CN107377008A - One kind carries palladium fiber base catalyst and its production and use - Google Patents
One kind carries palladium fiber base catalyst and its production and use Download PDFInfo
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- CN107377008A CN107377008A CN201710610999.5A CN201710610999A CN107377008A CN 107377008 A CN107377008 A CN 107377008A CN 201710610999 A CN201710610999 A CN 201710610999A CN 107377008 A CN107377008 A CN 107377008A
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- Prior art keywords
- palladium
- carrier
- fiber
- catalyst
- base catalyst
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000000835 fiber Substances 0.000 title claims abstract description 81
- 239000003054 catalyst Substances 0.000 title claims abstract description 53
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 123
- 239000005416 organic matter Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 31
- 239000000919 ceramic Substances 0.000 claims description 21
- 239000003365 glass fiber Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 21
- 238000006555 catalytic reaction Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 15
- 230000009467 reduction Effects 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000005554 pickling Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 238000010828 elution Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229920000914 Metallic fiber Polymers 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000012958 reprocessing Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- YTXAYGAYACWVGD-UHFFFAOYSA-N palladium;hydrate Chemical compound O.[Pd] YTXAYGAYACWVGD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002241 glass-ceramic Substances 0.000 claims description 2
- 150000002431 hydrogen Chemical group 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000000746 purification Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 6
- 238000012546 transfer Methods 0.000 abstract description 6
- 238000007493 shaping process Methods 0.000 abstract description 4
- 231100000004 severe toxicity Toxicity 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 239000002657 fibrous material Substances 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 22
- 239000012855 volatile organic compound Substances 0.000 description 17
- 239000001569 carbon dioxide Substances 0.000 description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 description 11
- 238000011156 evaluation Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 8
- 239000000523 sample Substances 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- 238000002242 deionisation method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000010970 precious metal Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 238000003915 air pollution 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
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- PBAYDYUZOSNJGU-UHFFFAOYSA-N chelidonic acid Natural products OC(=O)C1=CC(=O)C=C(C(O)=O)O1 PBAYDYUZOSNJGU-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Environmental & Geological Engineering (AREA)
- Thermal Sciences (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Catalysts (AREA)
Abstract
The invention provides one kind to carry palladium fiber base catalyst and its production and use.The load palladium fiber base catalyst of the present invention, the carrier of the catalyst is fiber, palladium of the active component for load on the carrier, is counted using the quality of the carrier as 100%, and the quality of the palladium is 0.05~2%.The present invention is used as carrier using fiber, utilize the advantages that fibrous material voidage is high, mass-transfer efficiency is high, the load palladium fiber base catalyst of burning purification benzene is prepared using it as carrier loaded active noble metals palladium, can efficient degradation severe toxicity volatile organic matter benzene, the catalyst has the advantages such as voidage is high, mass-transfer efficiency is high, shaping is easy, degraded benzene reaction temperature is low, with preferable application prospect, it is widely used in the stationary sources such as smeltery, oil plant, chemical plant and discharges the purified treatment containing benzene in waste gas.
Description
Technical field
The invention belongs to catalyst technical field, is related to a kind of load palladium fiber base catalyst and its production and use,
More particularly to a kind of load palladium fiber base catalyst of catalysis burning for volatile organic matter and preparation method thereof, more particularly to
A kind of load palladium fiber base catalyst of catalysis burning for benzene and preparation method thereof.
Background technology
With the intensity increase of human industry's activity, substantial amounts of volatile organic matter (Volatile Organic
Compound, abbreviation VOCs) it is discharged into atmospheric environment, reacted by sequence of chemical and trigger environmental pollution.For example, some are active
Strong VOCs can be with another atmosphere pollution nitrogen oxides (NOx) photochemical reaction occurs, cause surface ozone concentration liter
Height, form photochemical pollution；The VOCs that some steam force down can also be formed by complex process nucleation and growth process secondary to be had
Machine aerosol, and secondary organic aerosol is exactly fine particle PM2.5 important component.It can be seen that VOCs is to form photochemistry
Pollution and the important precursor of Brownish haze.In addition, VOCs can also form grave danger to health in itself.Example
Such as, common VOCs such as formaldehyde, benzene, toluene etc. has carcinogenic, teratogenesis harm.Therefore, photochemical fog, reduction to be removed
Grain thing pollution, improves urban air-quality, protects the health of the common people, VOCs emission controls and removal are imperative.
