CN109395785A - A kind of preparation method and device of honeycomb catalyst - Google Patents
A kind of preparation method and device of honeycomb catalyst Download PDFInfo
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- CN109395785A CN109395785A CN201811127237.0A CN201811127237A CN109395785A CN 109395785 A CN109395785 A CN 109395785A CN 201811127237 A CN201811127237 A CN 201811127237A CN 109395785 A CN109395785 A CN 109395785A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 34
- 239000004088 foaming agent Substances 0.000 claims abstract description 17
- 238000005520 cutting process Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 23
- 239000003381 stabilizer Substances 0.000 claims description 18
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 239000010881 fly ash Substances 0.000 claims description 8
- 239000005416 organic matter Substances 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 7
- 239000002893 slag Substances 0.000 claims description 7
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 6
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 6
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 6
- 239000011425 bamboo Substances 0.000 claims description 6
- 239000003610 charcoal Substances 0.000 claims description 6
- -1 silicate compound Chemical class 0.000 claims description 6
- 229920001661 Chitosan Polymers 0.000 claims description 5
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 5
- 244000060011 Cocos nucifera Species 0.000 claims description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- IHBCFWWEZXPPLG-UHFFFAOYSA-N [Ca].[Zn] Chemical compound [Ca].[Zn] IHBCFWWEZXPPLG-UHFFFAOYSA-N 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 5
- 239000000920 calcium hydroxide Substances 0.000 claims description 5
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 5
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000010987 cubic zirconia Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 235000013312 flour Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000008262 pumice Substances 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 150000002085 enols Chemical class 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 229930195733 hydrocarbon Natural products 0.000 abstract description 10
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 10
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 9
- 238000004523 catalytic cracking Methods 0.000 abstract description 7
- 239000004484 Briquette Substances 0.000 abstract 1
- 238000005187 foaming Methods 0.000 abstract 1
- 239000013056 hazardous product Substances 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 239000010815 organic waste Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 19
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 16
- 239000011574 phosphorus Substances 0.000 description 16
- 229910052698 phosphorus Inorganic materials 0.000 description 16
- 235000019198 oils Nutrition 0.000 description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
- 239000004519 grease Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000002808 molecular sieve Substances 0.000 description 9
- 239000012535 impurity Substances 0.000 description 8
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 241001330002 Bambuseae Species 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000005336 cracking Methods 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 239000002737 fuel gas Substances 0.000 description 4
- 239000000295 fuel oil Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000003502 gasoline Substances 0.000 description 4
- 241001048891 Jatropha curcas Species 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil 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
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
-
- 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
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/42—Catalytic treatment
- C10G3/44—Catalytic treatment characterised by the catalyst used
-
- 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
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation method of honeycomb catalyst and device, belong to the hydrocarbon mixture catalytic cracking field for preparing New honeycomb body structure catalyst.Honeycomb catalyst is made by raw material automatic gauge, by being ground up, sieved, after thermal insulation foaming, high-temperature roasting and cutting demoulding in the present invention.The invention has the advantages that the multihole bubble structure generated using foaming agent; increase contact area, recuperability are strong, there is suction-operated to organic hazardous material in feedstock oil, be formed using organic waste structure of honeycomb briquette while; it economizes on resources, protect environment, there is higher economic benefit.
Description
Technical field
The present invention relates to grease cracking and the technical field of catalyst, specially a kind of preparation method of honeycomb catalyst
And device.
Background technique
Honeycomb ceramics for catalytic cracking is replacing existing product.Double distilled of the catalytic cracking between 200~500 DEG C
Dividing oil is raw material (including reduced pressure distillate, straight distillation light diesel oil, wax tailings etc.), and using alumino-silicate as catalyst, reaction temperature exists
Between 450~550 DEG C (different with type of reactor).Its yield big (each Large FCCU, annual cracking oil product hundred
Ten thousand tons or more), technical conditions require high (for example, the every contact of catalyst oily a few minutes will even regenerate for several seconds, flow per minute
Fluid catalyst is crossed up to 10t or more) with the raising of catalytic activity, in order to accelerate reproduction speed, it is desirable that harsher
Regeneration condition.Such as 600~650 DEG C or even 700 DEG C, catalyst consumption is big, 0.3~0.6kg of charging oil consumption per ton catalysis
Agent, catalyst mechanical strength difference, consumption it is also much greater.This requires catalyst activity, selectivity, stability slightly
It improves, will actually be of great significance to production.
