CN110314702A - A kind of preparation method of the tunica fibrosa of supported precious metal catalyst - Google Patents
A kind of preparation method of the tunica fibrosa of supported precious metal catalyst Download PDFInfo
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- CN110314702A CN110314702A CN201910598236.2A CN201910598236A CN110314702A CN 110314702 A CN110314702 A CN 110314702A CN 201910598236 A CN201910598236 A CN 201910598236A CN 110314702 A CN110314702 A CN 110314702A
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- tunica fibrosa
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- metal catalyst
- precious metal
- acetone
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- 239000003054 catalyst Substances 0.000 title claims abstract description 29
- 239000010970 precious metal Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 62
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 43
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 23
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 23
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 23
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000006166 lysate Substances 0.000 claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 238000004804 winding Methods 0.000 claims abstract description 12
- 238000004064 recycling Methods 0.000 claims abstract description 9
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000005286 illumination Methods 0.000 claims abstract description 6
- 238000009987 spinning Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 2
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 abstract description 7
- 239000011347 resin Substances 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 abstract description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 8
- 229910003445 palladium oxide Inorganic materials 0.000 description 8
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 4
- 150000002576 ketones Chemical class 0.000 description 4
- 229910052763 palladium Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- MUMZUERVLWJKNR-UHFFFAOYSA-N oxoplatinum Chemical compound [Pt]=O MUMZUERVLWJKNR-UHFFFAOYSA-N 0.000 description 2
- 229910003446 platinum oxide Inorganic materials 0.000 description 2
- 239000013464 silicone adhesive Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical compound [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- YGSFNCRAZOCNDJ-UHFFFAOYSA-N propan-2-one Chemical compound CC(C)=O.CC(C)=O YGSFNCRAZOCNDJ-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J35/59—Membranes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of the tunica fibrosa of supported precious metal catalyst, and acid chloride is added and is stirred evenly into acetone, and ethyl cellulose is then added and forms palladium-acetone soln；Low temperature is added into toluene in dimethyldichlorosilane to stir evenly, obtains silane lysate, the slow constant temperature of palladium-acetone soln is added into silane lysate, stirring to acetone removes, and obtains the first mixed liquor；Distilled water is slowly added into the first mixed liquor stirring to thick solution；Viscous solution is added to device for spinning high temperature electrostatic spinning, tunica fibrosa is obtained；Tunica fibrosa is put into ultraviolet irradiation 2-4h in illumination reaction kettle, obtains porous fiber film, winding obtains porous precious metal catalyst film after squeezing.The present invention promotes the surface area of tunica fibrosa, while the being adhered fixed property of tunica fibrosa using the large surface characteristic of tunica fibrosa and the stereoeffect of methyl silicon resin, solves nanoscale precious metal catalyst recycling problem.
Description
Technical field
The invention belongs to catalyst fields, and in particular to a kind of preparation method of the tunica fibrosa of supported precious metal catalyst.
Background technique
Nanometer science and technology obtains great development in recent years, to nano material accurately regulate and control synthesis but also we
Bigger initiative is occupied during preparing material, can tentatively realize the controlledly synthesis of the microstructure of nano material,
Realize " design " for nano material, catalyst material only when size it is small to a certain extent when could play to the maximum extent
Its catalytic action, size are also correspondingly in nanoscale.Control noble metal granule size both can effectively improve catalysis
The efficiency of agent, and the consumption of catalyst can be reduced as far as possible, meet the trend of green chemical industry.
With the development of nanocatalyst technology of preparing, method is varied.It is more commonly used be polyol reduction method and
Modify reducing agent method.However, polyol process need to flow back at high temperature restores noble metal, not only energy consumption is higher, but also can make
It is uneven at particle, and a large amount of aggregations, make average grain diameter in 20nm or more, obtained metallic catalyst activity is low, raw material
Utilization rate is low；Modification reducing agent method need to add surfactant, and surfactant is readily adsorbed in precious metal surface, it is difficult to go
It removes, covers surface-active site, influence catalytic activity.
Summary of the invention
For the problems of the prior art, the present invention provides a kind of preparation side of the tunica fibrosa of supported precious metal catalyst
Method promotes the surface area of tunica fibrosa using the large surface characteristic of tunica fibrosa and the stereoeffect of methyl silicon resin, while fine
The being adhered fixed property for tieing up film solves nanoscale precious metal catalyst recycling problem.
