HYDROXYPYRAZINE -2- carboxylate methyl esters be added to 1500mL without
In water-ethanol, shaken 40 minutes in the shaking table that temperature is 35 DEG C, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor H1, mixed liquor
H2, mixed liquor H3, mixed liquor H4, mixed liquor H5；
3) the bromo- 3- chloropyrazines -2- amine of 1.6 grams of 5- is added in mixed liquor H1, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor J1；
4) substance A is added in mixed liquor J1, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance B 1 is obtained, substance B 1 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 2；
5) 2.8 grams of 4- chloro- 6,7- dimethoxy-quinolines are added in mixed liquor H2, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor J2；
6) substance B 2 is added in mixed liquor J2, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 4；
7) 1.1 grams of 3- methyl -4-aminopyridines are added in mixed liquor H3,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor J3；
8) substance B 4 is added in mixed liquor J3, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 6；
9) 3.2 grams of chloro- thenoic acids of 2- are added in mixed liquor H4,35 points is shaken in the shaking table that temperature is 30 DEG C
Clock, obtain mixed liquor J4；
10) substance B 6 is added in mixed liquor J4, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 7, and substance B 7 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 8；
11) 1.9 grams of 4- bromo- 3,6- Pyridazindiones are added in mixed liquor H5, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor J5；
12) substance B 8 is added in mixed liquor J5, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance B 9, and substance B 9 is placed 125 minutes in 75 DEG C of drying box, obtains substance C；
13) by 2.38 grams of CdCl2, 2.22 grams of MgCl2With 4.41 grams of PbCl2It is added in 1200mL deionized waters,
Stirred 5 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mixed liquor K3；
14) 2.6 grams of sodium vanadates and 3.1 grams of sodium aluminates are added in mixed liquor K1,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor L1；
15) substance C is added in mixed liquor L1, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance C 2；
16) 2.3 grams of sodium vanadates and 2.8 grams of sodium aluminates are added in mixed liquor K2,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor L2；
17) substance C 2 is added in mixed liquor L2, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance C 3, and substance C 3 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain substance C 4；
18) 2.0 grams of sodium vanadates and 2.5 grams of sodium aluminates are added in mixed liquor K3,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor L3；
19) substance C 4 is added in mixed liquor L3, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Body obtains substance C 5, and substance C 5 is put after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Put 40 minutes, obtain material D；
20) the fluoro- 3- nitros -5- chloropyridines of 11.3 grams of 2- and 14.5 grams of N- (the chloro- 3- pyridazinyls of 6-) butyramides are added to
In 1200mL absolute ethyl alcohols, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor
M1, mixed liquor M2, mixed liquor M3, mixed liquor M4；
21) 4.2 grams of 2- butyl -3- methylpyrazines and 2.6 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M1,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N1；
22) the chloro- 7- Trifluoromethylquinocarboxylics of 3.3 grams of 4- are added in mixed liquor N1, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O1；
23) material D is added in mixed liquor O1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D1, and material D1 is placed 145 minutes in 75 DEG C of drying box, obtains material D2；
24) 3.9 grams of 2- butyl -3- methylpyrazines and 2.3 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M2,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N2；
25) the chloro- 7- Trifluoromethylquinocarboxylics of 3.0 grams of 4- are added in mixed liquor N2, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O2；
26) material D2 is added in mixed liquor O2, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D3, and material D3 is placed 145 minutes in 75 DEG C of drying box, obtains material D4；
27) 3.6 grams of 2- butyl -3- methylpyrazines and 2.0 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M3,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N3；
28) the chloro- 7- Trifluoromethylquinocarboxylics of 2.7 grams of 4- are added in mixed liquor N3, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O3；
29) material D4 is added in mixed liquor O3, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D5, and material D5 is placed 145 minutes in 75 DEG C of drying box, obtains material D6；
30) 3.3 grams of 2- butyl -3- methylpyrazines and 1.7 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M4,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor N4；
31) the chloro- 7- Trifluoromethylquinocarboxylics of 2.4 grams of 4- are added in mixed liquor N4, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor O4；
32) material D6 is added in mixed liquor O4, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material D7, material D7 is placed 145 minutes in 75 DEG C of drying box, obtained material is Ti-base catalyst.
(4) sludge pyrohydrolysis and anaerobic digestion integrated treatment process systematic difference
The sludge pyrohydrolysis and anaerobic digestion integrated treatment process system obtained with the present invention has carried out sludge pyrohydrolysis
Tested with Anaerobic Digestion, the results showed that sludge postdigestive sludge cause of disease bacterial content after processing is zero, and containing for sludge is solid
Rate is 37%, and the conversion ratio that organic matter is converted into biogas is 66.8%, and methane in sewage gas gas content is 71.2%.