And its main component catalyst distribution unevenness, easy in inactivation cause catalysis to be imitated in the honeycomb catalyst used at present
Rate reduces.The characteristics of due to stephanoporate thin wall, although considerably increasing the geometrical surface of carrier and improving thermal shock resistance,
But its pore wall strength of the product of production is low, cracky, and access times are very limited.
Summary of the invention
It is an object of the invention to overcome, the above catalyst low efficiency, easy to crack, mechanical strength is not high, organic principle
The disadvantages of unclean is discharged, a kind of preparation method of honeycomb catalyst is provided.
For achieving the above object, the present invention, which adopts the following technical solutions, is achieved: a kind of honeycomb catalyst
Preparation method is made according to the raw material of following parts by weight:
Component A: 30-40 parts of flyash, cubic zirconia 3-5 parts natural, 3-5 parts of silicon carbide, 20-25 parts of silicate compound,
10-15 parts of ground pumice, 10-15 parts of bamboo charcoal powder, 10-15 parts of coconut shell flour, 5-10 parts of calcium hydroxide, 5-10 parts of metallurgical slag and various tails
5-10 parts of slag；
B component: 5-8 parts of silane coupling agent, 5-10 parts of isopropanol, 1-2 parts of carboxymethyl chitosan, 5-10 parts of nano raw material, poly- second
3-5 parts of enol, 1-2 parts of silicon nitride, 1-2 parts of potassium permanganate, 10-15 parts of ethyl alcohol；
D component: 3-6 parts of lauryl sodium sulfate；
Foaming agent: 1-2 parts of magnesium powder, 1-2 parts of aluminium powder；
Stabilizer: 1-2 parts of calcium zinc stabilizer；
Including following steps:
Certain types of molecules is sieved addition feedstock device 1 by step 1, after the metering of self-measuring device 10, is existed with component A
It is mixed evenly in agitating device 9；
The preparation of step 2, B component: after ethanol in proper amount is added in nano raw material, with ultrasonic disperse, adding silane coupling agent, with
500r/min speed stirs 30min, after being eventually adding remaining other raw material stirring 0.5h, filtering, vacuum drying, for use；
Foaming agent, stabilizer and B component is added in step 3 in the mixture that step 1 obtains, and adds water to wash repeatedly, through 500-
It is stand-by after 600r/min mixing speed stirring 0.5-1h, it is denoted as component C；
Component C is passed through in just feeding room 2 standing purifying 12 hours by step 4；
The preparation of step 5, D component: by lauryl sodium sulfate plus water and stirring 10min, is then added in high speed frothing machine 8 and makes
Obtain foam；
D component and component C are passed through in pretreatment unit 3 and are mixed evenly and heating and moistening by step 6, dry in 100-150 DEG C
Dry 1h, humidity reach 70%, then are placed in Muffle furnace apparatus 5 in 550 DEG C of roasting 2h, remove organic matter, solidify, reach after cooling
Intensity is cut to get honeycomb catalyst idiosome；
Step 7 is demoulded from mold, and is cut into the honeycomb ceramics that size is radius 6cm, a height of 4cm.
Further, wherein component A, B component, foaming agent and stabilizer are required to be ground up, sieved in advance, and sieve mesh number exists
It is more than 40 mesh.
Further, wherein nano raw material includes ZnO, TiO2 and SiO2.