To realize the above technical purpose, the technical scheme is that
A kind of preparation method of the tunica fibrosa of supported precious metal catalyst, includes the following steps:
Step 1, acid chloride is added and is stirred evenly into acetone, ethyl cellulose is then added and forms palladium-acetone soln；
Step 2, low temperature is added into toluene in dimethyldichlorosilane to stir evenly, obtains silane lysate, by palladium-the third
The slow constant temperature of ketone solution is added into silane lysate, and stirring to acetone removes, and obtains the first mixed liquor；
Step 3, distilled water is slowly added into the first mixed liquor stirring to thick solution；
Step 4, viscous solution is added to device for spinning high temperature electrostatic spinning, obtains tunica fibrosa；
Step 5, tunica fibrosa is put into ultraviolet irradiation 2-4h in illumination reaction kettle, porous fiber film is obtained, after winding squeezes
Obtain porous precious metal catalyst film.
The concentration of acid chloride in acetone in the step 1 is 200-300g/L, mixing speed 300-600r/min；
The quality of ethyl cellulose is the 40-60% of acid chloride.
Concentration of the dimethyldichlorosilane in toluene in the step 2 is 100-200g/L, the matter of the acid chloride
Amount is the 20-40% of dimethyldichlorosilane, and the temperature of low temperature stirring is 2-4 DEG C, and the temperature that slow constant temperature is added is 50-60
DEG C, speed 5-9mL/min, acetone recycling is reused.
The additional amount of distilled water in the step 3 is the 30-50% of acid chloride quality, and being slowly added to speed is 2-5mL/
Min, mixing speed 500-1000r/min.
Temperature in the step 4 is 130-150 DEG C, and push distance is 3-5mm, voltage 10-20KV.
Exposure intensity in the step 5 is 5-10mW/cm2, and temperature is 100-120 DEG C, and the pressure for winding extruding is 2-
4MPa。
Step 1 dissolves acid chloride in acetone, and ethyl cellulose is then added and forms palladium-acetone soln, utilizes ethyl
The dispersibility of cellulose is able to ascend the dispersing uniformity of acid chloride in acetone, promotes distributing homogeneity, while ethyl cellulose
Element can increase the density of acetone soln, reduce the flowing velocity of acid chloride in acetone.
Low temperature stirring is added into toluene in dimethyldichlorosilane by step 2, using dimethyldichlorosilane in toluene
Dissolubility, obtain silane-toluene liquid, then palladium-acetone be added into lysate, it is stirred using the volatility of acetone
Acetone is recycled in journey, is put into step 1 and reuses；Acid chloride and ethyl cellulose are dispersed in toluene simultaneously, while second
Base cellulose adheres to the palladium ion of acid chloride, forms half mulching protective shell.
Distilled water in step 3 is slowly added in mixed liquor, and hydrolysis occurs for dimethyldichlorosilane anti-in whipping process
It answers, forms hydrolysate, while acid chloride forms hydrolysis, and not formed agglomeration under the action of ethyl cellulose because meeting water,
And solution it is whole formed under the hydrolysate effect of dimethyldichlorosilane it is thick.
Thick solution is carried out high temperature electrostatic spinning by step 4, during electrostatic spinning, forms stable fiber filament knot
Structure ultimately forms tunica fibrosa, while dimethyldichlorosilane is converted into methyl silicon resin structure, and acetic acid under temperature action
The palladium dydroxide dehydration that palladium is formed forms palladium oxide, is confined in methyl silicon resin fiber filament via ethyl cellulose.
Step 5 under ultraviolet lighting, degrade by the ethyl cellulose in tunica fibrosa, while getting off platinum oxide is exposed,
Because ethyl cellulose itself belongs to half mulching property, so platinum oxide still has good stationarity, methyl silicon resin itself
Belong to solid space structure, while ethyl cellulose degrades to form certain hole, so tunica fibrosa forms porous structure, winding
Extruding forms the porous structure of structure more closely, and uniform exposed palladium oxide in porous structure.
From the above, it can be seen that the present invention has following advantages:
1. the present invention promotes tunica fibrosa using the large surface characteristic of tunica fibrosa and the stereoeffect of methyl silicon resin
Surface area, while the being adhered fixed property of tunica fibrosa solve nanoscale precious metal catalyst recycling problem.