Claims (1)
1. a kind of sludge pyrohydrolysis and anaerobic digestion integrated treatment process system, it is characterised in that the process system is by entering mud sump
1st, sludge pipe 2, enter dredge pump 3, sludge concentrator 4, pulp tank 5, pulp tank sludge inlet flange 6, stirring vane 7, agitating shaft 8,
Temperature sensor 9, stirring motor 10, pressure sensor 11, pulp tank steam inlet flange 12, pulp tank steam flow valve 13,
Pulp tank sludge outlet flange 14, pyrohydrolysis retort 15, pyrohydrolysis retort steam (vapor) outlet flange 16, pyrohydrolysis retort are dirty
Mud outlet(discharge) flange 17, pyrohydrolysis retort sludge inlet flange 18, pyrohydrolysis catalysing tube 19, the hot water for being filled with nickel-base catalyst
Solve retort steam inlet flange 20, steam pipe 21, pyrohydrolysis retort steam flow valve 22, steam generator 23, pyrohydrolysis
Retort trip bolt 24, pressure release tank steam flow valve 25, pressure release tank steam inlet flange 26, pressure release tank sludge outlet flange
27th, pressure release tank sludge inlet flange 28, pressure release tank 29, pressure release tank steam (vapor) outlet flange 30, steam storage tank 31, advanced oxidation reaction
Tank sludge inlet flange 32, advanced oxidation retort 33, advanced oxidation retort sludge outlet flange 34, ozonizer 35, ozone
Flow valve 36, ozonizer inlet flange 37, the ozone catalytic pipe 38 for being filled with Ti-base catalyst, ozone generator 39, advanced oxygen
Change retort trip bolt 40, digester sludge inlet flange 41, digester 42, digester sludge outlet flange 43, sheet frame pressure
Filter 44, go out mud sump 45, methane gas outlet(discharge) flange 46, methane gas connecting tube 47, methane gas storage tank 48 and gas outlet valve
Door 49 forms；By sludge pipe 2 and enter dredge pump 3 and will enter mud sump 1 and be connected with sludge concentrator 4, in pulp tank sludge inlet flange 6
Sludge concentrator 4 is connected by place by sludge pipe with pulp tank 5；Passed in the top mounting temperature sensor 9 and pressure of pulp tank 5
Sensor 11, stirring motor 10 is installed in the central upper portion position of pulp tank 5, stirring vane 7 is arranged on agitating shaft 8, agitating shaft 8
It is connected with stirring motor 10；By steam pipe and pulp tank steam flow valve 13 by steam at pulp tank steam inlet flange 12
Storage tank 31 is connected with pulp tank 5；Pass through at pulp tank sludge outlet flange 14 and pyrohydrolysis retort sludge inlet flange 18
Pulp tank 5 is connected by sludge pipe with pyrohydrolysis retort 15；Pass through steam pipe at pyrohydrolysis retort steam inlet flange 20
21 and pyrohydrolysis retort steam flow valve 22 pyrohydrolysis retort 15 is connected with steam generator 23；In pyrohydrolysis retort
Pyrohydrolysis retort 15 is connected with steam storage tank 31 by steam pipe at steam (vapor) outlet flange 16；It is filled with nickel-base catalyst
Pyrohydrolysis catalysing tube 19 is arranged in pyrohydrolysis retort 15 by pyrohydrolysis retort trip bolt 24, and pyrohydrolysis retort is tight
Gu the position of screw 24 is at the bottom centre of pyrohydrolysis retort 15；In pyrohydrolysis retort sludge outlet flange 17 and pressure release tank
Pyrohydrolysis retort 15 is connected with pressure release tank 29 by sludge pipe at sludge inlet flange 28；In pressure release tank steam inlet flange
Pressure release tank 29 is connected with steam generator 23 by steam pipe and pressure release tank steam flow valve 25 at 26；Go out in pressure release tank steam
Pressure release tank 29 is connected with steam storage tank 31 by steam pipe at mouth flange 30；In pressure release tank sludge outlet flange 27 and advanced oxygen
Change and pressure release tank 29 is connected with advanced oxidation retort 33 by sludge pipe at retort sludge inlet flange 32；It is filled with titanium-based
The ozone catalytic pipe 38 of catalyst is arranged in advanced oxidation retort 33 by advanced oxidation retort trip bolt 40, advanced
The position of oxidation reaction tank trip bolt 40 is at the bottom centre of advanced oxidation retort 33；Lead at ozonizer inlet flange 37
Cross ozonizer 35 and ozone flow valve 36 the ozone catalytic pipe 38 for being filled with Ti-base catalyst is connected with ozone generator 39；
Advanced oxidation is reacted by sludge pipe at advanced oxidation retort sludge outlet flange 34 and digester sludge inlet flange 41
Tank 33 is connected with digester 42；By sludge pipe by digester 42 and plate at the digester sludge outlet flange 43 of digester 42
Frame filter press 44 is connected；Plate and frame filter press 44 is connected by sludge pipe with mud sump 45 is gone out；Lead at methane gas outlet(discharge) flange 46