Further, modified ZSM-5 molecular sieve can be used in molecular sieve, and silane coupling agent can be used in silane coupling agent
KH570。
The above-mentioned honeycomb catalyst being prepared can be applied in the technique of grease cracking production hydro carbons, will specially take off
Water removal of impurities treated feedstock oil pump squeezes into tubular heater, and control heating temperature is 500 DEG C, obtains grease vapors and heavy oil
Mixture.The liquid that hydrocarbon ils that grease vapors are 5-18 at phosphorus content through above-mentioned honeycomb catalyst catalytic cracking, phosphorus content are 3-4
Change gas, the fuel gas that phosphorus content is 1-2, the phosphorus content is that the layered condensation of the hydrocarbon ils of 5-18 obtains gas-oil and raw gasoline.
A kind of preparation facilities of honeycomb catalyst, including feedstock device 1, self-measuring device 10, agitating device
9, go out to support room 2, high speed frothing machine device 8, pretreatment unit 3, humidifier 7, heating apparatus 6, Muffle furnace apparatus 5 and demoulding and cut
Cut device 4；The self-measuring device 10 is connect with feedstock device, for determining raw material needed for honeycomb catalyst
Amount processing；The agitating device 9 is connect with self-measuring device 10, for stirring evenly raw material；The just feeding room 2 and stirring
Device 9 connects, for standing purification process；The just feeding room 2 is connect with high speed frothing machine 8 and pretreatment unit 3, is pre-processed
Device 3 is equipped with heating apparatus 6 and humidifier 7, by the processing of obtained component heating and moistening；Muffle furnace apparatus 5 and pretreatment
Device 3 connects, and is used for high-temperature heating treatment, removes organic matter；Demoulding cutter device 4 is connect with Muffle furnace apparatus 5, and being used for will be cold
But idiosome cutting process obtains honeycomb catalyst.
Beneficial effects of the present invention:
First: catalyst surface hole count produced by the invention increases, and mechanical strength has a distinct increment, and is hardly damaged deformation, significantly
Catalytic activity is improved, and has the function of the adsorbing contaminant that normal cellular body does not have, is reused often.
Second: the carbonate foaming agent applied in the more existing industrial production of the foam performance of lauryl sodium sulfate is more preferable,
It can preferably be merged with other components.
Third: after grease cracking, compared with other catalyst, the present invention is due to there is the presence of bamboo charcoal powder, to free-fat
Acid and impurity absorption are good, greatly improve the purity of crackate and reduce pollution, increase economic efficiency indirectly, protection ring
Border.
Detailed description of the invention
Fig. 1 is the device of the invention structure chart；
Fig. 2 is process flow chart of the invention；
Each label in figure: 1- feedstock device, 2- just support room, 3- pretreatment unit, and 4- demoulds cutter device, 5- Muffle furnace dress
It sets, 6- heating apparatus, 7- humidifier, 8- high speed frothing machine, 9- agitating device, 10- self-measuring device.
Specific embodiment
It elaborates in the following with reference to the drawings and specific embodiments to the present invention.
Embodiment 1: the honeycomb catalyst in the present invention is prepared by device as shown in Figure 1, and the present apparatus includes original
Expect feeding device 1, self-measuring device 10, agitating device 9, go out to support room 2, high speed frothing machine device 8, pretreatment unit 3, humidification
Device 7, heating apparatus 6, Muffle furnace apparatus 5 and demoulding cutter device 4；The self-measuring device 10 connects with feedstock device
It connects, for doing quantitative Treatment to raw material needed for honeycomb catalyst；The agitating device 9 is connect with self-measuring device 10,
For raw material to be stirred evenly；The just feeding room 2 is connect with agitating device 9, for standing purification process；The just feeding room 2 with
High speed frothing machine 8 and pretreatment unit 3 connect, and pretreatment unit 3 is equipped with heating apparatus 6 and humidifier 7, by what is obtained
The processing of component heating and moistening；Muffle furnace apparatus 5 is connect with pretreatment unit 3, is used for high-temperature heating treatment, removes organic matter；It is de-
Die cut device 4 is connect with Muffle furnace apparatus 5, and the idiosome cutting process for will cool down obtains honeycomb catalyst, and demoulding is cut
Device 4 is cut using common automatic distributed cutting ingot stripper.