2. the present invention utilizes the half mulching characteristic of ethyl cellulose, influence it by silicone adhesive power, it is ensured that oxygen
The stability for changing palladium adherency, also solves the problems, such as falling off for palladium oxide.
3. the present invention is degraded the hole to be formed using ethyl cellulose, the space multistory in conjunction with methylcellulose itself is netted
Structure, the large area for forming palladium oxide is exposed, improves the catalytic effect of palladium oxide.
Specific embodiment
The specific embodiment that the present invention will be described in detail in conjunction with the embodiments, but claim of the invention is not done any
It limits.
Embodiment 1
A kind of preparation method of the tunica fibrosa of supported precious metal catalyst, includes the following steps:
Step 1, acid chloride is added and is stirred evenly into acetone, ethyl cellulose is then added and forms palladium-acetone soln；
Step 2, low temperature is added into toluene in dimethyldichlorosilane to stir evenly, obtains silane lysate, by palladium-the third
The slow constant temperature of ketone solution is added into silane lysate, and stirring to acetone removes, and obtains the first mixed liquor；
Step 3, distilled water is slowly added into the first mixed liquor stirring to thick solution；
Step 4, viscous solution is added to device for spinning high temperature electrostatic spinning, obtains tunica fibrosa；
Step 5, tunica fibrosa is put into ultraviolet irradiation 2h in illumination reaction kettle, obtains porous fiber film, winding obtains after squeezing
To porous precious metal catalyst film.
The concentration of acid chloride in acetone in the step 1 is 200g/L, mixing speed 300r/min；Ethyl cellulose
The quality of element is the 40% of acid chloride.
Concentration of the dimethyldichlorosilane in toluene in the step 2 is 100g/L, and the quality of the acid chloride is
The 20% of dimethyldichlorosilane, the temperature of low temperature stirring are 2 DEG C, and the temperature that slow constant temperature is added is 50 DEG C, speed 5mL/
Min, acetone recycling are reused.
The additional amount of distilled water in the step 3 is the 30% of acid chloride quality, and being slowly added to speed is 2mL/min,
Mixing speed is 500r/min.
Temperature in the step 4 is 130 DEG C, and push distance is 3mm, voltage 10KV.
Exposure intensity in the step 5 is 5mW/cm2, temperature is 100 DEG C, and the pressure for winding extruding is 2MPa.
Embodiment 2
A kind of preparation method of the tunica fibrosa of supported precious metal catalyst, includes the following steps:
Step 1, acid chloride is added and is stirred evenly into acetone, ethyl cellulose is then added and forms palladium-acetone soln；
Step 2, low temperature is added into toluene in dimethyldichlorosilane to stir evenly, obtains silane lysate, by palladium-the third
The slow constant temperature of ketone solution is added into silane lysate, and stirring to acetone removes, and obtains the first mixed liquor；
Step 3, distilled water is slowly added into the first mixed liquor stirring to thick solution；
Step 4, viscous solution is added to device for spinning high temperature electrostatic spinning, obtains tunica fibrosa；
Step 5, tunica fibrosa is put into ultraviolet irradiation 4h in illumination reaction kettle, obtains porous fiber film, winding obtains after squeezing
To porous precious metal catalyst film.
The concentration of acid chloride in acetone in the step 1 is 300g/L, mixing speed 600r/min；Ethyl cellulose
The quality of element is the 60% of acid chloride.
Concentration of the dimethyldichlorosilane in toluene in the step 2 is 200g/L, and the quality of the acid chloride is
The 40% of dimethyldichlorosilane, the temperature of low temperature stirring are 4 DEG C, and the temperature that slow constant temperature is added is 60 DEG C, speed 9mL/
Min, acetone recycling are reused.
The additional amount of distilled water in the step 3 is the 50% of acid chloride quality, and being slowly added to speed is 5mL/min,
Mixing speed is 1000r/min.
Temperature in the step 4 is 150 DEG C, and push distance is 5mm, voltage 20KV.
Exposure intensity in the step 5 is 10mW/cm2, temperature is 120 DEG C, and the pressure for winding extruding is 4MPa.