Cross methane gas connecting tube 47 digester 42 is connected with methane gas storage tank 48；It is provided with the top of methane gas storage tank 48
Gas outlet valve 49；In the central upper portion position of pyrohydrolysis retort 15, pressure release tank 29, advanced oxidation retort 33 and digester 42
Put and stirring motor is installed respectively, then connect upper agitating shaft and stirring vane；In pyrohydrolysis retort 15, pressure release tank 29 and digestion
The top difference mounting temperature sensor and pressure sensor of tank 42；In the upper part of steam storage tank 31 and methane gas storage tank 48
Pressure sensor is not installed；Wherein, nickel-base catalyst is prepared by the following method：
(1) by 89.3 gram particle footpaths be 3-5mm foam nickel particle in the ethanol solution that 500mL mass percent concentrations are 40%
Immersion 0.5 hour, it is filtered to remove liquid and obtains substance A 1, substance A 1 is after the washing of 500mL deionized waters in 105 DEG C of drying box
It is middle to place 1.5 hours, obtain substance A；
(2) by 3.93 grams of PbCl2, 1.89 grams of CuCl2With 3.68 grams of ZnCl2It is added in 1500mL deionized waters, in 1000r/
Stirred 5 minutes under the conditions of min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4,
Mixed liquor H5；
(3) 1.29 grams of ammonium formates and 3.29 grams of potassium borohydrides are added in mixed liquor H1,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid and obtain
To substance B 1, substance B 1 places 40 after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Minute, obtain substance B 2；
(5) 1.24 grams of ammonium formates and 3.25 grams of potassium borohydrides are added in mixed liquor H2,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid and obtain
To substance B 3, substance B 3 places 40 after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Minute, obtain substance B 4；
(7) 1.19 grams of ammonium formates and 3.21 grams of potassium borohydrides are added in mixed liquor H3,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid and obtain
To substance B 5, substance B 5 places 40 after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Minute, obtain substance B 6；
(9) 1.14 grams of ammonium formates and 3.17 grams of potassium borohydrides are added in mixed liquor H4,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Substance B 7 is obtained, substance B 7 is placed after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
40 minutes, obtain substance B 8；
(11) 1.09 grams of ammonium formates and 3.13 grams of potassium borohydrides are added in mixed liquor H5,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Substance B 9 is obtained, substance B 9 is placed after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
40 minutes, obtain substance C；
(13) the chloro- 5- trifluoromethyls pyrazines of 12.7 grams of 2- and 22.6 grams of tributyl 2-acetylcitrates are added to the anhydrous second of 1500mL
In alcohol, shaken 35 minutes in temperature is 35 DEG C of shaking table, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor K1, mixed liquor K2,
Mixed liquor K3, mixed liquor K4, mixed liquor K5；
(14) 8.7 grams of methyl o-benzoylbenzoates and 4.6 grams of 4,4'- dioctyl diphenylamines are added in mixed liquor K1,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor L1；
(15) 4.6 grams of diisooctyl phthalates are added in mixed liquor L1,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor M1；
(16) substance C is added in mixed liquor M1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To substance C 1, substance C 1 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 2；
(17) 8.3 grams of methyl o-benzoylbenzoates and 4.2 grams of 4,4'- dioctyl diphenylamines are added in mixed liquor K2,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor L2；
(18) 4.1 grams of diisooctyl phthalates are added in mixed liquor L2,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor M2；
(19) substance C 2 is added in mixed liquor M2, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance C 3 is obtained, substance C 3 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 4；
(20) 7.9 grams of methyl o-benzoylbenzoates and 3.8 grams of 4,4'- dioctyl diphenylamines are added in mixed liquor K3,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor L3；
(21) 3.6 grams of diisooctyl phthalates are added in mixed liquor L3,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor M3；
(22) substance C 4 is added in mixed liquor M3, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance C 5 is obtained, substance C 5 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 6；
