CN107020109A - The preparation method of ozone Heterogeneous oxidation solid catalyst - Google Patents
The preparation method of ozone Heterogeneous oxidation solid catalyst Download PDFInfo
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- CN107020109A CN107020109A CN201710274706.0A CN201710274706A CN107020109A CN 107020109 A CN107020109 A CN 107020109A CN 201710274706 A CN201710274706 A CN 201710274706A CN 107020109 A CN107020109 A CN 107020109A
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 230000003647 oxidation Effects 0.000 title claims abstract description 25
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 25
- 239000011949 solid catalyst Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 40
- 230000003197 catalytic effect Effects 0.000 claims abstract description 25
- -1 monoalky lether trimethyl ammonium chloride Chemical class 0.000 claims abstract description 19
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- LWXVCCOAQYNXNX-UHFFFAOYSA-N lithium hypochlorite Chemical compound [Li+].Cl[O-] LWXVCCOAQYNXNX-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004575 stone Substances 0.000 claims abstract description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000010881 fly ash Substances 0.000 claims abstract description 12
- 235000012222 talc Nutrition 0.000 claims abstract description 11
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010443 kyanite Substances 0.000 claims abstract description 10
- 229910052850 kyanite Inorganic materials 0.000 claims abstract description 10
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims abstract description 10
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000454 talc Substances 0.000 claims abstract description 9
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- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 8
- 239000010941 cobalt Substances 0.000 claims abstract description 8
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 8
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 8
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 claims abstract description 8
- BYDILAVGJRCJOJ-UHFFFAOYSA-N O.O.[Y+3] Chemical compound O.O.[Y+3] BYDILAVGJRCJOJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- QAMFBRUWYYMMGJ-UHFFFAOYSA-N hexafluoroacetylacetone Chemical compound FC(F)(F)C(=O)CC(=O)C(F)(F)F QAMFBRUWYYMMGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 6
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 6
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021538 borax Inorganic materials 0.000 claims abstract description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 6
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- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims abstract description 6
- NQNOMXXYKHWVKR-UHFFFAOYSA-N methylazanium;sulfate Chemical compound NC.NC.OS(O)(=O)=O NQNOMXXYKHWVKR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims abstract description 5
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- KZXFBCUXEQXICP-UHFFFAOYSA-N [W].C=1(O)C(O)=CC=CC1.C(CN)N Chemical compound [W].C=1(O)C(O)=CC=CC1.C(CN)N KZXFBCUXEQXICP-UHFFFAOYSA-N 0.000 claims abstract description 4
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- ZGGPNDKKJIWQJU-UHFFFAOYSA-N 2-(pyridine-4-carbonylhydrazinylidene)propanoic acid Chemical compound OC(=O)C(C)=NNC(=O)C1=CC=NC=C1 ZGGPNDKKJIWQJU-UHFFFAOYSA-N 0.000 claims description 3
- KPQDSKZQRXHKHY-UHFFFAOYSA-N gold potassium Chemical compound [K].[Au] KPQDSKZQRXHKHY-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
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- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims 2
- 241000195493 Cryptophyta Species 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 17
- 230000000694 effects Effects 0.000 abstract description 6
- 238000001994 activation Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- QSJXEFYPDANLFS-UHFFFAOYSA-N Diacetyl Chemical group CC(=O)C(C)=O QSJXEFYPDANLFS-UHFFFAOYSA-N 0.000 abstract 1
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- 238000005245 sintering Methods 0.000 description 4
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
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- 241000206761 Bacillariophyta Species 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
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- 239000002671 adjuvant Substances 0.000 description 2
- ONRPGGOGHKMHDT-UHFFFAOYSA-N benzene-1,2-diol;ethane-1,2-diamine Chemical class NCCN.OC1=CC=CC=C1O ONRPGGOGHKMHDT-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 229940048820 edetates Drugs 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 2