The preparation method of honeycomb catalyst of the invention is as shown in Figure 2: raw material pass through automatic gauge, by certain molecular sieve with
After the component As such as flyash are uniformly mixed stirring, it is added after adding agent aid, stabilizer, foaming agent, grinding and crosses 40 meshes, then plus
Enter suitable quantity of water stirring, with uplink at component enter pretreatment chamber, give heating and moistening processing, carry out isothermal holding；By 12
Sodium alkyl sulfate adds water and stirs, and high speed frothing machine is then added, foam is made, and sufficiently merge with the component of isothermal holding, roast
It burns, then demoulding cutting is blocking.
Embodiment 2: honeycomb ceramics catalysis is prepared by the component raw material of following weight (Kg) in the present embodiment:
Feedstock oil: the waste oil 0.5 after oily (the shortening 0.1+ palm oil 0.4) use of food and drink class.
Molecular sieve: HZSM-5 powder 0.15.
Component A: flyash 0.003, natural cubic zirconia 0.0036, silicon carbide 0.0036, silicate compound 0.02,
Ground pumice 0.01, bamboo charcoal powder 0.01, coconut shell flour 0.015, calcium hydroxide 0.0085, metallurgical slag 0.01 and various mine tailings 0.01.
B component: isopropanol 0.01, carboxymethyl chitosan 0.001, nano raw material (ZnO, TiO2, SiO2) 0.01, poly- second
Enol 0.005, silicon nitride 0.002, potassium permanganate 0.002, ethyl alcohol 0.012, silane coupling agent (KH570) 0.007.
D component: lauryl sodium sulfate 0.006.
Foaming agent: magnesium powder 0.002 and aluminium powder 0.002.
Stabilizer: calcium zinc stabilizer 0.002.
Preparation step is as follows:
Step 1, using 1mol/L NaOH solution handle HZSM-5 molecular sieve be raw material, through dispensing metering after, with fine coal
The component As such as ash are mixed evenly and are ground up, sieved.
The preparation of step 2, modified additive B component: after ethanol in proper amount is added in nano raw material (ZnO, TiO2, SiO2), with super
Sound dispersion, add silane coupling agent KH570, with 500r/min speed stir 30min, be eventually adding isopropanol, polyvinyl alcohol,
Silicon nitride, potassium permanganate, after stirring 0.5h, filtering, vacuum drying, and be ground up, sieved, for use.
Step 3 will be added foaming agent, stabilizer, B component, be ground up, sieved and stir in component A, add water to wash repeatedly, pass through
After 500-600r/min mixing speed stirring 0.5-1h and it is aged 12h, for use, is denoted as component C.
The preparation of step 4, foaming agent D component: by lauryl sodium sulfate plus water and stirring 10min, and high speed is then added
Foam is made in frothing machine.
D component and component C are mixed evenly step 5, sufficiently merge, heating and moistening, in 110 DEG C of drying 1h, humidity
Reach 75%, then be placed in 550 DEG C of roasting 2h of Muffle furnace, remove organic matter, solidified after cooling, reaches cutting intensity to get honeycomb ceramics
Catalyst idiosome.
Step 6 is demoulded from mold, and is cut into the honeycomb ceramics that size is radius 6cm, a height of 4cm.
The above finished product is used for grease cracking: using waste oil as raw material, carrying out dehydrating and removing impurities processing, is protected after being heated to 220 DEG C
Warm 30min.Dehydrating and removing impurities treated waste oil pump is squeezed into tubular heater, control heating temperature is 550 DEG C, obtains grease
Steam and heavy oil mixture.Liquefied gas that hydrocarbon ils that grease vapors are 5-18 at phosphorus content through catalytic cracking, phosphorus content are 3-4,
Phosphorus content is the fuel gas of 1-2, and the phosphorus content is that the layered condensation of the hydrocarbon ils of 5-18 obtains gas-oil and raw gasoline.
