CN107020087A - The preparation method of ozone Heterogeneous oxidation solid catalyst - Google Patents
The preparation method of ozone Heterogeneous oxidation solid catalyst Download PDFInfo
- Publication number
- CN107020087A CN107020087A CN201710276703.0A CN201710276703A CN107020087A CN 107020087 A CN107020087 A CN 107020087A CN 201710276703 A CN201710276703 A CN 201710276703A CN 107020087 A CN107020087 A CN 107020087A
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- weight
- component
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- solid catalyst
- potassium
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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 23
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 23
- 239000011949 solid catalyst Substances 0.000 title claims abstract description 19
- 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 48
- 230000003197 catalytic effect Effects 0.000 claims abstract description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 239000004575 stone Substances 0.000 claims abstract description 14
- -1 boromagnesite Substances 0.000 claims abstract description 13
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical class OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000010881 fly ash Substances 0.000 claims abstract description 11
- LWXVCCOAQYNXNX-UHFFFAOYSA-N lithium hypochlorite Chemical compound [Li+].Cl[O-] LWXVCCOAQYNXNX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000002148 esters Chemical class 0.000 claims abstract description 10
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 10
- 239000010456 wollastonite Substances 0.000 claims abstract description 10
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 9
- 235000005340 Asparagus officinalis Nutrition 0.000 claims abstract description 8
- 150000001412 amines Chemical class 0.000 claims abstract description 8
- 150000001413 amino acids Chemical class 0.000 claims abstract description 8
- 125000003963 dichloro group Chemical group Cl* 0.000 claims abstract description 8
- 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 8
- 235000016768 molybdenum Nutrition 0.000 claims abstract description 8
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 8
- 235000010339 sodium tetraborate Nutrition 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
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 7
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 7
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 6
- 229910021538 borax Inorganic materials 0.000 claims abstract description 6
- ITZXULOAYIAYNU-UHFFFAOYSA-N cerium(4+) Chemical compound [Ce+4] ITZXULOAYIAYNU-UHFFFAOYSA-N 0.000 claims abstract description 6
- RWXOJQGSZWUIEJ-UHFFFAOYSA-K lanthanum(3+);octadecanoate Chemical compound [La+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O RWXOJQGSZWUIEJ-UHFFFAOYSA-K 0.000 claims abstract description 6
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 6
- 229960004889 salicylic acid Drugs 0.000 claims abstract description 6
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract description 4
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229940094989 trimethylsilane Drugs 0.000 claims abstract description 4
- AUZRORBINHVFFD-UHFFFAOYSA-N [Rh]N=O Chemical compound [Rh]N=O AUZRORBINHVFFD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 3
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 230000007704 transition Effects 0.000 claims description 8
- 241000234427 Asparagus Species 0.000 claims description 7
- 239000010970 precious metal Substances 0.000 claims description 7
- 229910001868 water Inorganic materials 0.000 claims description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- 239000003995 emulsifying agent Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- OLGPDUKUFCIQPH-UHFFFAOYSA-N [Na].[Na].[Na].N(=O)[Rh] Chemical compound [Na].[Na].[Na].N(=O)[Rh] OLGPDUKUFCIQPH-UHFFFAOYSA-N 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- ILRLTAZWFOQHRT-UHFFFAOYSA-N potassium;sulfuric acid Chemical compound [K].OS(O)(=O)=O ILRLTAZWFOQHRT-UHFFFAOYSA-N 0.000 claims 1
- PDSVZUAJOIQXRK-UHFFFAOYSA-N trimethyl(octadecyl)azanium Chemical compound CCCCCCCCCCCCCCCCCC[N+](C)(C)C PDSVZUAJOIQXRK-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 17
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 abstract description 9
- 238000001994 activation Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 2
- 244000003416 Asparagus officinalis Species 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000003245 coal Substances 0.000 abstract 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 230000004913 activation Effects 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000010433 feldspar Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- TZIZDKHKROKBAJ-UHFFFAOYSA-N [Rh].[Na].[Na].[Na] Chemical compound [Rh].[Na].[Na].[Na] TZIZDKHKROKBAJ-UHFFFAOYSA-N 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000006385 ozonation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 150000003870 salicylic acids Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- QNFVGEYXTFRSLK-UHFFFAOYSA-N 2-$l^{1}-sulfanylethanamine Chemical group NCC[S] QNFVGEYXTFRSLK-UHFFFAOYSA-N 0.000 description 1
- 229910004835 Na2B4O7 Inorganic materials 0.000 description 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000010883 coal ash Substances 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 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
- 239000000839 emulsion Substances 0.000 description 1
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 125000000018 nitroso group Chemical group N(=O)* 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/652—Chromium, molybdenum or tungsten
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
