CN106608638B - A method of preparing multi-stage porous Y type molecular sieve - Google Patents
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- 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 37
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002425 crystallisation Methods 0.000 claims abstract description 48
- 230000008025 crystallization Effects 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 20
- 239000010703 silicon Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- KXGYGLSAOVEXPN-UHFFFAOYSA-N pentane;hydrobromide Chemical class Br.CCCCC KXGYGLSAOVEXPN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910001868 water Inorganic materials 0.000 claims abstract description 12
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 3
- 230000000996 additive effect Effects 0.000 claims abstract description 3
- 230000032683 aging Effects 0.000 claims abstract description 3
- 238000011084 recovery Methods 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 235000019353 potassium silicate Nutrition 0.000 claims description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 6
- 238000003756 stirring Methods 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 229910001388 sodium aluminate Inorganic materials 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 230000000274 adsorptive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910000632 Alusil Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-O hydron;octadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCC[NH3+] REYJJPSVUYRZGE-UHFFFAOYSA-O 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- -1 polycyclic compound Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PZJJKWKADRNWSW-UHFFFAOYSA-N trimethoxysilicon Chemical compound CO[Si](OC)OC PZJJKWKADRNWSW-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
A method of preparing multi-stage porous Y type molecular sieve, it is characterised in that this method comprises: silicon source, silicon source and water, which 1) are mixed ageing, obtains crystallization director；2) first crystallization director and silicon source are mixed, then silicon source is added and water obtains reactive silicon Aluminum sol, reactive silicon Aluminum sol is obtained into crystallization liquid I in crystallization, the additive amount of the crystallization director is the 0.5~5% of the reactive silicon Aluminum sol gross mass meter；3) bis- (N- crassitude) the pentane bromides of 1,5- and crystallization liquid I are mixed to get crystallization liquid II, crystallization liquid II is in 80~105 DEG C of 10~25h of crystallization and recovery product.
Description
Technical field
The present invention relates to a kind of methods for preparing Y type molecular sieve, and further, the present invention relates to a kind of two crystallization legal systems
The method of standby multi-stage porous Y type molecular sieve.
Background technique
Y type molecular sieve (HY, REY, USY) is since the sixties in last century of use for the first time, just always catalytic cracking (FCC)
The chief active constituent element of catalyst.However, the polycyclic compound content in FCC feedstock is significant with the aggravation of crude oil heaviness
Increase, the diffusivity in zeolite cavity is but remarkably decreased.And as the Y type molecular sieve of predominant cracking constituent element as a kind of
Poromerics, aperture only have 0.74nm, and duct diffusion limitation is more serious, it is made to be highly susceptible to carbon deposit in catalysis reaction
Influence and inactivate, and many secondary responses (Cohen ER.Quantities, units and symbols easily occurs
In physical chemistry:Royal Society of Chemistry；2007).
In order to overcome the defect of general microporous molecular sieve, reducing zeolite crystal size and be introduced into molecular sieve crystal
Multi-stage porous can be effectively improved its diffusion.Compared to traditional micro porous molecular sieve, the multistage transgranular external diffusion of porous molecular sieve
It has excellent performance, shows unique catalytic activity in the catalysis reaction of macromolecular, and catalyst inactivation can be delayed, reduce coke
Yield (Perez-Ramirez J, et al.Chemical Society Reviews 2008；37:2530-42).
Hydro-thermal method is industrially to prepare the method that ultrastable generallys use at present, can be in Y type molecular sieve directly
Introducing is certain mesoporous, and still, hydro-thermal method, since silicon cannot migrate in time, fills into scarce aluminium vacancy, cause lattice in dealumination process
It collapses, non-skeleton clogged with fragments duct.The blocking in duct affects mesoporous connectivity, to affect connecing for reaction molecular
Nearly property.
A kind of novel mesopore molecular sieve is disclosed in CN1349929A, and y-type zeolite is introduced in molecular sieve hole wall
Primary and secondary structural unit makes it have the basic structure of traditional Y type molecular sieve, but its acid and hydrothermal stability improvement
Still very limited, the requirement of FCC is not achieved.