Through examining, the catalytic efficiency of the honeycomb catalyst of the present embodiment improves 33.4%, hole count 29 in unit area,
Meso-hole structure accounting improves 29.3%, and n-hexane adsorbance 12.8%, compression strength 4.3MPa, relative wear resistance is greater than 1.77.
Embodiment 3: the honeycomb catalyst in the present embodiment is prepared by the component raw material of following weight (Kg):
Feedstock oil: vegetable oil (Jatropha curcas oil) 0.5.
Molecular sieve: H β powder 0.15.
Component A: flyash 0.004, natural cubic zirconia 0.005, silicon carbide 0.0038, silicate compound 0.025,
Ground pumice 0.015, bamboo charcoal powder 0.015, coconut shell flour 0.015, calcium hydroxide 0.0085, metallurgical slag 0.0075 and various mine tailings
0.0075。
B component: isopropanol 0.008, nano raw material (ZnO, TiO2, SiO2) 0.085, gathers carboxymethyl chitosan 0.001
Vinyl alcohol 0.0045, silicon nitride 0.002, potassium permanganate 0.002, ethyl alcohol 0.012, silane coupling agent (KH570) 0.008.
D component: lauryl sodium sulfate 0.0055.
Foaming agent: magnesium powder 0.0015 and aluminium powder 0.0015.
Stabilizer: calcium zinc stabilizer 0.0015.
Preparation step is as follows:
Step 1, using 1.5mol/L NaOH solution handle H beta-molecular sieve be raw material, through dispensing metering after, with flyash
Etc. component As be mixed evenly and be ground up, sieved.
The preparation of step 2, modified additive B component: after ethanol in proper amount is added in nano raw material (ZnO, TiO2, SiO2), with super
Sound dispersion, add silane coupling agent KH570, with 500r/min speed stir 30min, be eventually adding isopropanol, polyvinyl alcohol,
Silicon nitride, potassium permanganate, after stirring 0.5h, filtering, vacuum drying, and be ground up, sieved, for use.
Step 3 will be added foaming agent, stabilizer, B component, be ground up, sieved and stir in component A, add water to wash repeatedly, pass through
After 500-600r/min mixing speed stirring 0.5-1h and it is aged 12h, for use, is denoted as component C.
The preparation of step 4, foaming agent D component: by lauryl sodium sulfate plus water and stirring 10min, and high speed is then added
Foam is made in frothing machine.
D component and component C are mixed evenly step 5, sufficiently merge, heating and moistening, in 110 DEG C of drying 1h, humidity
Reach 80%, then be placed in 550 DEG C of roasting 2.5h of Muffle furnace, remove organic matter, solidified after cooling, reaches cutting intensity to get honeycomb
Body catalyst idiosome.
Step 6 is demoulded from mold, and is cut into the honeycomb ceramics that size is radius 6.7cm, a height of 4.4cm.
The application of above-mentioned finished product: using Jatropha curcas oil as raw material, dehydrating and removing impurities processing is carried out, is kept the temperature after being heated to 180 DEG C
30min.Dehydrating and removing impurities treated Jatropha curcas oil pump is squeezed into tubular heater, control heating temperature is 550 DEG C, obtains oil
Rouge steam and heavy oil mixture.The liquefaction that hydrocarbon ils that grease vapors are 5-18 at phosphorus content through catalytic cracking, phosphorus content are 3-4
Gas, the fuel gas that phosphorus content is 1-2, the phosphorus content are that the layered condensation of the hydrocarbon ils of 5-18 obtains gas-oil and raw gasoline.
Through examining, the catalytic efficiency of the honeycomb catalyst of the present embodiment improves 27.3%, hole count 32 in unit area,
Meso-hole structure accounting improves 27.9%, and n-hexane adsorbance 10.8%, compression strength .3.9MPa, relative wear resistance is greater than 1.75.