VOCs wide material sources, mainly include oil, chemical industry, medicine, packaging, printing, application etc., using paint industry as
Example, nearly 7,000,000 tons/year of its VOCs discharge capacity, accounts for the 1/3 of VOCs total releases.Purification neck is eliminated in paint industry VOCs
Domain, west Main Developed Countries and Japan's starting are more early.Nineteen fifty-five the U.S. just promulgated《Air Pollution Control Board preparation method》, it is right
Air pollutant emission classification and total amount have done detailed regulation, promulgate again later《Pure air method》, and in 1970 and
Nineteen ninety has done revises twice；Technicality regulation has been formulated in VOCs discharges in 1966 also exclusively for paint industry, i.e. " 66 methods
Rule ".Law obligate the promotion with company interest under, difference eliminate VOCs technologies be developed and use.
China pays much attention to VOCs pollution problem at present, it is desirable to the year two thousand twenty, realize substantially VOCs from raw material to product,
From production to the overall process emission reduction of consumption.Therefore, VOCs emission-reduction technology has obtained extensive research and probe.
Benzene is the larger one kind of volatile organic matter Poisoning,《Code for indoor environmental pollution control of civil building engineering》
Strict limitation is carried out to its concentration in GB50325-2001, it is desirable to which it is less than 0.09mg/m3.Therefore to tail of the emission source containing benzene
Gas is handled very necessary.Catalysis burning benzene is current more efficient control technology, still, conventional powder catalyst at present
The shortcomings of difficult forming and big resistance to mass tranfer be present.
The content of the invention
In view of the shortcomings of the prior art, an object of the present invention is to provide a kind of load palladium fiber base catalyst, catalysis
Activity is high, voidage is high, mass-transfer efficiency is high, shaping is easy, degraded benzene reaction temperature is low.
To use following technical scheme up to this purpose, the present invention：
One kind carries palladium fiber base catalyst, and the carrier of the catalyst is fiber, and active component is to be supported on the carrier
On palladium, counted using the quality of the carrier as 100%, the quality of the palladium is 0.05~2%.
The present invention is using fiber as carrier, using the advantages that fibrous material voidage is high, mass-transfer efficiency is high, using it as carrier
Supported active precious metal palladium prepares the load palladium fiber base catalyst of burning purification benzene, can efficient degradation severe toxicity volatile organic matter
Benzene, the catalyst have the advantages such as voidage is high, mass-transfer efficiency is high, shaping is easy, degraded benzene reaction temperature is low, had preferable
Application prospect.
Fiber of the present invention is ceramic fibre, glass fibre, metallic fiber, one kind in NACF or at least
Two kinds of mixture；The typical but unrestricted mixture of the mixture is the mixture of two kinds of fibers, such as ceramic fibre, glass
The mixture of glass fiber, ceramic fibre, the mixture of metallic fiber, ceramic fibre, the mixture of NACF, glass fibers
Dimension, the mixture of metallic fiber, glass fibre, the mixture of NACF, metallic fiber, the mixture of NACF；
The mixture can be the mixture of three kinds of fibers, such as the mixture of ceramic fibre, glass fibre, metallic fiber, ceramics
Fiber, glass fibre, the mixture of NACF, glass fibre, metallic fiber, the mixture of NACF；It is described mixed
Compound can be the mixture of four kinds of fibers, such as the mixture of ceramic fibre, glass fibre, metallic fiber, NACF.
Preferably, the fiber is the quality of the mixture of glass fibre and ceramic fibre, the glass fibre and the ceramic fibre
Than for (7~9):(1~3), such as 7:3、8:2、9:1, preferably 8:2.
In the present invention, counted using the quality of the carrier as 100%, the quality of the palladium is 0.05~2%, such as the palladium
Quality for 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%,
1.6%th, 1.7%, 1.8%, 1.9%, 2%, it is preferable that counted using the quality of the carrier as 100%, the quality of the palladium is
1%.
