CN109261196A - A kind of preparation method of the composite microporous molecular sieve catalyst of high dielectric - Google Patents
A kind of preparation method of the composite microporous molecular sieve catalyst of high dielectric Download PDFInfo
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- CN109261196A CN109261196A CN201811145950.8A CN201811145950A CN109261196A CN 109261196 A CN109261196 A CN 109261196A CN 201811145950 A CN201811145950 A CN 201811145950A CN 109261196 A CN109261196 A CN 109261196A
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- molecular sieve
- composite microporous
- sieve catalyst
- microporous molecular
- catalyst
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- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 34
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 22
- 239000006260 foam Substances 0.000 claims abstract description 20
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 20
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 229910001868 water Inorganic materials 0.000 claims abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 7
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 7
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 7
- 239000011780 sodium chloride Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims abstract description 3
- 239000012153 distilled water Substances 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 238000006555 catalytic reaction Methods 0.000 abstract description 9
- 238000000197 pyrolysis Methods 0.000 abstract description 7
- 239000002028 Biomass Substances 0.000 abstract description 6
- 239000003921 oil Substances 0.000 abstract description 3
- 239000010802 sludge Substances 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 229930195733 hydrocarbon Natural products 0.000 description 8
- 150000002430 hydrocarbons Chemical class 0.000 description 8
- 239000010453 quartz Substances 0.000 description 8
- 239000004215 Carbon black (E152) Substances 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 238000001833 catalytic reforming Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000007233 catalytic pyrolysis Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 150000003384 small molecules Chemical class 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012075 bio-oil Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000006324 decarbonylation Effects 0.000 description 1
- 238000006606 decarbonylation reaction Methods 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000005979 thermal decomposition reaction 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/035—Microporous crystalline materials not having base exchange properties, such as silica polymorphs, e.g. silicalites
-
- B01J35/30—
-
- 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
- B01J37/344—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 electromagnetic wave energy
- B01J37/346—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 electromagnetic wave energy of microwave energy
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
- C10B53/00—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form
- C10B53/02—Destructive distillation, specially adapted for particular solid raw materials or solid raw materials in special form of cellulose-containing material
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1011—Biomass
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
A kind of preparation method of the composite microporous molecular sieve catalyst of high dielectric, first calcines foam silicon carbide ceramics；Again by tetrapropylammonium hydroxide, tetraethyl orthosilicate, sodium chloride, sodium aluminate, water, uniformly mixed, stirring, standing, formation gel；Foam silicon carbide ceramics are mixed with gel, reaction kettle is packed into, is placed in microwave dissolver, microwave treatment；Then it cleans, is transferred to Muffle furnace calcining, then be placed in ammonium chloride solution, last Muffle furnace calcining obtains the composite microporous molecular sieve catalyst of high dielectric.The addition of the high composite microporous molecular sieve catalyst of dielectric of the present invention changes traditional catalyst in the heating and catalysis behavior of reaction system, effectively increases the catalytic efficiency of catalyst.The micro ware auxiliary catalysis pyrolysis of biomass, unedible oil rouge and sludge can be widely applied.
Description
Technical field
The invention belongs to catalyst fields, and in particular to a kind of preparation method of the high composite microporous molecular sieve catalyst of dielectric
And application.
Background technique
The selection of catalyst is most important in biomass microwave quick catalysis method for pyrolysis.In recent years, micropore, it is mesoporous and
Macroporous catalyst (modification derivant of ZSM-5, MCM-41, FCC, LOSA-1, SBA-15, CNT and these catalyst) is wide
General to be applied to catalytic pyrolysis reaction, result of study shows that micro porous molecular sieve and mesopore molecular sieve catalytic pyrolysis effect are preferable.Wherein
ZSM-5 molecular sieve is to be most widely used at present and effective catalyst, has good catalytic deoxidation effect, can be made just
Oxygen carrier catalytic pyrolysis in grade pyrolysis steam, forms hydro carbons, and O is then with H2O、CO、CO2Form removing.ZSM-5 points
The intersection micropore that sub- sifter device has straight hole road chord type hole road (nanoscale) two-way, primary pyrolysis steam in oxygen carrier be exactly
Catalytic deoxidation is completed by reactions such as dehydration, decarbonylation base and decarboxylations in these ducts.
