CN107020095A - 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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- CN107020095A CN107020095A CN201710276754.3A CN201710276754A CN107020095A CN 107020095 A CN107020095 A CN 107020095A CN 201710276754 A CN201710276754 A CN 201710276754A CN 107020095 A CN107020095 A CN 107020095A
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- potassium
- stone
- iii
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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 24
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 24
- 239000011949 solid catalyst Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000004575 stone Substances 0.000 claims abstract description 25
- 230000003197 catalytic effect Effects 0.000 claims abstract description 24
- -1 boromagnesite Substances 0.000 claims abstract description 23
- 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
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical class OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 12
- 235000012222 talc Nutrition 0.000 claims abstract description 12
- LWXVCCOAQYNXNX-UHFFFAOYSA-N lithium hypochlorite Chemical compound [Li+].Cl[O-] LWXVCCOAQYNXNX-UHFFFAOYSA-N 0.000 claims abstract description 11
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000000454 talc Substances 0.000 claims abstract description 10
- 229910052623 talc Inorganic materials 0.000 claims abstract description 10
- 239000010456 wollastonite Substances 0.000 claims abstract description 10
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 10
- 235000005340 Asparagus officinalis Nutrition 0.000 claims abstract description 8
- 241000723346 Cinnamomum camphora Species 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 8
- 239000002253 acid Substances 0.000 claims abstract description 8
- 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 8
- 150000001413 amino acids Chemical class 0.000 claims abstract description 8
- 229930008380 camphor Natural products 0.000 claims abstract description 8
- 125000003963 dichloro group Chemical group Cl* 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
- 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
- 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
- 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 7
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 7
- 229960004889 salicylic acid Drugs 0.000 claims abstract description 7
- 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
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 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 5
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 4
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000002604 ultrasonography Methods 0.000 claims description 10
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 9
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 241000234427 Asparagus Species 0.000 claims description 7
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 7
- 230000007704 transition Effects 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 5
- 239000010970 precious metal Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000003995 emulsifying agent Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- KPQDSKZQRXHKHY-UHFFFAOYSA-N gold potassium Chemical compound [K].[Au] KPQDSKZQRXHKHY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 241000209140 Triticum Species 0.000 claims 1
- 235000021307 Triticum Nutrition 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 235000012054 meals Nutrition 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 16
- 238000001994 activation Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 4
- PTGJVXFGOMJCCW-UHFFFAOYSA-J Cl[Au](Cl)(Cl)(Cl)[K] Chemical compound Cl[Au](Cl)(Cl)(Cl)[K] PTGJVXFGOMJCCW-UHFFFAOYSA-J 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 244000003416 Asparagus officinalis Species 0.000 abstract 1
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 abstract 1
- 229940063953 ammonium lauryl sulfate Drugs 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 125000004044 trifluoroacetyl group Chemical group FC(C(=O)*)(F)F 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
- 229910001868 water Inorganic materials 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 230000004913 activation Effects 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 5
- 150000002910 rare earth metals Chemical class 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
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 229910052777 Praseodymium Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-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
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000001590 oxidative effect Effects 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
- 238000000926 separation method Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 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
- 239000000306 component Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 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
- 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
- 150000002500 ions Chemical class 0.000 description 1