The second object of the present invention is to provide a kind of preparation method as described above for carrying palladium fiber base catalyst, and this is urged
Agent preparation method is simple, obtained catalyst activity is excellent, has preferable application potential, and the preparation method includes as follows
Step：
1) carrier fibre is subjected to pickling；
2) carrier fibre after step 1) pickling is placed in palladium-containing solution and impregnated, is then evaporated, drying and processing；
3) product after step 2) is dried carries out calcination process；
4) product after step 3) calcination process is subjected to high temperature reduction reprocessing, obtains carrying palladium fiber base catalyst.
The surface smoother of carrier fibre, the present invention make the surface of fiber after overpickling by pickling carrier fibre
The surface defects such as unsaturated site are formed, these unsaturated sites can combine more precious metal palladiums, be unlikely to the palladium of load
Reunion forms bulky grain together, and palladium is more uniformly carried on carrier fibre, so as to improve the activity of catalyst.The present invention's
In step 1), the process of the pickling is that carrier fibre is dipped in acid, and elution liquid is filtered dropwise in vacuum drips filter flask.
Preferably, the sour mass percent be 10~60%, such as 10%, 20%, 30%, 40%, 50%,
60%, preferably 50%.
Preferably, the acid is sulfuric acid or nitric acid, preferably sulfuric acid.
Preferably, the carrier fibre and the sour solid-to-liquid ratio are 1/100~1/10g/mL, such as the carrier fibre
It is 1/100,1/90,1/80,1/70,1/60,1/50,1/40,1/30,1/20,1/10, preferably 1/ with the sour solid-to-liquid ratio
50g/mL。
Preferably, the time of the elution is 20~40min, for example, the time of elution be 20min, 25min, 30min,
35min, 40min, preferably 30min, the number of the elution is 1~3 time.
In step 1), fiber after the pickling carries out deionized water rinsing, the pH value after the deionized water rinsing
For neutrality.
Preferably, dry step is also included after the deionized water rinsing；
Preferably, the drying is carried out in an oven, and the temperature of the drying is 100~150 DEG C, such as dry
Temperature is 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, preferably 140 DEG C, 150 DEG C, 120 DEG C.
Preferably, the time of the drying is 5~24h, for example, 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h,
15h, 16h, 17h, 18h, 19h, 20h, preferably 12h.
In step 2), the palladium-containing solution is one kind in two water palladium nitrate solutions, palladium chloride solution, palladium acetate solution.
Preferably, the dipping is ultrasonic assistant soakage, and the detailed process of the ultrasonic assistant soakage is：After pickling
Carrier fibre, which is placed in palladium-containing solution, obtains solid-liquid system, and the solid-liquid system is placed in into progress ultrasonic wave added leaching in ultrasonic wave pond
Stain, the temperature of the ultrasonic assistant soakage are room temperature, preferably 23~27 DEG C, such as 23 DEG C, 24 DEG C, 25 DEG C, 26 DEG C, 27 DEG C；
The ultrasonic frequency of the ultrasonic assistant soakage is 40~50kHz, for example, ultrasound frequency for 40kHz, 41kHz, 42kHz,
43kHz, 44kHz, 45kHz, 46kHz, 47kHz, 48kHz, 49kHz, 50kHz, preferably 44kHz, the ultrasonic assistant soakage
Time be 10~60min, such as 10min, 20min, 30min, 40min, 50min, 60min, preferably 30min.
In step 2), the evaporation process is carried out in rotary evaporation bottle, and the speed of the rotary evaporation is
20~200r/min, for example, speed be 20r/min, 30r/min, 40r/min, 50r/min, 60r/min, 70r/min,
80r/min、90r/min、100r/min、110r/min、120r/min、130r/min、140r/min、150r/min、160r/
Min, 170r/min, 180r/min, 190r/min, 200r/min, preferably 60r/min, the temperature of the rotary evaporation is 50
~70 DEG C, for example, rotary evaporation temperature for 50 DEG C, 51 DEG C, 52 DEG C, 53 DEG C, 54 DEG C, 55 DEG C, 56 DEG C, 57 DEG C, 58 DEG C, 59 DEG C,
60 DEG C, 61 DEG C, 62 DEG C, 63 DEG C, 64 DEG C, 65 DEG C, 66 DEG C, 67 DEG C, 68 DEG C, preferably 69 DEG C, 70 DEG C, 60 DEG C.