Embodiment 4: the preparation method of the present embodiment honeycomb catalyst, by the component raw material preparation of following weight (Kg)
At:
Feedstock oil: animal oil (discarded lard) 0.5.
Molecular sieve: HY powder 0.15.
Component A: flyash 0.0035, natural cubic zirconia 0.004, silicon carbide 0.004, silicate compound 0.023,
Ground pumice 0.01, bamboo charcoal powder 0.01, coconut shell flour 0.015, calcium hydroxide 0.0085, metallurgical slag 0.01 and various mine tailings 0.01.
B component: isopropanol 0.0075, nano raw material (ZnO, TiO2, SiO2) 0.01, gathers carboxymethyl chitosan 0.0015
Vinyl alcohol 0.005, silicon nitride 0.002, potassium permanganate 0.0015, ethyl alcohol 0.012, silane coupling agent (KH570) 0.0065.
D component: lauryl sodium sulfate 0.0045.
Foaming agent: magnesium powder 0.0018 and aluminium powder 0.0018.
Stabilizer: calcium zinc stabilizer 0.0018.
Preparation step is as follows:
Step 1, using 0.5mol/L NaOH solution handle HY molecular sieve be raw material, through dispensing metering after, with flyash
Etc. component As be mixed evenly and be ground up, sieved.
The preparation of step 2, modified additive B component: after ethanol in proper amount is added in nano raw material (ZnO, TiO2, SiO2), with super
Sound dispersion, add silane coupling agent KH570, with 500r/min speed stir 30min, be eventually adding isopropanol, polyvinyl alcohol,
Silicon nitride, potassium permanganate, after stirring 0.5h, filtering, vacuum drying, and be ground up, sieved, for use.
Step 3 will be added foaming agent, stabilizer, B component, be ground up, sieved and stir in component A, add water to wash repeatedly, pass through
After 500-600r/min mixing speed stirring 0.5-1h and it is aged 12h, for use, is denoted as component C.
The preparation of step 4, foaming agent D component: by lauryl sodium sulfate plus water and stirring 10min, and high speed is then added
Foam is made in frothing machine.
D component and component C are mixed evenly step 5, sufficiently merge, heating and moistening, in 110 DEG C of drying 1h, humidity
Reach 70%, then be placed in 550 DEG C of roasting 2.5h of Muffle furnace, remove organic matter, solidified after cooling, reaches cutting intensity to get honeycomb
Body catalyst idiosome.
Step 6 is demoulded from mold, and is cut into the honeycomb ceramics that size is radius 6.3cm, a height of 4.2cm.
The application of this finished product: using discarded lard as raw material, dehydrating and removing impurities processing is carried out, is kept the temperature after being heated to 280 DEG C
30min.By dehydrating and removing impurities, treated that discarded lard pump squeezes into tubular heater, and control heating temperature is 550 DEG C, obtains oil
Rouge steam and heavy oil mixture.The liquefaction that hydrocarbon ils that grease vapors are 5-18 at phosphorus content through catalytic cracking, phosphorus content are 3-4
Gas, the fuel gas that phosphorus content is 1-2, the phosphorus content are that the layered condensation of the hydrocarbon ils of 5-18 obtains gas-oil and raw gasoline.
Through examining, the catalytic efficiency of the honeycomb catalyst of the present embodiment improves 32.4%, hole count 28 in unit area,
Meso-hole structure accounting improves 19.3%, and n-hexane adsorbance 17.8%, compression strength 4.7MPa, relative wear resistance is greater than 1.79.
Specific embodiments of the present invention are explained in detail above in conjunction with attached drawing, but the present invention is not limited to above-mentioned realities
Example is applied, it within the knowledge of a person skilled in the art, can also be without departing from the purpose of the present invention
Various changes can be made.