- TXZLDPUFIHXKPH-UHFFFAOYSA-N lanthanum;octadecanoic acid Chemical compound [La].CCCCCCCCCCCCCCCCCC(O)=O TXZLDPUFIHXKPH-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 125000002524 organometallic group Chemical group 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
- 239000000843 powder Substances 0.000 description 1
- WCWKKSOQLQEJTE-UHFFFAOYSA-N praseodymium(3+) Chemical compound [Pr+3] WCWKKSOQLQEJTE-UHFFFAOYSA-N 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
- 150000003870 salicylic acids Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 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
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/683—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten
- B01J23/686—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum or tungsten with molybdenum
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
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- 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, talcum and sal soda masonry carrier, carrier is after lithium hypochlorite and double (acetylacetone,2,4-pentanedione) beryllium reamings, add octadecyl trimethyl ammonium chloride and surface 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 (3 trifluoroacetyl group D camphors) praseodymiums (III), catalytic active center component predecessor titanocenes ring substituted salicylic acid complex, L lucid asparagus amino acid molybdenums, tetrachloro gold potassium, the ammino platinum of dichloro two, hydro-thermal reaction is carried out under the effect of β hydroxyethyl dimethyls ammonium lauryl sulfate, 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
The adsorptivity of catalyst, catalytic activity auxiliary agent predecessor, normal transition Organometallic are made using Rare-earth chemicals
Compound and precious metal chemical complex are made catalytic active center predecessor and prepared with multicomponent porous carrier through hydro-thermal reaction, high temperature sintering
Ozone Heterogeneous oxidation solid catalyst containing multi-element metal has to improve the preparation method of catalyst mithridatism and catalytic activity
There are 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 by medical stone, wollastonite, potassium feldspar, boromagnesite, talcum,
Sal soda stone is constituted, by weight, medical stone:Wollastonite:Potassium feldspar:Boromagnesite:Talcum:The weight ratio of sal soda stone=（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 octadecyl 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, Lanthanum Stearate, four (DPM dpm,dipivalomethane acid) ceriums (IV), three (3- trifluoroacetyls
Base-D- camphors) praseodymium (III) Rare-earth chemicals, catalytic active center predecessor normal transition metallo-organic compound
The golden potassium of titanocenes ring substituted salicylic acid complex, L- lucid asparagus amino acid molybdenums and precious metal chemical complex tetrachloro, the ammino platinum of dichloro two,
Emulsifying agent beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate is constituted, by weight, borax:Potassium sulfate:Three (hexafluoroacetylacetones)
Yttrium (III) dihydrate:Lanthanum Stearate:Four (DPM dpm,dipivalomethane acid) ceriums (IV):Three (3- trifluoroacetyls
Base-D- camphors) praseodymium (III):Titanocenes ring substituted salicylic acid complex:L- lucid asparagus amino acid molybdenums:Tetrachloro gold potassium:Dichloro diamino
Close platinum:The weight ratio of beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate=（4~8）:（6~10）:（3~6）:（4~7）:（5
~8）:（6~9）:（10~15）:（12~18）:（4~7）:（6~9）:（6~20）.The medical stone of the B component, wollastonite,
Potassium feldspar, boromagnesite, talcum, sal soda stone 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, talcum and sal soda stone 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 (3- trifluoroacetyl group-D- camphors) praseodymium (III) C36H42F9O6Pr Rare-earth chemicals, are urged
Change 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 the golden potassium KAuCl of tetrachloro4, the ammino of dichloro two
Platinum Pt (NH3)2Cl2Precious metal chemical complex, in emulsifying agent beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate [C12H25N(CH3)2CH2CH2OH]+CH3SO4 - Effect is lower to carry out hydro-thermal reaction, and mineralizer accelerates diffusion, activates reactant lattice, promotes
The progress of solid phase reaction, it is ultrasonic surface activated carrier and Rare-earth chemicals, normal transition metallo-organic compound, expensive
Metallic compound Uniform Doped, emulsifying agent beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate makes reaction solution form quasi-stationary emulsion
Separation of solid and liquid, sedimentation are prevented, while to the further surface active of porous carrier, by anti-in certain temperature, the hydro-thermal of time
Should, drying obtains the fine silt thing of Uniform Doped；The fine silt thing of Uniform Doped is therein through high temperature sintering in Muffle furnace
Organic matter carbonization further enhances the microcellular structure of porous carrier, obtain porous carrier supported rare earth metal oxide,
The ozone Heterogeneous oxidation solid catalyst of transition metal oxide and the catalytic active center of noble metal formation, improves catalysis
The mithridatism and catalytic activity of agent.