Preferably, in step 2), the drying and processing is carried out in an oven, and the temperature of the drying is 80~120
DEG C, such as the temperature of drying is 80 DEG C, 90 DEG C, 100 DEG C, preferably 110 DEG C, 120 DEG C, 100 DEG C, the time of the drying is 10
~15h, such as the time of drying is 10h, 11h, 12h, 13h, 14h, 15h, preferably 12h.
In step 3), the temperature of the calcination process is 400~600 DEG C, for example, the temperature of roasting is 400 DEG C, 410 DEG C,
420℃、430℃、440℃、450℃、460℃、470℃、480℃、490℃、500℃、510℃、520℃、530℃、540
DEG C, 550 DEG C, 560 DEG C, 570 DEG C, 580 DEG C, preferably 590 DEG C, 600 DEG C, 550 DEG C；The time of the roasting is 2~5h, such as
Roasting time is 2h, 3h, 4h, 5h, preferably 3h；The heating rate of the roasting is 2~10 DEG C/min, such as heating rate is
2℃/min、3℃/min、4℃/min、5℃/min、6℃/min、7℃/min、8℃/min、9℃/min、10℃/min。
In step 4), the process of the high temperature reduction reprocessing is：Product through step 3) calcination process is put into atmosphere
Heating reduction processing is carried out in stove.
Preferably, the atmosphere in the atmosphere furnace is reducing atmosphere, with nitrogen as Balance Air, it is preferable that the reduction
Atmosphere is hydrogen, and the volume ratio shared by the hydrogen is 1~100%, for example, hydrogen volume ratio for 1%, 10%, 20%,
30%th, 40%, 50%, 60%, 70%, 80%, 90%, 100%, preferably 5%.
Preferably, the heating rate of the heating reduction is 2~10 DEG C/min, for example, heating rate be 2 DEG C/min, 3 DEG C/
Min, 4 DEG C/min, 5 DEG C/min, 6 DEG C/min, 7 DEG C/min, 8 DEG C/min, preferably 9 DEG C/min, 10 DEG C/min, 5 DEG C/min；Institute
State heating after temperature be 200~400 DEG C, such as heating after temperature for 200 DEG C, 210 DEG C, 220 DEG C, 230 DEG C, 240 DEG C,
250℃、260℃、270℃、280℃、290℃、300℃、310℃、320℃、330℃、340℃、350℃、360℃、370
DEG C, 380 DEG C, preferably 390 DEG C, 400 DEG C, 300 DEG C；Preferably, the time of the high temperature reduction reprocessing is 2~5h, such as
Roasting time is 2h, 3h, 4h, 5h, preferably 2h.Catalyst by reduction treatment can be directly used for volatile organic matter benzene
Catalysis burning.
The third object of the present invention is to provide a kind of purposes for carrying palladium fiber base catalyst, the load palladium fiber base is urged
The catalysis that agent is used for volatile organic matter benzene is burnt.
Load palladium fiber base catalyst produced by the present invention is in thread stacking, easy forming processes, is in cotton shape after filling, phase
For powdery, pellet type catalyst its good permeability, it is easy to load, the secondary pollution such as no dust, and catalyst efficiency is high, extensively
The purified treatment containing benzene waste gas is discharged suitable for stationary sources such as smeltery, oil plant, chemical plant, is burnt through catalysis hypertoxic dirty
Dye thing benzene can all be decomposed into nontoxic carbon dioxide and water.
Compared with prior art, beneficial effects of the present invention are：
(1) load palladium fiber base catalyst of the invention is in thread stacking, good permeability, easy forming processes, no dust etc.
Secondary pollution.
(2) load palladium fiber base method for preparing catalyst of the invention is simple and easy, and obtained load palladium fiber base catalyst is wide
It is general to discharge the purified treatment containing benzene waste gas suitable for stationary sources such as smeltery, oil plant, chemical plant, through catalysis burning severe toxicity
Pollutant benzene can all be decomposed into nontoxic carbon dioxide and water.
(3) when load palladium fiber base catalyst of the invention is used for the catalysis burning of volatile organic matter benzene, there is voidage
The advantages of high, mass-transfer efficiency height, shaping are easily, degraded benzene reaction temperature is low, catalyst efficiency is high, air speed is 90L/ (gh)
When, the conversion ratio of reaction temperature benzene at 250 DEG C is with regard to that can reach more than 95%.