Although micro porous molecular sieve is widely used in the pyrolysis of biomass microwave quick catalysis and effect is preferable, simultaneously still
There are a series of distinct issues, comprising: (1) microporous molecular sieve catalyst is easy to coking and deactivation, influences service life, burnt life
Further polymerization at mainly thermal decomposition product on molecular sieve catalyst surface, forming process are a series of selecting for deep dehydrogenations
Shaped reaction, burnt ingredient are mainly the macromolecular condensed-nuclei aromatics substance that more carbon lack hydrogen.For HZSM-5 catalyst, had
Two kinds of pore size very littles having, so its inner surface does not have burnt growth extension space, so that the coke that molecular structure is very big
It can only be generated in the outer surface of HZSM-5 catalyst.Burnt generation will lead to the blocking of catalyst duct, and limited reactions object is to catalysis
Diffusion in agent duct makes catalyst loss of catalytic activity.(2) micro porous molecular sieve aperture radius is small, and macromolecular substances have been difficult to
Effect enters, therefore micro porous molecular sieve is suitable for small-molecule substance catalytic deoxidation, causes in pyrolysis oil macromolecular substances more and holds
It is easy to aging.If macromolecular quick catalysis can be pyrolyzed as small molecule before pyrogenic steam enters micro porous molecular sieve, it is expected to reality
Now to effective upgrading of bio oil.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and applications of high composite microporous molecular sieve catalyst of dielectric.
The present invention is achieved by the following technical solutions.
A kind of preparation method of high composite microporous molecular sieve catalyst of dielectric of the present invention, as follows.
(1) foam silicon carbide ceramics are placed in Muffle furnace in 850-1000 DEG C of calcining 3-6h.
(2) following substance presses mass fraction: 2 20-30 parts of mol/L tetrapropylammonium hydroxide solution, tetraethyl orthosilicate
It 60-70 parts, 10-15 parts of sodium chloride, 0.4-0.8 parts of sodium aluminate, 900-1100 parts of water, is uniformly mixed, strong stirring 3-5 h is quiet
It sets 10-20min and forms gel.
(3) gel in calcined foam silicon carbide ceramics in step (1) and step (2) is pressed into mass fraction 1:2-1:1
Mixing is packed into ptfe autoclave, is placed in microwave dissolver, microwave power 600-900 W, controls temperature 150-170
DEG C, the reaction time is 2-4 h.
(4) it by foam silicon carbide ceramics 3-5 times wash with distilled water after reaction in step (3), is transferred to Muffle furnace and exists
5-7 h is calcined in 500-650 DEG C, is subsequently placed in 20-36h in 75-90 DEG C of 1mol/L ammonium chloride solution, is transferred to Muffle
450-600 DEG C of calcining 3-5 h of furnace, obtains the composite microporous molecular sieve catalyst of high dielectric.
A kind of high composite microporous molecular sieve catalyst of dielectric of the present invention, when biomass pyrolytic steam is by a kind of high
When the composite microporous molecular sieve catalyst of dielectric, external high dielectric property porous ceramics, external high dielectric property porous ceramics are initially entered
It quickly absorbs microwave heating in microwave field macromolecular substances micro ware auxiliary catalysis be pyrolyzed as small-molecule substance, it is subsequent all small
Molecular substance, which enters back into internal capillary molecular sieve, realizes efficient deoxidation, and gained bio oil is rich in hydro carbons and non-aging in this way.
The present invention alleviates China's energy shortage to biomass comprehensive is improved using level, has very important theoretical and realistic meaning.
The addition of the high composite microporous molecular sieve catalyst of dielectric of the present invention changes traditional catalyst in the liter of reaction system
Temperature and catalysis behavior, effectively increase the catalytic efficiency of catalyst.Biomass, unedible oil rouge and sludge can be widely applied
Micro ware auxiliary catalysis pyrolysis.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
Foam silicon carbide ceramics are placed in Muffle furnace in 900 DEG C of calcining 4h.Then 2 mol/L tetrapropyl hydrogen are accurately weighed
25 g of ammonium hydroxide solution, 65 g of tetraethyl orthosilicate, 12 g of sodium chloride, 0.5 g of sodium aluminate, 1000 g of water, 4 h of strong stirring,
It stands 15 min and forms gel；It calcined foam silicon carbide ceramics will mix, be packed by mass fraction 1:2 with gel among the above
Ptfe autoclave is placed in microwave dissolver, microwave power 800W, controls 160 DEG C of temperature, reaction time 3h；Instead
Foam silicon carbide ceramics after answering 5 times wash with distilled water, are transferred to Muffle furnace and calcine 6h in 600 DEG C, be subsequently placed in 85 DEG C
1mol/L ammonium chloride solution in 24 h, transfer to 500 DEG C of Muffle furnace 4 h of calcining, obtain the composite microporous molecular sieve of high dielectric
Catalyst.