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.With medical stone, wollastonite, potassium feldspar, boromagnesite, flyash and taking coal gangue as carrier, carrier is after lithium hypochlorite and double (acetylacetone,2,4-pentanedione) beryllium reamings, add octadecyl trimethyl ammonium chloride and activation process is carried out under ul-trasonic irradiation, then activated carrier in hydrothermal reaction kettle with composite mineralizer borax and potassium sulfate, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone) yttrium (III) dihydrate, Lanthanum Stearate, four (2, 2, 6, 6 tetramethyls 3, 5 heptadione acid) cerium (IV), three [N, double (trimethyl silane) amine of N] erbium, catalytic active center component predecessor titanocenes ring substituted salicylic acid complex, L lucid asparagus amino acid molybdenums, six nitroso rhodium trisodiums, the ammino platinum of dichloro two, hydro-thermal reaction is carried out under the effect of etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester, drying removes 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 medical stone, wollastonite, potassium feldspar, boromagnesite, fine coal
Ash, gangue composition, by weight, medical stone:Wollastonite:Potassium feldspar:Boromagnesite:Flyash:The weight ratio of gangue=（5
~15）:（7~17）:（9~19）:（11~21）:（13~23）:（15~25）, by weight, component A:The weight of B component it
Than=1:（10~20）, component C is octadecyl trimethyl ammonium chloride, by weight, component C:The weight of reaming modified support it
Than=1:（5~10）, D components are by composite mineralizer borax, potassium sulfate, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone)
Yttrium (III) dihydrate, Lanthanum Stearate, four (DPM dpm,dipivalomethane acid) ceriums (IV), three [N, N- double (three
Methyl-monosilane) amine] erbium Rare-earth chemicals, the cyclopentadienyl of catalytic active center predecessor normal transition metallo-organic compound two
Titanacycle substituted salicylic acid complex, L- lucid asparagus amino acid molybdenums and the nitroso rhodium trisodium of precious metal chemical complex six, the ammino of dichloro two
Platinum, emulsifying agent etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester composition, by weight, borax:Potassium sulfate:Three (hexafluoroacetylacetone) yttriums
(III) dihydrate:Lanthanum Stearate:Four (DPM dpm,dipivalomethane acid) ceriums (IV):Three [double (the front threes of N, N-
Base silane) amine] erbium:Titanocenes ring substituted salicylic acid complex:L- lucid asparagus amino acid molybdenums:Six nitroso rhodium trisodiums:Dichloro two
Ammino platinum:The weight ratio of etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester=（4~8）:（6~10）:（3~6）:（4~7）:（5~
8）:（6~9）:（10~15）:（12~18）:（4~7）:（6~9）:（6~20）.Medical stone, wollastonite, the potassium of the B component
Feldspar, boromagnesite, flyash, gangue are crushed respectively, and deionized water washing, which is dried, to be removed after moisture, is entered through standard screen
- 200 mesh of row ,+400 mesh sieves point, it is the mm of 0.0370mm~0.0750 control particle diameter.
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
Medical stone, wollastonite, potassium feldspar, boromagnesite, 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 octadecyl trimethyl ammonium chloride
[C18H37N(CH3)3]+Cl- The aqueous solution, control ultrasonic power density, ultrasonic frequency, temperature and sonic oscillation time, in ultrasound
Under ripple cavitation, octadecyl trimethyl ammonium chloride [C18H37N(CH3)3]+Cl- It is easy to escape into reaming from the aqueous solution and changes
Property carrier duct or be attached to reaming modified support surface, be beneficial to being interconnected and carrier surface activation for carrier duct, increase
Strong adsorptivity；After the completion of ultrasonic activation, ultrasonic surface activated carrier mixed liquor is transferred in hydrothermal reaction kettle, with borax
Na2B4O7·10H2O, potassium sulfate K2SO4Composite mineralizer, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone) yttrium (III)
Dihydrate C15H3F18O6Y·2H2O, Lanthanum Stearate La (C18H35O2)3, four (DPM dpm,dipivalomethanes acid)
Cerium (IV) C22H38CeO4, three [N, N- double (trimethyl silane) amine] erbium C18H54ErN3Si6Rare-earth chemicals, catalysis
Activated centre component predecessor normal transition metallo-organic compound titanocenes ring substituted salicylic acid complex (C10H10)Ti
(C7H4O3), L- lucid asparagus amino acid molybdenum Mo [OOCCH2CH(NH2)COO]3(H2O)3With six nitroso rhodium trisodium Na3Rh(NO2)6、
The ammino platinum Pt (NH of dichloro two3)2Cl2Precious metal chemical complex, in emulsifying agent etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester [(C16H33)N
(CH3)2C2H5]+ C2H5SO4 -Effect is lower to carry out hydro-thermal reaction, and mineralizer accelerates diffusion, activates reactant lattice, promotes
The progress of solid phase reaction, ultrasonic surface activated carrier and Rare-earth chemicals, normal transition metallo-organic compound,
Precious metal chemical complex Uniform Doped, it is anti-that emulsifying agent etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester makes reaction solution form quasi-stationary emulsion
Stop separation of solid and liquid, sedimentation, while to the further surface active of porous carrier, by certain temperature, the hydro-thermal reaction of time,
Drying obtains the fine silt thing of Uniform Doped；The fine silt thing of Uniform Doped is in Muffle furnace, through high temperature sintering, therein organic
Thing carbonization further enhances the microcellular structure of porous carrier, obtains porous carrier supported rare earth metal oxide, transition
The ozone Heterogeneous oxidation solid catalyst of metal oxide and the catalytic active center of noble metal formation, improves catalyst
Mithridatism and catalytic activity.