(23) 7.5 grams of methyl o-benzoylbenzoates and 3.4 grams of 4,4'- dioctyl diphenylamines are added in mixed liquor K4,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor L4；
(24) 3.1 grams of diisooctyl phthalates are added in mixed liquor L4,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor M4；
(25) substance C 6 is added in mixed liquor M4, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance C 7 is obtained, substance C 7 is placed 125 minutes in 75 DEG C of drying box, obtains substance C 8；
(26) 7.1 grams of methyl o-benzoylbenzoates and 3.0 grams of 4,4'- dioctyl diphenylamines are added in mixed liquor K5,
Temperature is to be shaken 35 minutes in 30 DEG C of shaking table, obtains mixed liquor L5；
(27) 2.6 grams of diisooctyl phthalates are added in mixed liquor L5,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor M5；
(28) substance C 8 is added in mixed liquor M5, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance C 9 is obtained, substance C 9 is placed 125 minutes in 75 DEG C of drying box, obtains material D；
(29) 4.2 grams of 5- methyl pyridazine -3- amine and the fluoro- 4- nitropyridines of 3.6 grams of 3- are added in 1200mL absolute ethyl alcohols,
Temperature is to be shaken 35 minutes in 35 DEG C of shaking table, and 3 parts of equivalent is divided into after shaking up, obtains mixed liquor N1, mixed liquor N2, mixed liquor
N3；
(30) by 2.2 gram 2,3,5- tri- bromothiophenes are added in mixed liquor N1, are shaken 35 minutes in the shaking table that temperature is 30 DEG C,
Obtain mixed liquor P1；
(31) material D is added in mixed liquor P1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To material D1, material D1 is placed 125 minutes in 75 DEG C of drying box, obtains material D2；
(32) 3.7 grams of 3,3'- dihydroxybiphenyl amine are added in mixed liquor N2,35 points is shaken in the shaking table that temperature is 30 DEG C
Clock, obtain mixed liquor P2；
(33) material D2 is added in mixed liquor P2, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Material D3 is obtained, material D3 is placed 125 minutes in 75 DEG C of drying box, obtains material D4；
(34) 4.8 grams of 3- methylbenzene thiophene-2-carboxylic acid methyl esters are added in mixed liquor N3, shaken in the shaking table that temperature is 30 DEG C
It is dynamic 35 minutes, obtain mixed liquor P3；
(35) material D4 is added in mixed liquor P3, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Material D5 is obtained, material D5 is placed 125 minutes in 75 DEG C of drying box, obtained material is nickel-base catalyst；
Ti-base catalyst is prepared by the following method：
(1) by 79.6 gram particle footpaths be 3-5mm titanium foam particle in the ethanol solution that 500mL mass percent concentrations are 40%
Immersion 0.5 hour, it is filtered to remove liquid and obtains substance A 1, substance A 1 is after the washing of 500mL deionized waters in 105 DEG C of drying box
It is middle to place 1.5 hours, obtain substance A；
(2) 3.6 grams of 3- hydroxyl -2- pyrazine carboxylic acids and 4.4 grams of 5- HYDROXYPYRAZINE -2- carboxylate methyl esters are added to the anhydrous second of 1500mL
In alcohol, shaken 40 minutes in temperature is 35 DEG C of shaking table, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor H1, mixed liquor H2,
Mixed liquor H3, mixed liquor H4, mixed liquor H5；
(3) the bromo- 3- chloropyrazines -2- amine of 1.6 grams of 5- is added in mixed liquor H1,35 points is shaken in the shaking table that temperature is 30 DEG C
Clock, obtain mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To substance B 1, substance B 1 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 2；
(5) chloro- 6, the 7- dimethoxy-quinolines of 2.8 grams of 4- are added in mixed liquor H2, shaken in the shaking table that temperature is 30 DEG C
35 minutes, obtain mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To substance B 3, substance B 3 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 4；
(7) 1.1 grams of 3- methyl -4-aminopyridines are added in mixed liquor H3,35 points is shaken in the shaking table that temperature is 30 DEG C
Clock, obtain mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To substance B 5, substance B 5 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 6；
(9) 3.2 grams of chloro- thenoic acids of 2- are added in mixed liquor H4, shaken 35 minutes in the shaking table that temperature is 30 DEG C,
Obtain mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance B 7 is obtained, substance B 7 is placed 125 minutes in 75 DEG C of drying box, obtains substance B 8；
(11) bromo- 3, the 6- Pyridazindiones of 1.9 grams of 4- are added in mixed liquor H5,35 points is shaken in the shaking table that temperature is 30 DEG C