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- 229910000510 noble metal Inorganic materials 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
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- YRDGEBQKBARXFW-UHFFFAOYSA-N (dimethyl-$l^{3}-sulfanyl)methane Chemical compound C[S](C)C YRDGEBQKBARXFW-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229910004835 Na2B4O7 Inorganic materials 0.000 description 1
- 241000255964 Pieridae Species 0.000 description 1
- 229910052773 Promethium Inorganic materials 0.000 description 1
- AXNBHOOQHIIQFA-UHFFFAOYSA-N [S].C(F)(F)F Chemical compound [S].C(F)(F)F AXNBHOOQHIIQFA-UHFFFAOYSA-N 0.000 description 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- ZQSSRUAWBFTSKE-UHFFFAOYSA-N benzene-1,2-diol;tungsten Chemical compound [W].OC1=CC=CC=C1O ZQSSRUAWBFTSKE-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
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- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8993—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with chromium, molybdenum or tungsten
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Abstract
The present invention relates to a kind of preparation method of ozone Heterogeneous oxidation solid catalyst, category environmental protection and technical field of chemical engineering catalysts.It is pure with diatom, kyanite, talcum, sal soda stone, flyash and taking coal gangue as carrier are after lithium hypochlorite and double (acetylacetone,2,4-pentanedione) beryllium reamings, add surfactant monoalky lether trimethyl ammonium chloride and activation process is carried out under ul-trasonic irradiation, then carrier in hydrothermal reaction kettle with composite mineralizer borax and potassium sulfate, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone) yttrium (III) dihydrate, three cyclopentadiene promethiums, three (4, 4, (2 thiophene) 1 of 4 trifluoro 1, 3 diacetyl) europium, trifluoromethayl sulfonic acid thulium (III), catalytic active center predecessor pyruvic acid isonicotinoyl hydrazone vanadium, cobalt edetate, ethylenediamine pyrocatechol tungsten complex and the golden potassium of tetrachloro, hydro-thermal reaction is carried out under the effect of emulsifying agent oleamide oxypropyl trimethyl sulfate methyl ammonium, drying is removed after moisture, calcination obtains ozone Heterogeneous oxidation solid catalyst in Muffle furnace.
Description
Technical field
The present invention relates to a kind of preparation method of ozone Heterogeneous oxidation solid catalyst, category environmental protection and chemical catalyst skill
Art field.
Background technology
Ozonation technology using ozone oxidation ability it is strong the characteristics of, can be by many organic pollution oxidation Decompositions, extensively
For wastewater treatment.Catalytic ozonation technology is divided into ozone homogeneous catalytic oxidation and ozone heterogeneous catalytic oxidation, and ozone is equal
Phase catalysis oxidation has that the more difficult separation and recovery of catalyst is reused, ozone utilization rate is low causes water process operating cost higher,
Organic pollutant removal rate is relatively low simultaneously and easily causing secondary pollution of water is limited to its application;Ozone heterogeneous catalysis oxygen
There is change technology catalyst to be easily isolated and recycled and reusable, ozone utilization rate is high, organic pollutant removal rate is higher, drop
Low water process operating cost and receive significant attention its application the advantages of do not result in secondary pollution.Ozone heterogeneous catalysis
It is to reach local organic matter enrichment by catalyst surface absorption organic matter that oxidation of organic compounds, which is decomposed, while ozone molecule absorption exists
The hydroxyl radical free radical that catalyst surface produces high activity under catalyst action decomposes organic matter.Ozone heterogeneous catalytic oxidation
Handle in waste water technology, core technology is the preparation of ozone Heterogeneous oxidation solid catalyst.
Ozone Heterogeneous oxidation solid catalyst is generally made up of carrier, activated centre and auxiliary agent.Due to being polluted in waste water
Species are various, complex chemical composition feature, can produce harmful effect to performance such as absorption, the mithridatism of catalyst.
Prepare that the carrier structure that ozone Heterogeneous oxidation solid catalyst uses is more single at present, adsorptivity is relatively low;Activated centre is universal
Using normal transition metal salt, mithridatism is poor;Preparation method mainly has infusion process, the precipitation method, mixing method and collosol and gel etc.