Embodiment 3
A kind of preparation method of the tunica fibrosa of supported precious metal catalyst, includes the following steps:
Step 1, acid chloride is added and is stirred evenly into acetone, ethyl cellulose is then added and forms palladium-acetone soln；
Step 2, low temperature is added into toluene in dimethyldichlorosilane to stir evenly, obtains silane lysate, by palladium-the third
The slow constant temperature of ketone solution is added into silane lysate, and stirring to acetone removes, and obtains the first mixed liquor；
Step 3, distilled water is slowly added into the first mixed liquor stirring to thick solution；
Step 4, viscous solution is added to device for spinning high temperature electrostatic spinning, obtains tunica fibrosa；
Step 5, tunica fibrosa is put into ultraviolet irradiation 3h in illumination reaction kettle, obtains porous fiber film, winding obtains after squeezing
To porous precious metal catalyst film.
The concentration of acid chloride in acetone in the step 1 is 250g/L, mixing speed 500r/min；Ethyl cellulose
The quality of element is the 50% of acid chloride.
Concentration of the dimethyldichlorosilane in toluene in the step 2 is 150g/L, and the quality of the acid chloride is
The 30% of dimethyldichlorosilane, the temperature of low temperature stirring are 3 DEG C, and the temperature that slow constant temperature is added is 55 DEG C, speed 7mL/
Min, acetone recycling are reused.
The additional amount of distilled water in the step 3 is the 40% of acid chloride quality, and being slowly added to speed is 4mL/min,
Mixing speed is 800r/min.
Temperature in the step 4 is 140 DEG C, and push distance is 4mm, voltage 15KV.
Exposure intensity in the step 5 is 8mW/cm2, temperature is 110 DEG C, and the pressure for winding extruding is 3MPa.
Performance detection
It is commercial powder noble metal catalyst that comparative example, which uses,
Embodiment 1-3 and comparative example are placed on using oxygen as in the solvent-free oxidation reaction of the benzyl alcohol of oxidant, specific feelings
Condition is as follows:
In conclusion the invention has the following advantages that
1. the present invention promotes tunica fibrosa using the large surface characteristic of tunica fibrosa and the stereoeffect of methyl silicon resin
Surface area, while the being adhered fixed property of tunica fibrosa solve nanoscale precious metal catalyst recycling problem.
2. the present invention utilizes the half mulching characteristic of ethyl cellulose, influence it by silicone adhesive power, it is ensured that oxygen
The stability for changing palladium adherency, also solves the problems, such as falling off for palladium oxide.
3. the present invention is degraded the hole to be formed using ethyl cellulose, the space multistory in conjunction with methylcellulose itself is netted
Structure, the large area for forming palladium oxide is exposed, improves the catalytic effect of palladium oxide.
It is understood that being merely to illustrate the present invention above with respect to specific descriptions of the invention and being not limited to this
Technical solution described in inventive embodiments.Those skilled in the art should understand that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technical effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (6)
1. a kind of preparation method of the tunica fibrosa of supported precious metal catalyst, characterized by the following steps:
Step 1, acid chloride is added and is stirred evenly into acetone, ethyl cellulose is then added and forms palladium-acetone soln；
Step 2, low temperature is added into toluene in dimethyldichlorosilane to stir evenly, obtains silane lysate, palladium-acetone is molten
The slow constant temperature of liquid is added into silane lysate, and stirring to acetone removes, and obtains the first mixed liquor；
Step 3, distilled water is slowly added into the first mixed liquor stirring to thick solution；
Step 4, viscous solution is added to device for spinning high temperature electrostatic spinning, obtains tunica fibrosa；
Step 5, tunica fibrosa is put into ultraviolet irradiation 2-4h in illumination reaction kettle, obtains porous fiber film, winding obtains after squeezing
Porous precious metal catalyst film.
2. the preparation method of the tunica fibrosa of supported precious metal catalyst according to claim 1, it is characterised in that: the step
The concentration of acid chloride in acetone in rapid 1 is 200-300g/L, mixing speed 300-600r/min；The matter of ethyl cellulose
Amount is the 40-60% of acid chloride.
3. the preparation method of the tunica fibrosa of supported precious metal catalyst according to claim 1, it is characterised in that: the step
Concentration of the dimethyldichlorosilane in toluene in rapid 2 is 100-200g/L, and the quality of the acid chloride is dimethyl dichloro
The 20-40% of silane, the temperature of low temperature stirring are 2-4 DEG C, and the temperature that slow constant temperature is added is 50-60 DEG C, speed 5-9mL/
Min, acetone recycling are reused.