It takes the composite microporous molecular sieve catalyst of 50g high dielectric to be loaded on quartz pipe, and is placed in microwave heating sleeve,
Adjusting microwave power control catalytic temperature is 450 DEG C.Using 100 g Chinese tallows as raw material, steam is by being filled with after microwave-heating
The quartz pipe of the high composite microporous molecular sieve catalyst of dielectric obtains 78 .3g of hydrocarbon-rich fuel oil after catalytic reforming condenses, virtue
Fragrant hydrocarbon and aromatic series oxygenates level are 80.9%.
Embodiment 2.
Foam silicon carbide ceramics are placed in Muffle furnace in 900 DEG C of calcining 4h.Then 2 mol/L tetrapropyl hydrogen are accurately weighed
25 g of ammonium hydroxide solution, 65 g of tetraethyl orthosilicate, 14 g of sodium chloride, 0.6 g of sodium aluminate, 1100 g of water, 4 h of strong stirring,
It stands 15 min and forms gel；It calcined foam silicon carbide ceramics will mix, be packed by mass fraction 1:2 with gel among the above
Ptfe autoclave is placed in microwave dissolver, microwave power 800W, controls 160 DEG C of temperature, reaction time 3h；Instead
Foam silicon carbide ceramics after answering 5 times wash with distilled water, are transferred to Muffle furnace and calcine 6h in 600 DEG C, be subsequently placed in 85 DEG C
1mol/L ammonium chloride solution in 24 h, transfer to 500 DEG C of Muffle furnace 4 h of calcining, obtain the composite microporous molecular sieve of high dielectric
Catalyst.
It takes the composite microporous molecular sieve catalyst of 50g high dielectric to be loaded on quartz pipe, and is placed in microwave heating sleeve,
Adjusting microwave power control catalytic temperature is 450 DEG C.Using 100 g stalks as raw material, steam is by being filled with height after microwave-heating
The quartz pipe of the composite microporous molecular sieve catalyst of dielectric obtains 38 .9g of hydrocarbon-rich fuel oil after catalytic reforming condenses, fragrance
Hydrocarbon and aromatic series oxygenates level are 53%.
Embodiment 3.
Foam silicon carbide ceramics are placed in Muffle furnace in 1000 DEG C of calcining 5h.Then 2 mol/L tetrapropyls are accurately weighed
30 g of Ammonia, 70 g of tetraethyl orthosilicate, 12 g of sodium chloride, 0.5 g of sodium aluminate, 1000 g of water, strong stirring 4
H stands 15 min and forms gel；It calcined foam silicon carbide ceramics will mix, fill by mass fraction 1:2 with gel among the above
Enter ptfe autoclave, be placed in microwave dissolver, microwave power 800W controls 160 DEG C of temperature, reaction time 3h；
Foam silicon carbide ceramics after reaction 5 times wash with distilled water, are transferred to Muffle furnace and calcine 6h in 600 DEG C, be subsequently placed in 85
DEG C 1mol/L ammonium chloride solution in 24 h, transfer to 500 DEG C of Muffle furnace 4 h of calcining, obtain the composite microporous molecule of high dielectric
Sieve catalyst.
It takes the composite microporous molecular sieve catalyst of 50g high dielectric to be loaded on quartz pipe, and is placed in microwave heating sleeve,
Adjusting microwave power control catalytic temperature is 450 DEG C.Using 100 g soap stocks as raw material, steam is by being filled with height after microwave-heating
The quartz pipe of the composite microporous molecular sieve catalyst of dielectric obtains hydrocarbon-rich fuel oil 67.6g, aromatic hydrocarbon after catalytic reforming condenses
It is 90.8% with aromatic series oxygenates level.
Embodiment 4.