Method attachment activity center and adjuvant component are easily liquated out in carrier surface, activated centre and adjuvant component, cause catalyst
Easily lose catalytic activity.For exist in current ozone Heterogeneous oxidation solid catalyst preparation method Catalyst Adsorption compared with
Low, mithridatism is poor and easily loses catalytic activity problem, and exploitation is strengthened using multicomponent porous carrier through reaming, surface active
Catalyst Adsorption, makees catalytic activity auxiliary agent predecessor, normal transition Organometallic using Rare-earth chemicals and closes
Thing and precious metal chemical complex are made catalytic active center predecessor and contained with multicomponent porous carrier through hydro-thermal reaction, high temperature sintering preparation
The ozone Heterogeneous oxidation solid catalyst of multi-element metal has to improve the preparation method of catalyst mithridatism and catalytic activity
Larger environmental benefit and higher practical value.
The content of the invention
For existing in current ozone Heterogeneous oxidation solid catalyst preparation method, Catalyst Adsorption is relatively low, mithridatism
Poor to lose catalytic activity problem with easy, exploitation strengthens catalyst using multicomponent porous carrier through reaming, surface active
Adsorptivity, catalytic activity auxiliary agent predecessor, normal transition metallo-organic compound and expensive are made using Rare-earth chemicals
Metallic compound is made catalytic active center predecessor and prepared with multicomponent porous carrier through hydro-thermal reaction, high temperature sintering containing polynary gold
The ozone Heterogeneous oxidation solid catalyst of category to improve the preparation method of catalyst mithridatism and catalytic activity, it is characterized in that
Component A can be added in closed reactor and deionized water stirring prepares the aqueous solution, the weight concentration for control component A is 2%~6%,
After the completion of prepared by solution, B component is added under agitation, 35 DEG C~50 DEG C are warming up to, continues stirring reaction 3h~6h, is filtered, instead
Product is answered to obtain reaming modified support after 102 DEG C~106 DEG C dry constant weights;Reaming modified support puts into ultrasound reactor,
The aqueous solution prepared by component C and deionized water is added, the weight concentration of component C is 3%~8%, is uniformly mixed, and control is super
Sound power density is 0.3~0.8W/m3, frequency 20kHz~30kHz, 40 DEG C~55 DEG C, sonic oscillation 2h~5h obtains ultrasound
Surface active carrier mixed liquor;Ultrasonic surface activated carrier mixed liquor is transferred in hydrothermal reaction kettle, add D components and go from
The aqueous solution that sub- water is prepared, the weight concentration of D components is 40%~55%, by weight, D component deionized water solutions:Ultrasonic table
Weight ratio=1 of face activated carrier mixed liquor:(1.5~2), control 120 DEG C~180 DEG C of temperature, the hydro-thermal reaction time be 8h~
16h, then dries to obtain fine particle;Fine particle is in Muffle furnace, 600 DEG C~950 DEG C, and calcination 3h~8h obtains ozone non-
Homogeneous oxidizing solid catalyst.The component A is made up of lithium hypochlorite, double (acetylacetone,2,4-pentanedione) berylliums, by weight, lithium hypochlorite:
Weight ratio=1 of double (acetylacetone,2,4-pentanedione) berylliums:(1~1.6), B component is by diatom is pure, kyanite, talcum, sal soda stone, flyash,
Gangue is constituted, and by weight, diatom is pure:Kyanite:Talcum:Sal soda stone:Flyash:The weight ratio of gangue=(5~
15):(7~17):(9~19):(11~21):(13~23):(15~25), by weight, component A:The weight ratio of B component
=1:(10~20), component C is monoalky lether trimethyl ammonium chloride, by weight, component C:The weight ratio of reaming modified support
=1:(5~10), D components are by composite mineralizer borax, potassium sulfate, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone) yttrium
(III) dihydrate, three cyclopentadiene promethiums, three (4,4,4- tri- fluoro- 1- (2- thiophene) -1,3- diacetyl) europiums, fluoroform sulphur
Sour thulium (III) Rare-earth chemicals, catalytic active center predecessor normal transition metallo-organic compound pyruvic acid is different
The golden potassium of icotinoylhydrazones vanadium, cobalt edetate, ethylenediamine pyrocatechol tungsten complex and precious metal chemical complex tetrachloro, emulsifying agent oleamide
Oxypropyl trimethyl sulfate methyl ammonium is constituted, by weight, borax:Potassium sulfate:Three (hexafluoroacetylacetone) yttriums (III) two are hydrated
Thing:Three cyclopentadiene promethiums:Three (4,4,4- tri- fluoro- 1- (2- thiophene) -1,3- diacetyl) europiums:Trifluoromethayl sulfonic acid thulium (III):Third
Ketone acid isonicotinoyl hydrazone vanadium:Cobalt edetate:Ethylenediamine pyrocatechol tungsten complex:Tetrachloro gold potassium:Oleamide oxypropyl trimethyl sulphur
The weight ratio of sour ammonium methyl=(4~8):(6~10):(3~6):(4~7):(5~8):(6~9):(10~15):(12~
18):(4~7):(6~9):(6~20).The diatom of the B component is pure, kyanite, talcum, sal soda stone, flyash, gangue
Crushed respectively, deionized water washing, which is dried, to be removed after moisture, is carried out -200 mesh ,+400 mesh sieves point through standard screen, is controlled grain
Footpath is the mm of 0.0370mm~0.0750.