4. the preparation method of the tunica fibrosa of supported precious metal catalyst according to claim 1, it is characterised in that: the step
The additional amount of distilled water in rapid 3 is the 30-50% of acid chloride quality, and being slowly added to speed is 2-5mL/min, and mixing speed is
500-1000r/min。
5. the preparation method of the tunica fibrosa of supported precious metal catalyst according to claim 1, it is characterised in that: the step
Temperature in rapid 4 is 130-150 DEG C, and push distance is 3-5mm, voltage 10-20KV.
6. the preparation method of the tunica fibrosa of supported precious metal catalyst according to claim 1, it is characterised in that: the step
Exposure intensity in rapid 5 is 5-10mW/cm2, and temperature is 100-120 DEG C, and the pressure for winding extruding is 2-4MPa.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124747A (en) * | 2019-06-26 | 2019-08-16 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of bamboo charcoal fiber composite noble metal catalyst |
| CN112675840A (en) * | 2021-01-11 | 2021-04-20 | 浙江工业大学上虞研究院有限公司 | Catalyst for nitroaniline and preparation method thereof |
| CN112675841A (en) * | 2021-01-12 | 2021-04-20 | 浙江工业大学上虞研究院有限公司 | Preparation method of composite palladium catalyst |
| CN112871155A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide based platinum oxide catalyst with shell-core structure |
| CN112934220A (en) * | 2021-02-05 | 2021-06-11 | 浙江工业大学上虞研究院有限公司 | Preparation method of hollow palladium catalyst microspheres |
| CN112958080A (en) * | 2021-02-05 | 2021-06-15 | 浙江工业大学上虞研究院有限公司 | Preparation method of mesoporous palladium catalyst |
| CN112958081A (en) * | 2021-02-05 | 2021-06-15 | 浙江工业大学上虞研究院有限公司 | Preparation method of hollow composite palladium catalyst |
| CN112973793A (en) * | 2021-03-03 | 2021-06-18 | 江门职业技术学院 | Photocatalysis nanofiber membrane and oily sewage treatment equipment used by same |
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2019
- 2019-07-04 CN CN201910598236.2A patent/CN110314702A/en not_active Withdrawn
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124747A (en) * | 2019-06-26 | 2019-08-16 | 陕西瑞科新材料股份有限公司 | A kind of preparation method of bamboo charcoal fiber composite noble metal catalyst |
| CN110124747B (en) * | 2019-06-26 | 2021-09-21 | 陕西瑞科新材料股份有限公司 | Preparation method of bamboo charcoal fiber composite noble metal catalyst |
| CN112675840A (en) * | 2021-01-11 | 2021-04-20 | 浙江工业大学上虞研究院有限公司 | Catalyst for nitroaniline and preparation method thereof |
| CN112675841A (en) * | 2021-01-12 | 2021-04-20 | 浙江工业大学上虞研究院有限公司 | Preparation method of composite palladium catalyst |
| CN112871155A (en) * | 2021-01-20 | 2021-06-01 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide based platinum oxide catalyst with shell-core structure |
| CN112871155B (en) * | 2021-01-20 | 2023-03-24 | 陕西瑞科新材料股份有限公司 | Preparation method of zirconium dioxide based platinum oxide catalyst with shell-core structure |
| CN112934220A (en) * | 2021-02-05 | 2021-06-11 | 浙江工业大学上虞研究院有限公司 | Preparation method of hollow palladium catalyst microspheres |
| CN112958080A (en) * | 2021-02-05 | 2021-06-15 | 浙江工业大学上虞研究院有限公司 | Preparation method of mesoporous palladium catalyst |
| CN112958081A (en) * | 2021-02-05 | 2021-06-15 | 浙江工业大学上虞研究院有限公司 | Preparation method of hollow composite palladium catalyst |
| CN112934220B (en) * | 2021-02-05 | 2022-10-04 | 浙江工业大学上虞研究院有限公司 | Preparation method of hollow palladium catalyst microspheres |
| CN112973793A (en) * | 2021-03-03 | 2021-06-18 | 江门职业技术学院 | Photocatalysis nanofiber membrane and oily sewage treatment equipment used by same |
| CN112973793B (en) * | 2021-03-03 | 2021-12-10 | 江门职业技术学院 | Photocatalysis nanofiber membrane and oily sewage treatment equipment used by same |
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