Relative to art methods, outstanding feature of the present invention is long using medical stone, wollastonite, potassium in technology of preparing
Stone, boromagnesite, talcum, sal soda stone porous material make carrier, due to lithium hypochlorite LiClO and double (acetylacetone,2,4-pentanedione) beryllium C10H14BeO4
Reaming effect, octadecyl trimethyl ammonium chloride [C18H37N(CH3)3]+Cl-, beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate
[C12H25N(CH3)2CH2CH2OH]+CH3SO4 - To being interconnected and surface activation for duct；Rare earth is made by hydro-thermal reaction
Metallo-organic compound, normal transition metallo-organic compound and precious metal chemical complex reach Uniform Doped and are attached to carrier table
In face and duct, high temperature sintering makes organic matter carbonization strengthen and form multi-level microcellular structure, porous carrier load
The multi-element metal catalytic active center of rare-earth oxide, transition metal oxide and noble metal formation is combined with porous carrier
More firmly, the ozone Heterogeneous oxidation solid catalyst of preparation has stronger adsorptivity, the cooperative effect of multi-element metal, spy
It is not that the noble metal adulterated has stability and high activity, liquating out for metal catalytic activity component can be suppressed, improve and urge
The mithridatism and catalytic activity of agent, 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 talcums, 7.75g sal soda stones, hypochlorous acid
The weight of 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 reacting 3.2h, filtering, 103 DEG C of dry constant weights；In 500ml ultrasound reactors, input expands
Hole modified support 31g, adds the aqueous solution that 3.25g octadecyl trimethyl ammonium chlorides are dissolved in 100ml deionized waters, and this is water-soluble
The weight concentration of liquid 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；Ultrasound
After the completion of activation, the ultrasonic surface activated carrier mixed liquor in ultrasound reactor is transferred in 500ml hydrothermal reaction kettles, then
Add by 2.1g boraxs, 3.05g potassium sulfates, 1.6g tri- (hexafluoroacetylacetone) yttrium (III) dihydrate, 2.05g stearic acid
Lanthanum, 2.6g tetra- (DPM dpm,dipivalomethane acid) cerium (IV), 3.05g tri- (3- trifluoroacetyl group-D- camphors) praseodymium
(III), the golden potassium of 5.05g titanocenes ring substituted salicylic acid complex, 6.1gL- lucid asparagus amino acid molybdenum, 2.05g tetrachloros, 3.1g
The aqueous solution that the ammino platinum of dichloro two, 3.05g beta-hydroxyethyls dimethyl dodecyl base ammonium sulfate and 50ml deionized waters are prepared, the water
The weight concentration of solution 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 powder
Grain thing is in Muffle furnace, 620 DEG C, calcination 3.2h, after cooling down, can obtain the ozone Heterogeneous oxidation solid of fine particle shape
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 talcums, 2.45g sal soda stones, hypochlorous acid
The weight of lithium and double (acetylacetone,2,4-pentanedione) berylliums（0.6g）:The weight of porous material（11.7g）=1:19.5,48 DEG C are warming up to, continues to stir
Reaming modified support 11.5g is obtained after mixing reaction 5.8h, filtering, 105 DEG C of dry constant weights；In 100ml ultrasound reactors, throw
Enter reaming modified support 11.5g, add the aqueous solution that 2.2g octadecyl trimethyl ammonium chlorides are dissolved in 26ml deionized waters, should
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), (the 3- trifluoroacetyls of 0.87g tri-
Base-D- camphors) praseodymium (III), 1.48g titanocenes ring substituted salicylic acids complex, 1.77gL- lucid asparagus amino acid molybdenum, 0.68g
Tetrachloro gold potassium, the ammino platinum of 0.87g dichloros two, 1.98g beta-hydroxyethyls dimethyl dodecyl base ammonium sulfate and 10ml deionized waters are matched somebody with somebody
The aqueous solution of system, the weight concentration of the aqueous solution is 53.3%, the weight of the aqueous solution:Ultrasonic surface activated carrier mixed liquor
Weight=21.43g:39.7g =1:1.9,175 DEG C of temperature is controlled, the hydro-thermal reaction time is 15.5h, then dries carefully for 105 DEG C
Powder material；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 non-
Homogeneous oxidizing 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, talcum, sal soda stone, by weight, medical stone:Wollastonite:Potassium is long
Stone:Boromagnesite:Talcum:The weight ratio of sal soda stone=（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 octadecyl 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, Lanthanum Stearate, four (2,2,6,6- tetramethyls
Base -3,5- heptadione acid) cerium (IV), three (3- trifluoroacetyl group-D- camphors) praseodymium (III) Rare-earth chemicals, catalysis
Activated centre predecessor normal transition metallo-organic compound titanocenes ring substituted salicylic acid complex, L- lucid asparagus amino acid molybdenums
With the golden potassium of precious metal chemical complex tetrachloro, the ammino platinum of dichloro two, emulsifying agent beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate composition is 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 (3- trifluoroacetyl group-D- camphors) praseodymiums (III):Titanocenes ring substituted salicylic acid coordinates
Thing:L- lucid asparagus amino acid molybdenums:Tetrachloro gold potassium:The ammino platinum of dichloro two:The weight of beta-hydroxyethyl dimethyl dodecyl base ammonium sulfate
The ratio between=（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, talcum, sal soda stone according to claim 1, wheat
Meal stone, wollastonite, potassium feldspar, boromagnesite, talcum, sal soda stone are crushed respectively, and deionized water washing, which is dried, to be removed after moisture,
Sieved through standard screen, it is 0.0370mm~0.0750mm to control particle diameter.
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