What the technical method of the present invention was realized in:Lithium hypochlorite LiClO, double (second can be being added in closed reactor
Acyl acetone) beryllium C10H14BeO4The aqueous solution is prepared with deionized water stirring, it is 0.0370mm~0.0750mm to add particle diameter after screening
Diatom is pure, kyanite, talcum, sal soda stone, flyash and gangue porous material carrier, in certain temperature and stirring condition
Under, the small Be of aqueous solution Ionic Radius2+(0.31Å)、Li+(0.60Å)Displace part ion radius in porous material big
Ca2+(0.99Å)、K+(1.33Å)、Ba2+(1.35Å)Plasma, the aperture of porous material carrier becomes big, surface roughness increase,
Filtering, dries the reaming modified support input ultrasound reactor after constant weight, adds monoalky lether trimethyl ammonium chloride
C12H25O(CH2CH2O)3N+(CH3)3Cl-The aqueous solution, when control ultrasonic power density, ultrasonic frequency, temperature and sonic oscillation
Between, under ultrasonic cavitation effect, monoalky lether trimethyl ammonium chloride C12H25O(CH2CH2O)3N+(CH3)3Cl-It is easy to from water-soluble
Liquid escapes into reaming modified support duct or is attached to reaming modified support surface, be beneficial to carrier duct be interconnected and
Carrier surface is activated, and enhances adsorptivity;After the completion of ultrasonic activation, ultrasonic surface activated carrier mixed liquor is transferred to hydro-thermal reaction
In kettle, with borax Na2B4O7·10H2O, potassium sulfate K2SO4The composite mineralizer, (hexafluoroacetylacetonate of catalytic activity auxiliary agent predecessor three
Ketone) yttrium (III) dihydrate C15H3F18O6Y·2H2O, three cyclopentadiene promethium Pm (C5H5)3, three (fluoro- 1- (the 2- thiophenes of 4,4,4- tri-
Fen) -1,3- diacetyl) europium C24H18EuF9O6S3, trifluoromethayl sulfonic acid thulium (III) C3F9O9S3Tm Rare-earth chemicals,
Catalytic active center component predecessor normal transition metallo-organic compound pyruvic acid isonicotinoyl hydrazone vanadium [VO2(C9H8N3O5)]
(C5H5N), cobalt edetate C12H22 O14Co, ethylenediamine pyrocatechol tungsten complex (NH2 CH2CH2NH3)2[ W(VI)O2
(OC6H4O)2] and the golden potassium KAuCl of precious metal chemical complex tetrachloro4, in emulsifying agent oleamide oxypropyl trimethyl sulfate methyl ammonium
[C17H33COCH2CH2CH2N( CH3)3]+ CH3SO4 -Effect is lower to carry out hydro-thermal reaction, and mineralizer accelerates diffusion, makes reactant
Lattice is activated, and promotes the progress of solid phase reaction, ultrasonic surface activated carrier and Rare-earth chemicals, normal transition gold
Belong to organic compound, precious metal chemical complex Uniform Doped, emulsifying agent oleamide oxypropyl trimethyl sulfate methyl ammonium makes reaction solution shape
Separation of solid and liquid, sedimentation are prevented into quasi-stationary emulsion, while to the further surface active of porous carrier, by a constant temperature
Degree, the hydro-thermal reaction of time, drying obtain the fine silt thing of Uniform Doped;The fine silt thing of Uniform Doped is in Muffle furnace, warp
High temperature sintering, organic matter carbonization therein further enhances the microcellular structure of porous carrier, obtains porous carrier load
The ozone Heterogeneous oxidation solid of the catalytic active center of rare-earth oxide, transition metal oxide and noble metal formation is urged
Agent, improves the mithridatism and catalytic activity of catalyst.