Brief description of the drawings
Benzene when Fig. 1 is the catalysis burning that catalyst made from embodiments of the invention 1 is used for volatile organic matter benzene is net
Change curve and yield of carbon dioxide curve synoptic diagram；
Benzene when Fig. 2 is the catalysis burning that catalyst made from embodiments of the invention 2 is used for volatile organic matter benzene is net
Change curve and yield of carbon dioxide curve synoptic diagram；
Benzene when Fig. 3 is the catalysis burning that catalyst made from embodiments of the invention 3 is used for volatile organic matter benzene is net
Change curve and yield of carbon dioxide curve synoptic diagram；
Benzene when Fig. 4 is the catalysis burning that catalyst made from embodiments of the invention 4 is used for volatile organic matter benzene is net
Change curve and yield of carbon dioxide curve synoptic diagram；
Benzene when Fig. 5 is the catalysis burning that catalyst made from embodiments of the invention 1-6 is used for volatile organic matter benzene
Conversion ratio comparison diagram；
When Fig. 6 is the catalysis burning that catalyst made from embodiments of the invention 3,7,8 is used for volatile organic matter benzene
The comparison diagram of the conversion ratio of benzene；
Fig. 7 is that the SEM of catalyst made from embodiments of the invention 3 schemes；
Fig. 8 is that the SEM of catalyst made from embodiments of the invention 4 schemes；
Fig. 9 is the N of catalyst made from embodiments of the invention 82Absorption representation figure.
Embodiment
1-9 and technical scheme is further illustrated by embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A. ceramic fibre 10g, (Fisher Chemical Triton Kaowool ceramic fiber.Code are weighed:
T/3740/48 500ml deionized waters) are once used, is filtered by Buchner funnel and eluted repeatedly, once eluted about 30 minutes, sample is taken out
It is dry standby；Two water palladium nitrate 0.25g are weighed, is put into 100ml deionized waters, stirs and evenly mixs.Above-mentioned ceramic fibre is added
Among 100ml solution.Ultrasonic assistant soakage in ultrasonic cleaning tank is inserted again.Supersonic frequency 44KHz, impregnate 1h.By above-mentioned solid-liquid
System is transferred in rotary evaporation bottle, and 60 DEG C are gradually heating to by room temperature, solvent is evaporated clean.The product after dipping is put afterwards
Enter baking oven, 100 DEG C are continued to dry 12h.Then take out, be down to room temperature, be put into Muffle furnace and be calcined, 5 DEG C of heating rate is often assigned to
500 DEG C of constant temperature 3h.Then Temperature fall, it is standby.
B. the composition of reaction mixture gas is：Benzene [C6H6]=1500ppm, [O2]=20%, N2Make Balance Air, gas always flows
Measure as 300mL/min, air speed is 90L/ (gh), 150~400 DEG C of reaction temperature.The gas concentrations such as benzene, carbon dioxide, oxygen
Determined using gas chromatograph (Agilent -7980B, FID and TCD)；
C. above-mentioned catalyst amount is 0.2g, before reaction evaluating, need to first use H2Reduction treatment.Condition is：H2=5%,
N2Make Balance Air, total gas flow rate 400mL/min, 10 DEG C every point of heating rate, keep 2h in 300 DEG C of constant temperature, be down to afterwards
Room temperature starts to warm up evaluation；Obtain benzene purification curve and yield of carbon dioxide curve is as shown in Figure 1.
Embodiment 2
Weighing parent is：Glass fibre 10g, (ACROS Organic Glass wool, Code:386062500), other
Example 1 is performed as described above in operating parameter.Obtain benzene purification curve and yield of carbon dioxide curve is as shown in Figure 2.
Embodiment 3
Ceramic fibre 10g is weighed, configures 50 (wet) %H2SO4Solution, once with 500ml deionized waters, by Buchner funnel
Suction filtration elutes repeatedly, once elutes about 30 minutes, neutrality is washed till with deionization.Sample is drained standby；Other are prepared and evaluation side
Method obtains benzene purification curve and yield of carbon dioxide curve is as shown in Figure 3 as embodiment 1.To being urged made from the present embodiment
The pattern of agent carries out electron-microscope scanning, and SEM figures are as shown in Figure 7.