In addition there are mesoporous Y type molecular sieve is obtained with template direct synthesis technique, one is disclosed in CN103214003A
Mesoporous Y type molecular sieve of kind and preparation method thereof, it is characterised in that be prepared for y-type zeolite directed agents first, then have using amphiphilic
Machine silane N, N- dimethyl-N-[3- (trimethoxy silicon) propyl] chlorination octadecyl ammonium (TPOAC) are led as multi-stage porous template
To having synthesized mesoporous Y type molecular sieve, average pore size 3.8nm.
Summary of the invention
The object of the present invention is to provide a kind of two crystallization methods different from the prior art to prepare multi-stage porous Y type molecular sieve
Method.
A method of preparing multi-stage porous Y type molecular sieve, it is characterised in that this method comprises:
1. according to Al2O3: (1~30) SiO2: (12~30) Na2O:(200~450) H2The molar ratio of O by silicon source, silicon source and
Water mixing, then room temperature~80 DEG C at a temperature of ageing 0.2~40 hour after obtain crystallization director；
2. first mixing crystallization director and silicon source, silicon source and water is then added, obtaining molar ratio is Al2O3: (2~20)
SiO2: (1~5) Na2O:(150~400) H2The reactive silicon Aluminum sol of O, reactive silicon Aluminum sol is brilliant at 80~105 DEG C
Change 5~12h, obtain crystallization liquid I, the additive amount of the crystallization director is the reactive silicon Aluminum sol gross mass meter
0.5~5%；
3. by 1, bis- (N- crassitude) the pentane bromides of 5- are added in crystallization liquid I, in 80~105 DEG C of continuation crystallization 10~
Recovery product after 25h.
Bis- (N- crassitude) the pentane bromide additional amounts of template 1,5- are silicon source weight in crystallization liquid I
0.05-0.5, preferably 0.1-0.3；
The crystallization director preferably has Al2O3: (12~20) SiO2: (12~20) Na2O:(260~350) H2O's rubs
That ratio；
The reactive silicon Aluminum sol preferably has Al2O3: (5~10) SiO2: (1~3) Na2O:(180~300) H2O's
Molar ratio；
The silicon source can be one or more of waterglass, silica solution, silica gel, Alusil and white carbon black, wherein
Preferably waterglass, modulus are more preferable waterglass between 1.5~4, and modulus is between 2~3.
The silicon source is can be aluminum sulfate and sodium metaaluminate, wherein preferably aluminum sulfate, in more preferable control system
Na content.
The present invention with bis- (N- crassitude) the pentane bromides of 1,5- be multi-stage porous template, 1,5- bis- (N- crassitudes)
Pentane bromide shows as stronger positive charge, is easily adsorbed to the Y type molecular sieve crystallization liquid with certain ordered structure
Species surface, while its long-chain has the function of that structure directing forms multi-stage porous, forms multi-stage porous Y type molecular sieve structure.It is described
The Nitrogen adsorption isotherm of multi-stage porous Y type molecular sieve of method preparation show typical IV type feature, in 0.6-0.8P/P0
Adsorptive pressure with concentration shows pore size distribution curve, then its there are a kind of pore-size distributions at least at 7~9nm；In addition
Pore size distribution curve is serrated, and sample has the concatenated hierarchical porous structure of micropore-mesopore-macropore.
The template that the method for the present invention uses is cheap, and production cost is low, is conducive to industrialized production and application.This hair
Bright method is put forward for the first time by carrying out multi-stage porous Y type molecular sieve using bis- (N- crassitude) the pentane bromide templates of 1,5-
Synthesis, and crystallinity and the higher multi-stage porous Y type molecular sieve of purity can be synthesized.The modification Y type that the method for the present invention is prepared
Molecular sieve can be used for catalyst and catalyst carrier.The Y type molecular sieve has multi-stage porous topological structure, for the different of petroleum distillate
Structure pour point depression is hydrocracked, the process such as catalytic cracking.
Detailed description of the invention
Fig. 1 is the XRD spectra of the multi-stage porous Y type molecular sieve of the method for the present invention preparation.
Fig. 2 is low temperature nitrogen physical absorption-desorption curve of the multi-stage porous Y type molecular sieve of the method for the present invention preparation.
Fig. 3 is that the pore-size distribution of the multi-stage porous Y type molecular sieve for the method for the present invention preparation being calculated according to BJH model is bent
Line.
Specific embodiment
Below by embodiment, the invention will be further described, but content not thereby limiting the invention.