Relative to art methods, outstanding feature of the present invention be in technology of preparing using diatom is pure, kyanite, talcum,
Sal soda stone, flyash, gangue porous material make carrier, due to lithium hypochlorite LiClO and double (acetylacetone,2,4-pentanedione) beryllium C10H14BeO4
Reaming effect, monoalky lether trimethyl ammonium chloride C12H25O(CH2CH2O)3N+(CH3)3Cl-, oleamide oxypropyl trimethyl sulfuric acid
Ammonium methyl [C17H33COCH2CH2CH2N( CH3)3]+ CH3SO4 -To being interconnected and surface activation for duct;Pass through hydro-thermal
Reaction makes Rare-earth chemicals, normal transition metallo-organic compound and precious metal chemical complex reach Uniform Doped and attached
In in carrier surface and duct, high temperature sintering makes organic matter carbonization strengthen and form multi-level microcellular structure, many
The carrier loaded rare-earth oxide in hole, transition metal oxide and noble metal formation multi-element metal catalytic active center with it is many
Hole carrier combination is more firm, and the ozone Heterogeneous oxidation solid catalyst of preparation has stronger adsorptivity, multi-element metal
Cooperative effect, stability and high activity that particularly doped precious metal has, can suppress the liquate of metal catalytic activity component
Go out, improve the mithridatism and catalytic activity of catalyst, with good environmental benefit and economic benefit.
Embodiment
Embodiment 1:1.35g lithium hypochlorites, double (acetylacetone,2,4-pentanedione) berylliums of 1.65g, 140ml deionized waters, being added to volume is
500ml's can be uniformly mixed in closed reactor, and the weight concentration of the aqueous solution is 2.1%, lithium hypochlorite:Double (levulinics
Ketone) beryllium weight ratio=1:1.2;Add deionized water wash to it is neutral, 103 DEG C dry remove -200 mesh of sieving after moisture~+
The 2.75g diatoms of 400 mesh standard sieves are pure, 3.75g kyanites, 4.75g talcums, 5.75g sal soda stone, 6.75g flyash, 7.75g
The weight of gangue, lithium hypochlorite and double (acetylacetone,2,4-pentanedione) berylliums(3g):The weight of porous material(31.5g)=1:10.5, it is warming up to
36 DEG C, reaming modified support 31g is obtained after continuing stirring reaction 3.2h, filtering, 103 DEG C of dry constant weights;It is anti-in 500ml ultrasonic waves
Answer in device, put into reaming modified support 31g, add 3.25g monoalky lether trimethyl ammonium chlorides and be dissolved in 100ml deionized waters
The aqueous solution, the weight concentration of the aqueous solution is 3.1%, is uniformly mixed, monoalky lether trimethyl ammonium chloride(3.25g):Reaming
Modified support(31g )=1:9.5;It is 0.4W/m to control ultrasonic power density3, ultrasonic frequency 21kHz, 41 DEG C of temperature, ultrasound
Vibrate 2.2h;After the completion of ultrasonic activation, the ultrasonic surface activated carrier mixed liquor in ultrasound reactor is transferred to 500ml water
In thermal response kettle, add by 2.1g boraxs, 3.05g potassium sulfates, 1.6g tri- (hexafluoroacetylacetone) yttrium (III) dihydrate,
The cyclopentadiene promethiums of 2.05g tri-, 2.6g tri- (4,4,4- tri- fluoro- 1- (2- thiophene) -1,3- diacetyl) europium, 3.05g fluoroform sulphurs
Sour thulium (III), 5.05g pyruvic acid isonicotinoyl hydrazones vanadium, 6.1g cobalt edetates, 2.05g ethylenediamine pyrocatechols tungsten complex,
The aqueous solution that 3.1g tetrachloros gold potassium, 3.05g oleamide oxypropyl trimethyl sulfate methyl ammoniums and 50ml deionized waters are prepared, this is water-soluble
The weight concentration of liquid is 40.3%, the weight of the aqueous solution:Weight=83.8g of ultrasonic surface activated carrier mixed liquor:134.25g
=1:1.6,125 DEG C of temperature is controlled, the hydro-thermal reaction time is 8.3h, then dries to obtain fine silt thing for 105 DEG C;Fine silt thing is in horse
Not in stove, 620 DEG C, calcination 3.2h after cooling down, can obtain the ozone Heterogeneous oxidation solid catalyst of fine particle shape.