Embodiment 4
Glass fibre 10g is weighed, configures 50 (wet) %H2SO4Solution, once with 500ml deionized waters, by Buchner funnel
Suction filtration elutes repeatedly, once elutes about 30 minutes, neutrality is washed till with deionization.Sample is drained standby；Other are prepared and evaluation side
Method is as embodiment 1.Obtain benzene purification curve and yield of carbon dioxide curve is as shown in Figure 4.To being urged made from the present embodiment
The pattern of agent carries out electron-microscope scanning, and SEM figures are as shown in Figure 8.
Embodiment 5
Glass fibre 10g is weighed, configures 50 (wet) %HNO3Solution, once with 500ml deionized waters, by Buchner funnel
Suction filtration elutes repeatedly, once elutes about 30 minutes, neutrality is washed till with deionization.Sample is drained standby；Other are prepared and evaluation side
For method as embodiment 1, evaluation result is as shown in Figure 5.
Embodiment 6
Ceramic fibre 10g is weighed, configures 50 (wet) %HNO3Solution, once with 500ml deionized waters, by Buchner funnel
Suction filtration elutes repeatedly, once elutes about 30 minutes, neutrality is washed till with deionization.Sample is drained standby；Other are prepared and evaluation side
For method as embodiment 1, evaluation result is as shown in Figure 6.
Embodiment 7
Weigh ceramic fibre 7g and add glass fibre 3g, configure 50 (wet) %H2SO4Solution, once with 500ml deionized waters,
Filtered by Buchner funnel and eluted repeatedly, once eluted about 30 minutes, neutrality is washed till with deionization.Sample is drained standby；Other systems
It is standby as evaluation method and embodiment 1, evaluation result is as shown in Figure 6.
Embodiment 8
Weigh ceramic fibre 8g and add glass fibre 2g, (product source) configures 50 (wet) %H2SO4Solution, once use
500ml deionized waters, filtered by Buchner funnel and eluted repeatedly, once eluted about 30 minutes, neutrality is washed till with deionization.Sample is taken out
It is dry standby；Other are prepared as evaluation method and embodiment 1, and evaluation result is as shown in fig. 6, to catalysis made from the present embodiment
Agent carries out specific surface area detection, and experimental result is as shown in Figure 9.
To sum up test, as shown in figure 5, being eluted relative to the deionized water of embodiment 1, the pickling of embodiment 3, embodiment 4
The activity of catalyst made of ceramic fibre or glass fibre is greatly improved.Relative to embodiment 5, embodiment 6
Nitric acid elutes, the sulfuric acid elution of embodiment 3, embodiment 4, it can be seen that ceramic fibre or glass fibre are made for sulfuric acid elution
Catalyst activity lifting it is optimal.Compared with the glass fibre of embodiment 4, the ceramic fibre of embodiment 3 is with respect to glass
Fiber-reactive is more excellent, but the activity of the catalyst of two kinds of fibers preparations of the mixing of embodiment 7, embodiment 8 is optimal, as shown in Figure 6.
Carrier fibre is in bar-shaped arrangement it can be seen from Fig. 7,8, and precious metal palladium is relatively evenly carried on the table of carrier fibre
Face.
As seen from Figure 9, it is 2-3m relative to the specific surface area of ceramic fibre or glass fibre2For/g, embodiment 8
The specific surface area of obtained catalyst is greatly improved, and is 87.57m2/ g, the increase of specific surface area are advantageous to catalyst
Activity.
Above example is only used for the method detailed for illustrating the present invention, the invention is not limited in above-mentioned method detailed, i.e.,
Do not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Person of ordinary skill in the field is it will be clearly understood that right
Any improvement of the present invention, addition, the selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention
Deng within the scope of all falling within protection scope of the present invention and disclosing.
Claims (10)
1. one kind carries palladium fiber base catalyst, it is characterised in that the carrier of the catalyst is fiber, and active component is to be supported on
Palladium on the carrier, counted using the quality of the carrier as 100%, the quality of the palladium is 0.05~2%.