Relative to art methods, outstanding feature of the present invention is long using medical stone, wollastonite, potassium in technology of preparing
Stone, boromagnesite, flyash, gangue porous material make carrier, due to lithium hypochlorite LiClO and double (acetylacetone,2,4-pentanedione) berylliums
C10H14BeO4Reaming effect, octadecyl trimethyl ammonium chloride [C18H37N(CH3)3]+Cl-, etradecyldimethylamine QAE quaternary aminoethyl sulphur
Acid esters [(C16H33)N(CH3)2C2H5]+C2H5SO4 -To being interconnected and surface activation for duct；Made by hydro-thermal reaction dilute
Earth metal organic compound, normal transition metallo-organic compound and precious metal chemical complex reach Uniform Doped and are attached to carrier
In surface and duct, high temperature sintering makes organic matter carbonization strengthen and form multi-level microcellular structure, and porous carrier is born
Carry the multi-element metal catalytic active center and porous carrier knot of rare-earth oxide, transition metal oxide and noble metal formation
Close more firm, the ozone Heterogeneous oxidation solid catalyst of preparation has a stronger adsorptivity, the cooperative effect of multi-element metal,
Stability and high activity that particularly doped precious metal has, can suppress liquating out for metal catalytic activity component, 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, be added to volume for 500ml can be closed
It is uniformly mixed in reactor, the weight concentration of the aqueous solution is 2.1%, lithium hypochlorite:The weight of double (acetylacetone,2,4-pentanedione) berylliums it
Than=1:1.2；Add deionized water wash to it is neutral, 103 DEG C dry and remove the mesh standard sieve of -200 mesh of sieving after moisture~+400
2.75g medical stones, 3.75g wollastonites, 4.75g potassium feldspars, 5.75g boromagnesites, 6.75g flyash, 7.75g gangues, secondary chlorine
The weight of sour lithium and double (acetylacetone,2,4-pentanedione) berylliums（3g）:The weight of porous material（31.5g）=1:10.5,36 DEG C are warming up to, continues to stir
Reaming modified support 31g is obtained after mixing reaction 3.2h, filtering, 103 DEG C of dry constant weights；In 500ml ultrasound reactors, input
Reaming modified support 31g, adds the aqueous solution that 3.25g octadecyl trimethyl ammonium chlorides are dissolved in 100ml deionized waters, the water
The weight concentration of solution is 3.1%, is uniformly mixed, octadecyl trimethyl ammonium chloride（3.25g）:Reaming modified support
（31g ）=1:9.5；It is 0.4 W/m to control ultrasonic power density3, ultrasonic frequency 21kHz, 41 DEG C of temperature, sonic oscillation
2.2h；After the completion of ultrasonic activation, the ultrasonic surface activated carrier mixed liquor in ultrasound reactor is transferred to 500ml hydro-thermals anti-
Answer in kettle, add by 2.1g boraxs, 3.05g potassium sulfates, 1.6g tri- (hexafluoroacetylacetone) yttrium (III) dihydrate,
2.05g Lanthanum Stearates, 2.6g tetra- (DPM dpm,dipivalomethane acid) cerium (IV), [double (trimethyls of N, N- of 3.05g tri-
Silane) amine] erbium, 5.05g titanocenes ring substituted salicylic acids complex, 6.1gL- lucid asparagus amino acid molybdenum, the nitrosos of 2.05g six
It is water-soluble that rhodium trisodium, the ammino platinum of 3.1g dichloros two, 3.05g etradecyldimethylamine QAE quaternary aminoethyl sulfuric esters and 50ml deionized waters are prepared
Liquid, the weight concentration of the aqueous solution is 40.3%, the weight of the aqueous solution:The weight of ultrasonic surface activated carrier mixed liquor=
83.8g: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 for 105 DEG C
Thing；Fine silt thing is in Muffle furnace, 620 DEG C, calcination 3.2h, and after cooling down, the ozone that can obtain fine particle shape is heterogeneous
Oxidized solid catalyst.