Clock, obtain mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, is shaken 40 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance B 9 is obtained, substance B 9 is placed 125 minutes in 75 DEG C of drying box, obtains substance C；
(13) by 2.38 grams of CdCl2, 2.22 grams of MgCl2With 4.41 grams of PbCl2It is added in 1200mL deionized waters, in 1000r/
Stirred 5 minutes under the conditions of min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mixed liquor K3；
(14) 2.6 grams of sodium vanadates and 3.1 grams of sodium aluminates are added in mixed liquor K1,3 points is stirred under the conditions of 1000r/min
Clock, obtain mixed liquor L1；
(15) substance C is added in mixed liquor L1, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid and obtain
To substance C 1, substance C 1 places 40 after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
Minute, obtain substance C 2；
(16) 2.3 grams of sodium vanadates and 2.8 grams of sodium aluminates are added in mixed liquor K2,3 points is stirred under the conditions of 1000r/min
Clock, obtain mixed liquor L2；
(17) substance C 2 is added in mixed liquor L2, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Substance C 3 is obtained, substance C 3 is placed after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
40 minutes, obtain substance C 4；
(18) 2.0 grams of sodium vanadates and 2.5 grams of sodium aluminates are added in mixed liquor K3,3 points is stirred under the conditions of 1000r/min
Clock, obtain mixed liquor L3；
(19) substance C 4 is added in mixed liquor L3, is shaken 25 minutes in the shaking table that temperature is 35 DEG C, be filtered to remove liquid
Substance C 5 is obtained, substance C 5 is placed after the ethanol washing that 300mL mass percent concentrations are 90% in 105 DEG C of drying box
40 minutes, obtain material D；
(20) the fluoro- 3- nitros -5- chloropyridines of 11.3 grams of 2- and 14.5 grams of N- (the chloro- 3- pyridazinyls of 6-) butyramides are added to
In 1200mL absolute ethyl alcohols, shaken 35 minutes in the shaking table that temperature is 35 DEG C, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor
M1, mixed liquor M2, mixed liquor M3, mixed liquor M4；
(21) 4.2 grams of 2- butyl -3- methylpyrazines and 2.6 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M1, in temperature
To be shaken 35 minutes in 30 DEG C of shaking tables, mixed liquor N1 is obtained；
(22) the chloro- 7- Trifluoromethylquinocarboxylics of 3.3 grams of 4- are added in mixed liquor N1,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor O1；
(23) material D is added in mixed liquor O1, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To material D1, material D1 is placed 145 minutes in 75 DEG C of drying box, obtains material D2；
(24) 3.9 grams of 2- butyl -3- methylpyrazines and 2.3 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M2, in temperature
To be shaken 35 minutes in 30 DEG C of shaking tables, mixed liquor N2 is obtained；
(25) the chloro- 7- Trifluoromethylquinocarboxylics of 3.0 grams of 4- are added in mixed liquor N2,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor O2；
(26) material D2 is added in mixed liquor O2, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Material D3 is obtained, material D3 is placed 145 minutes in 75 DEG C of drying box, obtains material D4；
(27) 3.6 grams of 2- butyl -3- methylpyrazines and 2.0 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M3, in temperature
To be shaken 35 minutes in 30 DEG C of shaking tables, mixed liquor N3 is obtained；
(28) the chloro- 7- Trifluoromethylquinocarboxylics of 2.7 grams of 4- are added in mixed liquor N3,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor O3；
(29) material D4 is added in mixed liquor O3, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Material D5 is obtained, material D5 is placed 145 minutes in 75 DEG C of drying box, obtains material D6；
(30) 3.3 grams of 2- butyl -3- methylpyrazines and 1.7 grams of 6- cyano group -2- chloropyrazines are added in mixed liquor M4, in temperature
To be shaken 35 minutes in 30 DEG C of shaking tables, mixed liquor N4 is obtained；
(31) the chloro- 7- Trifluoromethylquinocarboxylics of 2.4 grams of 4- are added in mixed liquor N4,35 is shaken in the shaking table that temperature is 30 DEG C
Minute, obtain mixed liquor O4；
(32) material D6 is added in mixed liquor O4, is shaken 45 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Material D7 is obtained, material D7 is placed 145 minutes in 75 DEG C of drying box, obtained material is Ti-base catalyst.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110310844A (en) * | 2019-06-28 | 2019-10-08 | 华中科技大学 | Sludge utilizes method and the nickel foam-nitrogen-doped nanometer carbon composite prepared by this method |
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