Embodiment 2:0.24g lithium hypochlorites, double (acetylacetone,2,4-pentanedione) berylliums of 0.36g, 10ml deionized waters, being added to volume is
100ml's can be uniformly mixed in closed reactor, and the weight concentration of the aqueous solution is 5.7%, lithium hypochlorite:Double (levulinics
Ketone) beryllium weight ratio=1:1.5;Add deionized water wash to it is neutral, 103 DEG C dry remove -200 mesh of sieving after moisture~+
The 1.45g diatoms of 400 mesh standard sieves are pure, 1.65g kyanites, 1.85g talcums, 2.05g sal soda stone, 2.25g flyash, 2.45g
The weight of gangue, lithium hypochlorite and double (acetylacetone,2,4-pentanedione) berylliums(0.6g):The weight of porous material(11.7g)=1:19.5, heating
To 48 DEG C, reaming modified support 11.5g is obtained after continuing stirring reaction 5.8h, filtering, 105 DEG C of dry constant weights;In 100ml ultrasounds
In ripple reactor, reaming modified support 11.5g is put into, 2.2g monoalky lether trimethyl ammonium chlorides is added and is dissolved in 26ml deionizations
The aqueous solution of water, the weight concentration of the aqueous solution is 7.8%, is uniformly mixed, monoalky lether trimethyl ammonium chloride(2.2g):
Reaming modified support(11.5g )=1:5.2;It is 0.7W/m to control ultrasonic power density3, ultrasonic frequency 29kHz, temperature 54
DEG C, sonic oscillation 4.7h;After the completion of ultrasonic activation, the ultrasonic surface activated carrier mixed liquor in ultrasound reactor is transferred to
In 100ml hydrothermal reaction kettles, add by 0.78g boraxs, 0.97g potassium sulfates, 0.58g tri- (hexafluoroacetylacetone) yttrium (III)
Dihydrate, the cyclopentadiene promethiums of 0.67g tri-, 0.78g tri- (4,4,4- tri- fluoro- 1- (2- thiophene) -1,3- diacetyl) europium, 0.87g
Trifluoromethayl sulfonic acid thulium (III), 1.48g pyruvic acid isonicotinoyl hydrazones vanadium, 1.77g cobalt edetates, 0.68g ethylenediamine pyrocatechols
The water that the golden potassium of tungsten complex, 0.87g tetrachloros, 1.98g oleamide oxypropyl trimethyl sulfate methyl ammoniums and 10ml deionized waters are prepared
Solution, the weight concentration of the aqueous solution is 53.3%, the weight of the aqueous solution:The weight of ultrasonic surface activated carrier mixed liquor=
21.43g:39.7g=1:1.9,175 DEG C of temperature is controlled, the hydro-thermal reaction time is 15.5h, then dries to obtain fine silt thing for 105 DEG C;
Fine silt thing is in Muffle furnace, 930 DEG C, calcination 7.5h, after cooling down, can obtain the ozone Heterogeneous oxidation of fine particle shape
Solid catalyst.