2. load palladium fiber base catalyst according to claim 1, it is characterised in that the fiber is ceramic fibre, glass
One kind or at least two mixture in fiber, metallic fiber, NACF；
Preferably, the fiber is the mixture of glass fibre and ceramic fibre, the glass fibre and the ceramic fibre
Mass ratio is (7~9):(1~3), preferably 8:2；
Preferably, counted using the quality of the carrier as 100%, the quality of the palladium is 1%.
A kind of 3. preparation method as claimed in claim 1 or 2 for carrying palladium fiber base catalyst, it is characterised in that the preparation
Method comprises the following steps：
1) carrier fibre is subjected to pickling；
2) carrier fibre after step 1) pickling is placed in palladium-containing solution and impregnated, is then evaporated, drying and processing；
3) product after step 2) is dried carries out calcination process；
4) product after step 3) calcination process is subjected to high temperature reduction reprocessing, obtains carrying palladium fiber base catalyst.
4. preparation method according to claim 3, it is characterised in that in step 1), the process of the pickling is, by carrier
Fiber is dipped in acid, and elution liquid is filtered dropwise in vacuum drips filter flask；
Preferably, the sour mass percent is 10~60%, preferably 50%；
Preferably, the acid is sulfuric acid or nitric acid, preferably sulfuric acid；
Preferably, the carrier fibre and the sour solid-to-liquid ratio are 1/100~1/10g/mL, preferably 1/50g/mL；
Preferably, the time of the elution is 20~40min, preferably 30min, and the number of the elution is 1~3 time.
5. the preparation method according to claim 3 or 4, it is characterised in that in step 1), the fiber after the pickling enters
Row deionized water rinsing, the pH value after the deionized water rinsing are neutrality；
Preferably, dry step is also included after the deionized water rinsing；
Preferably, the drying is carried out in an oven, and the temperature of the drying is 100~150 DEG C, preferably 120 DEG C；
Preferably, the time of the drying is 5~24h, preferably 12h.
6. according to the preparation method described in one of claim 3-5, it is characterised in that in step 2), the palladium-containing solution is two
One kind in water palladium nitrate solution, palladium chloride solution, palladium acetate solution；
Preferably, the dipping is ultrasonic assistant soakage, and the detailed process of the ultrasonic assistant soakage is：By the carrier after pickling
Fiber, which is placed in palladium-containing solution, obtains solid-liquid system, and the solid-liquid system is placed in ultrasonic wave pond and carries out ultrasonic assistant soakage,
The temperature of the ultrasonic assistant soakage is 23~27 DEG C；The ultrasonic frequency of the ultrasonic assistant soakage is 40~50kHz, preferably
For 44kHz；The time of the ultrasonic assistant soakage is 10~60min, preferably 30min.
7. according to the preparation method described in one of claim 3-6, it is characterised in that in step 2), the evaporation process be
Carried out in rotary evaporation bottle, the speed of the rotary evaporation is 20~200r/min, preferably 60r/min；The rotation
The temperature for turning evaporation is 50~70 DEG C, preferably 60 DEG C；
Preferably, in step 2), the drying and processing is carried out in an oven, and the temperature of the drying is 80~120 DEG C, excellent
Elect 100 DEG C as；The time of the drying is 10~15h, preferably 12h.
8. according to the preparation method described in one of claim 3-7, it is characterised in that in step 3), the temperature of the calcination process
Spend for 400~600 DEG C, preferably 550 DEG C；The time of the roasting is 2~5h, preferably 3h；The heating rate of the roasting
For 2~10 DEG C/min.
9. according to the preparation method described in one of claim 3-8, it is characterised in that in step 4), the high temperature reduction is located again
The process of reason is：Product through step 3) calcination process is put into progress heating reduction processing in atmosphere furnace；
Preferably, the atmosphere in the atmosphere furnace is hydrogen, and the volume ratio shared by the hydrogen is 1~100%, preferably 5%；
Preferably, the heating rate of the heating reduction is 2~10 DEG C/min, preferably 5 DEG C/min, the temperature after the heating
For 200~400 DEG C, preferably 300 DEG C；Preferably, the time of the high temperature reduction reprocessing is 2~5h, preferably 2h.
10. a kind of purposes as claimed in claim 1 or 2 for carrying palladium fiber base catalyst, it is characterised in that the load palladium is fine
The catalysis that Wiki catalyst is used for volatile organic matter benzene is burnt.
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