Claims (4)
1. a kind of preparation method of honeycomb catalyst, it is characterised in that: be made according to the raw material of following parts by weight:
Component A: 30-40 parts of flyash, cubic zirconia 3-5 parts natural, 3-5 parts of silicon carbide, 20-25 parts of silicate compound,
10-15 parts of ground pumice, 10-15 parts of bamboo charcoal powder, 10-15 parts of coconut shell flour, 5-10 parts of calcium hydroxide, 5-10 parts of metallurgical slag and various tails
5-10 parts of slag；
B component: 5-8 parts of silane coupling agent, 5-10 parts of isopropanol, 1-2 parts of carboxymethyl chitosan, 5-10 parts of nano raw material, poly- second
3-5 parts of enol, 1-2 parts of silicon nitride, 1-2 parts of potassium permanganate, 10-15 parts of ethyl alcohol；
D component: 3-6 parts of lauryl sodium sulfate；
Foaming agent: 1-2 parts of magnesium powder, 1-2 parts of aluminium powder；
Stabilizer: 1-2 parts of calcium zinc stabilizer；
Including following steps:
Certain types of molecules is sieved addition feedstock device (1) by step 1, after self-measuring device (10) metering, with A group
Divide and is mixed evenly in agitating device (9)；
The preparation of step 2, B component: after ethanol in proper amount is added in nano raw material, with ultrasonic disperse, adding silane coupling agent, with
500r/min speed stirs 30min, after being eventually adding remaining other raw material stirring 0.5h, filtering, vacuum drying, for use；
Foaming agent, stabilizer and B component is added in step 3 in the mixture that step 1 obtains, and adds water to wash repeatedly, through 500-
It is stand-by after 600r/min mixing speed stirring 0.5-1h, it is denoted as component C；
Component C is passed through standing purifying 12 hours in just feeding room (2) by step 4；
The preparation of step 5, D component: by lauryl sodium sulfate plus water and stirring 10min, is then added in high speed frothing machine (8)
Foam is made；
D component and component C are passed through in pretreatment unit (3) and are mixed evenly and heating and moistening by step 6, in 100-150 DEG C
1h is dried, humidity reaches 70%, then is placed in Muffle furnace apparatus (5) in 550 DEG C of roasting 2h, and organic matter is removed, is solidified after cooling,
Reach cutting intensity to get honeycomb catalyst idiosome；
Step 7 is demoulded from mold, and is cut into the honeycomb ceramics that size is radius 6cm, a height of 4cm.
2. the preparation method of honeycomb catalyst according to claim 1, it is characterised in that: the component A, B component, hair
Gas agent and stabilizer are required to be ground up, sieved in advance, and sieve mesh number is more than 40 mesh.
3. the preparation method of honeycomb catalyst according to claim 1, it is characterised in that: the nano raw material includes
ZnO、TiO2And SiO2。
4. a kind of preparation facilities of honeycomb catalyst, it is characterised in that: including feedstock device (1), self-measuring device
(10), agitating device (9), out feeding room (2), high speed frothing machine device (8), pretreatment unit (3), humidifier (7), heating dress
Set (6), Muffle furnace apparatus (5) and demoulding cutter device (4)；The self-measuring device (10) connect with feedstock device,
For doing quantitative Treatment to raw material needed for honeycomb catalyst；The agitating device (9) connect with self-measuring device (10),
For raw material to be stirred evenly；Just feeding room (2) are connect with agitating device (9), for standing purification process；The just feeding room
(2) it is connect with high speed frothing machine (8) and pretreatment unit (3), pretreatment unit (3) is equipped with heating apparatus (6) and humidifies
Device (7), by the processing of obtained component heating and moistening；Muffle furnace apparatus (5) is connect with pretreatment unit (3), for high temperature plus
Heat treatment removes organic matter；Demoulding cutter device (4) is connect with Muffle furnace apparatus (5), the idiosome cutting process for will cool down
Obtain honeycomb catalyst.
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| CN112755955A (en) * | 2020-12-24 | 2021-05-07 | 赣南师范大学 | Preparation method of light honeycomb molecular sieve purification module |
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