Claims (2)
1. a kind of preparation method of ozone Heterogeneous oxidation solid catalyst, it is characterized in that A groups can added in closed reactor
Divide and deionized water stirring prepares the aqueous solution, the weight concentration for controlling component A is 2%~6%, after the completion of prepared by solution, in stirring
Lower addition B component, is warming up to 35 DEG C~50 DEG C, continues stirring reaction 3h~6h, and filtering, reaction product is dry at 102 DEG C~106 DEG C
Reaming modified support is obtained after dry constant weight, reaming modified support input ultrasound reactor, addition is matched somebody with somebody by component C and deionized water
The aqueous solution of system, the weight concentration of component C is 3%~8%, is uniformly mixed, and it is 0.3~0.8W/ to control ultrasonic power density
m3, frequency 20kHz~30kHz, 40 DEG C~55 DEG C, sonic oscillation 2h~5h obtains ultrasonic surface activated carrier mixed liquor, transfer
Into hydrothermal reaction kettle, the aqueous solution that D components and deionized water are prepared is added, the weight concentration of D components is 40%~55%, is pressed
Weight meter, D component deionized water solutions:Weight ratio=1 of ultrasonic surface activated carrier mixed liquor:(1.5~2), control temperature
120 DEG C~180 DEG C, the hydro-thermal reaction time is 8h~16h, then dries to obtain fine silt thing, fine silt thing is in Muffle furnace, 600
DEG C~950 DEG C, calcination 3h~8h obtains ozone Heterogeneous oxidation solid catalyst;The component A by expanding agent lithium hypochlorite,
Double (acetylacetone,2,4-pentanedione) beryllium compositions, by weight, lithium hypochlorite:Weight ratio=1 of double (acetylacetone,2,4-pentanedione) berylliums:(1~1.6), B groups
Point by diatom is pure, kyanite, talcum, sal soda stone, flyash and gangue are constituted, by weight, diatom is pure:Kyanite:It is sliding
Stone:Sal soda stone:Flyash:The weight ratio of gangue=(5~15):(7~17):(9~19):(11~21):(13~
23):(15~25), by weight, component A:Weight ratio=1 of B component:(10~20), component C is monoalky lether trimethyl
Ammonium chloride, by weight, component C:Weight ratio=1 of reaming modified support:(5~10), D components by composite mineralizer borax,
Potassium sulfate, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone) yttrium (III) dihydrate, three cyclopentadiene promethiums, three (4,
4,4- tri- fluoro- 1- (2- thiophene) -1,3- diacetyl) europium, trifluoromethayl sulfonic acid thulium (III) Rare-earth chemicals, catalysis
Activated centre predecessor normal transition metallo-organic compound pyruvic acid isonicotinoyl hydrazone vanadium, cobalt edetate, catechol second two
Amine tungsten complex and the golden potassium of precious metal chemical complex tetrachloro, emulsifying agent oleamide oxypropyl trimethyl sulfate methyl ammonium composition, by weight
Meter, borax:Potassium sulfate:Three (hexafluoroacetylacetone) yttrium (III) dihydrates:Three cyclopentadiene promethiums:Three (4,4,4- tri- is fluoro-
1- (2- thiophene) -1,3- diacetyl) europium:Trifluoromethayl sulfonic acid thulium (III):Pyruvic acid isonicotinoyl hydrazone vanadium:Cobalt edetate:
Ethylenediamine pyrocatechol tungsten complex:Tetrachloro gold potassium:The weight ratio of oleamide oxypropyl trimethyl sulfate methyl ammonium=(4~
8):(6~10):(3~6):(4~7):(5~8):(6~9):(10~15):(12~18):(4~7):(6~9):(6~
20).
2. B component is by diatom is pure, kyanite, talcum, sal soda stone, flyash and gangue are constituted, silicon according to claim 1
Algae is pure, kyanite, talcum, sal soda stone, flyash and gangue are crushed respectively, and deionized water washing, which is dried, removes moisture
Afterwards, sieved through standard screen, it is 0.0370mm~0.0750mm to control particle diameter.
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Application publication date: 20170808 |