In embodiments, Sample crystals structure is determined with X-ray diffraction (XRD), the spectrogram that 2 angles θ of record are 5 to 35 °.
In embodiments, sample specific surface and pore structure parameter are obtained by low temperature nitrogen adsorption desorption measurement.
Embodiment 1
According to 1Al2O3: 15SiO2: 16Na2O:320H28.2g NaOH is added to 55ml deionized water by the molar ratio of O
In, solution is stirred to clarify, 3.0g sodium metaaluminate is added in above-mentioned solution, 35.8g waterglass (modulus is then added
2.5), room temperature continues stirring to whole dissolutions, obtains directed agents after being then aged 8 hours at 40 DEG C.
It again by above-mentioned 10g directed agents, is added in 40g waterglass (modulus 2.5), stirs 0.5 hour, it is then that 6.3g is inclined
Sodium aluminate and 18g aluminum sulfate are added in reaction system, and 28ml water is added, and continue stirring 1.5 hours after adding, finally will mixing
Object is put into the stainless steel crystallizing kettle of teflon lined, it is closed after crystallization 8 hours in 95 DEG C of baking ovens, obtain crystallization liquid I.
Bis- (N- crassitude) the pentane bromide 8g of 1,5- are added in crystallization liquid I, after continuing crystallization 22h at 100 DEG C,
Filtering, washing, filter cake roast 4h at 600 DEG C and obtain multi-stage porous Y type molecular sieve in 120 DEG C of dry 8h.
Resulting multi-stage porous Y type molecular sieve XRD spectra is shown in Fig. 1.
Fig. 2 is low temperature nitrogen physical absorption-desorption curve, the multi-stage porous Y type molecular sieve of its preparation of the preparation method
Nitrogen adsorption isotherm show typical IV type feature, in 0.6-0.8P/P0With concentration adsorptive pressure.
Fig. 3 is the pore size distribution curve being calculated according to desorption BJH model, illustrates multi-stage porous Y type molecule of the invention
Sieve is there are relatively narrow multi-stage porous pore-size distribution, and there are a kind of pore-size distributions at least at 7~9nm；In addition pore size distribution curve
It is serrated, sample has the concatenated hierarchical porous structure of micropore-mesopore-macropore.
Embodiment 2
According to 1Al2O3: 15SiO2: 16Na2O:320H28.2g NaOH is added to 55ml deionized water by the molar ratio of O
In, solution is stirred to clarify, 3.0g sodium metaaluminate is added in above-mentioned solution, 35.8g waterglass (modulus is then added
2.5), room temperature continues stirring to whole dissolutions, obtains directed agents after being then aged 20 hours at 30 DEG C.
It again by above-mentioned 10g directed agents, is added in 40g waterglass (modulus 2.5), stirs 0.5 hour, it is then that 6.3g is inclined
Sodium aluminate and 18g aluminum sulfate are added in reaction system, and 28ml water is added, and continue stirring 1.5 hours after adding, finally will mixing
Object is put into the stainless steel crystallizing kettle of teflon lined, it is closed after crystallization 10 hours in 100 DEG C of baking ovens, obtain crystallization liquid
I。
Bis- (N- crassitude) the pentane bromide 10g of 1,5- are added in crystallization liquid I, continue crystallization 18h at 100 DEG C
Afterwards, it filters, washing, filter cake roasts 3h at 700 DEG C and obtain multi-stage porous Y type molecular sieve in 100 DEG C of dry 10h.
Chromatogram characteristic with Fig. 1, Fig. 2 and Fig. 3.
Embodiment 3
According to 1Al2O3: 15SiO2: 16.5Na2O:320H29.4g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains directed agents after being then aged 5 hours at 45 DEG C.
It again by above-mentioned 10g directed agents, is added in 40g waterglass (modulus 3.3), stirs 0.5 hour, then by 25g sulphur
Sour aluminium is added in reaction system, and 28ml water is added, and continues stirring 1.5 hours after adding, mixture is finally put into polytetrafluoro
In the stainless steel crystallizing kettle of vinyl liner, it is closed after crystallization 12 hours in 95 DEG C of baking ovens, obtain crystallization liquid I.