Embodiment 2:
0.24g lithium hypochlorites, double (acetylacetone,2,4-pentanedione) berylliums of 0.36g, 10ml deionized waters, be added to volume for 100ml can be closed
It is uniformly mixed in reactor, the weight concentration of the aqueous solution is 5.7%, lithium hypochlorite:The weight of double (acetylacetone,2,4-pentanedione) berylliums it
Than=1:1.5；Add deionized water wash to it is neutral, 103 DEG C dry and remove the mesh standard sieve of -200 mesh of sieving after moisture~+400
1.45g medical stones, 1.65g wollastonites, 1.85g potassium feldspars, 2.05g boromagnesites, 2.25g flyash, 2.45g gangues, secondary chlorine
The weight of sour lithium and double (acetylacetone,2,4-pentanedione) berylliums（0.6g）:The weight of porous material（11.7g）=1:19.5, it is warming up to 48 DEG C, continuation
Reaming modified support 11.5g is obtained after stirring reaction 5.8h, filtering, 105 DEG C of dry constant weights；In 100ml ultrasound reactors,
Reaming modified support 11.5g is put into, the aqueous solution that 2.2g octadecyl trimethyl ammonium chlorides are dissolved in 26ml deionized waters is added,
The weight concentration of the aqueous solution is 7.8%, is uniformly mixed, octadecyl trimethyl ammonium chloride（2.2g）:Reaming modified support
（11.5g ）=1:5.2；It is 0.7 W/m to control ultrasonic power density3, ultrasonic frequency 29kHz, 54 DEG C of temperature, sonic oscillation
4.7h；After the completion of ultrasonic activation, the ultrasonic surface activated carrier mixed liquor in ultrasound reactor is transferred to 100ml hydro-thermals anti-
Answer in kettle, add by 0.78g boraxs, 0.97g potassium sulfates, 0.58g tri- (hexafluoroacetylacetone) yttrium (III) dihydrate,
0.67g Lanthanum Stearates, 0.78g tetra- (DPM dpm,dipivalomethane acid) cerium (IV), [double (front threes of N, N- of 0.87g tri-
Base silane) amine] erbium, 1.48g titanocenes ring substituted salicylic acids complex, 1.77gL- lucid asparagus amino acid molybdenum, the nitrous of 0.68g six
What base rhodium trisodium, the ammino platinum of 0.87g dichloros two, 1.98g etradecyldimethylamine QAE quaternary aminoethyl sulfuric esters and 10ml deionized waters were prepared
The aqueous 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 for 105 DEG C
Thing；Fine silt thing is in Muffle furnace, 930 DEG C, calcination 7.5h, and after cooling down, the ozone that can obtain fine particle shape is heterogeneous
Oxidized 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
Divide and be made up of medical stone, wollastonite, potassium feldspar, boromagnesite, flyash, gangue, by weight, medical stone:Wollastonite:Potassium is long
Stone:Boromagnesite: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 chlorination octadecyl trimethyl
Ammonium, by weight, component C:Weight ratio=1 of reaming modified support:（5~10）, D components are by composite mineralizer borax, sulfuric acid
Potassium, catalytic activity auxiliary agent predecessor three (hexafluoroacetylacetone) yttrium (III) dihydrate, Lanthanum Stearate, four (2,2,6,6- tetra-
Methyl -3,5- heptadione acid) cerium (IV), three [N, N- double (trimethyl silane) amine] erbium Rare-earth chemicals, catalysis lives
Property center predecessor normal transition metallo-organic compound titanocenes ring substituted salicylic acid complex, L- lucid asparagus amino acid molybdenums and
The nitroso rhodium trisodium of precious metal chemical complex six, the ammino platinum of dichloro two, emulsifying agent etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester composition, are pressed
Weight meter, borax:Potassium sulfate:Three (hexafluoroacetylacetone) yttrium (III) dihydrates:Lanthanum Stearate:Four (2,2,6,6- tetramethyls
Base -3,5- heptadione acid) cerium (IV):Three [double (trimethyl silane) amine of N, N-] erbiums:Titanocenes ring substituted salicylic acid complex:L-
Lucid asparagus amino acid molybdenum:Six nitroso rhodium trisodiums:The ammino platinum of dichloro two:The weight ratio of etradecyldimethylamine QAE quaternary aminoethyl sulfuric ester
=（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 made up of medical stone, wollastonite, potassium feldspar, boromagnesite, flyash, gangue according to claim 1,
Medical stone, wollastonite, potassium feldspar, boromagnesite, flyash, gangue are crushed respectively, and deionized water washing, which is dried, removes water
After point, sieved through standard screen, it is 0.0370mm~0.0750mm to control particle diameter.
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