Foam silicon carbide ceramics are placed in Muffle furnace in 1000 DEG C of calcining 5h.Then 2 mol/L tetrapropyls are accurately weighed
30 g of Ammonia, 70 g of tetraethyl orthosilicate, 12 g of sodium chloride, 0.5 g of sodium aluminate, 1000 g of water, strong stirring 4
H stands 15 min and forms gel；It calcined foam silicon carbide ceramics will mix, fill by mass fraction 1:2 with gel among the above
Enter ptfe autoclave, be placed in microwave dissolver, microwave power 800W controls 160 DEG C of temperature, reaction time 3h；
Foam silicon carbide ceramics after reaction 5 times wash with distilled water, are transferred to Muffle furnace and calcine 6h in 600 DEG C, be subsequently placed in 85
DEG C 1mol/L ammonium chloride solution in 24 h, transfer to 500 DEG C of Muffle furnace 4 h of calcining, obtain the composite microporous molecule of high dielectric
Sieve catalyst.
It takes the composite microporous molecular sieve catalyst of 50g high dielectric to be loaded on quartz pipe, and is placed in microwave heating sleeve,
Adjusting microwave power control catalytic temperature is 450 DEG C.Using the dry sludge powder of 100 g as raw material, steam passes through dress after microwave-heating
It is filled with the quartz pipe of the composite microporous molecular sieve catalyst of high dielectric, hydrocarbon-rich fuel oil 52.6g is obtained after catalytic reforming condenses,
Aromatic hydrocarbon and aromatic series oxygenates level are 60.7%.
Claims (1)
1. a kind of preparation method of the composite microporous molecular sieve catalyst of high dielectric, it is characterized in that as follows:
(1) foam silicon carbide ceramics are placed in Muffle furnace in 850-1000 DEG C of calcining 3-6h；
(2) following substance presses mass fraction: 2 20-30 parts of mol/L tetrapropylammonium hydroxide solution, tetraethyl orthosilicate 60-70
Part, it 10-15 parts of sodium chloride, 0.4-0.8 parts of sodium aluminate, 900-1100 parts of water, is uniformly mixed, strong stirring 3-5 h, stands 10-
20min forms gel；
(3) calcined foam silicon carbide ceramics in step (1) are mixed with gel in step (2) by mass fraction 1:2-1:1,
It is packed into ptfe autoclave, is placed in microwave dissolver, microwave power 600-900 W, controls 150-170 DEG C of temperature, instead
It is 2-4 h between seasonable；
(4) by foam silicon carbide ceramics 3-5 times wash with distilled water after reaction in step (3), Muffle furnace is transferred in 500-
5-7 h is calcined in 650 DEG C, is subsequently placed in 20-36h in 75-90 DEG C of 1mol/L ammonium chloride solution, is transferred to Muffle furnace
450-600 DEG C of calcining 3-5 h, obtains the composite microporous molecular sieve catalyst of high dielectric.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112495423A (en) * | 2020-11-27 | 2021-03-16 | 南昌大学 | Preparation method and application of microwave response composite catalyst |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857462A (en) * | 2009-04-07 | 2010-10-13 | 中国科学院金属研究所 | Preparation method for molecular sieve coating material on porous silicon carbide ceramic surface |
| US20110160508A1 (en) * | 2008-05-21 | 2011-06-30 | Ding Ma | Production of aromatics from methane |
| CN102716762A (en) * | 2011-06-10 | 2012-10-10 | 中国科学院金属研究所 | Ultrafine molecular sieve structured catalytic material based on porous silicon carbide carrier and preparation thereof |
| CN103252253A (en) * | 2013-05-07 | 2013-08-21 | 中国科学院金属研究所 | Porous silicon-carbide carrier surface gradient pore molecular sieve coating and preparation method thereof |
-
2018
- 2018-09-29 CN CN201811145950.8A patent/CN109261196B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110160508A1 (en) * | 2008-05-21 | 2011-06-30 | Ding Ma | Production of aromatics from methane |
| CN101857462A (en) * | 2009-04-07 | 2010-10-13 | 中国科学院金属研究所 | Preparation method for molecular sieve coating material on porous silicon carbide ceramic surface |
| CN102716762A (en) * | 2011-06-10 | 2012-10-10 | 中国科学院金属研究所 | Ultrafine molecular sieve structured catalytic material based on porous silicon carbide carrier and preparation thereof |
| CN103252253A (en) * | 2013-05-07 | 2013-08-21 | 中国科学院金属研究所 | Porous silicon-carbide carrier surface gradient pore molecular sieve coating and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ZHOU NAN ET AL: "Silicon carbide foam supported ZSM-5 composite catalyst for microwave assisted pyrolysis of biomass", 《BIORESOURCE TECHNOLOGY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112495423A (en) * | 2020-11-27 | 2021-03-16 | 南昌大学 | Preparation method and application of microwave response composite catalyst |
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