Bis- (N- crassitude) the pentane bromide 8g of 1,5- are added in crystallization liquid I, after continuing crystallization 15h at 100 DEG C,
Filtering, washing, filter cake roast 6h at 550 DEG C and obtain multi-stage porous Y type molecular sieve in 80 DEG C of dry 11h.
Chromatogram characteristic with Fig. 1, Fig. 2 and Fig. 3.
Embodiment 4
According to 1Al2O3: 15SiO2: 16.5Na2O:320H29.4g waterglass (modulus 3.3) is added to by the molar ratio of O
In 6.9g sodium aluminate solution, stirring and dissolving obtains crystallization director after being then aged 20 hours at 30 DEG C.
It again by above-mentioned 10g directed agents, is added in 40g waterglass (modulus 3.3), stirs 0.5 hour, it is then that 6.3g is inclined
Sodium aluminate and 18g aluminum sulfate are added in reaction system, and 28ml water is added, and continue stirring 1.5 hours after adding, finally will mixing
Object is put into the stainless steel crystallizing kettle of teflon lined, it is closed after crystallization 5 hours in 95 DEG C of baking ovens, obtain crystallization liquid I.
Bis- (N- crassitude) the pentane bromide 8g of 1,5- are added in crystallization liquid I, after continuing crystallization 25h at 100 DEG C,
Filtering, washing, filter cake roast 4h at 600 DEG C and obtain multi-stage porous Y type molecular sieve in 120 DEG C of dry 8h.
Chromatogram characteristic with Fig. 1, Fig. 2 and Fig. 3.
Claims (5)
1. a kind of prepare there are a kind of method of the multi-stage porous Y type molecular sieve of pore-size distribution at least at 7~9nm, feature exists
In this method comprises:
1) according to Al2O3: (1~30) SiO2: (12~30) Na2O:(200~450) H2The molar ratio of O mixes silicon source, silicon source and water
Close, then room temperature~80 DEG C at a temperature of ageing 0.2~40 hour after obtain crystallization director；
2) first crystallization director and silicon source are mixed, silicon source and water is then added, obtaining molar ratio is Al2O3: (2~20) SiO2:
(1~5) Na2O:(150~400) H2The reactive silicon Aluminum sol of O, by reactive silicon Aluminum sol at 80~105 DEG C crystallization 5~
12h, obtains crystallization liquid I, the additive amount of the crystallization director be the reactive silicon Aluminum sol gross mass meter 0.5~
5%；
3) bis- (N- crassitude) the pentane bromides of 1,5- and crystallization liquid I are mixed to get crystallization liquid II, crystallization liquid II in 80~
105 DEG C of 10~25h of crystallization and recovery product, bis- (N- crassitude) the pentane bromide additional amounts of 1, the 5- are crystallization liquid I
The 0.05~0.5 of middle silicon source weight.
2. according to the method for claim 1 wherein the crystallization director has Al2O3: (12~20) SiO2: (12~20)
Na2O:(260~350) H2The molar ratio of O.
3. according to the method for claim 1 wherein the reactive silicon colloidal sol has Al2O3: (5~10) SiO2: (1~3)
Na2O:(180~300) H2The molar ratio of O.
4. according to the method for claim 1 wherein the silicon source is waterglass.
5. according to the method for claim 1 wherein the silicon source is aluminum sulfate.
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| EP0946416B1 (en) * | 1996-10-21 | 2002-02-20 | Institut Français du Pétrole | Im-5 zeolite, method of preparation and catalytic applications thereof |
| CN1840474A (en) * | 2005-03-31 | 2006-10-04 | 中国石油化工股份有限公司 | Process for synthesis of NaY molecular sieve |
| CN102452666A (en) * | 2010-10-21 | 2012-05-16 | 中国石油化工股份有限公司 | Method for synthesizing IM-5 molecular sieve |
| CN102616807A (en) * | 2012-03-29 | 2012-08-01 | 北京化工大学 | Method for synthesizing Y type molecular sieve |
| CN103723740A (en) * | 2012-10-12 | 2014-04-16 | 中国石油化工股份有限公司 | Synthesis method of IM-5 molecular sieve |
| CN104229822A (en) * | 2013-06-13 | 2014-12-24 | 天津神能科技有限公司 | Preparation method for small-crystal-grain Y molecular sieve with high specific surface area and high silicon-aluminium ratio |
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