CN102442678A - Preparation method of NU-85 molecular sieve - Google Patents
Preparation method of NU-85 molecular sieve Download PDFInfo
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- CN102442678A CN102442678A CN2010105092001A CN201010509200A CN102442678A CN 102442678 A CN102442678 A CN 102442678A CN 2010105092001 A CN2010105092001 A CN 2010105092001A CN 201010509200 A CN201010509200 A CN 201010509200A CN 102442678 A CN102442678 A CN 102442678A
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- crystallization
- molecular sieve
- sio
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- sodium
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Links
- 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 73
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000002425 crystallisation Methods 0.000 claims abstract description 58
- 230000008025 crystallization Effects 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010703 silicon Substances 0.000 claims abstract description 22
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 6
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 28
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 17
- 239000004411 aluminium Substances 0.000 claims description 9
- 230000031709 bromination Effects 0.000 claims description 5
- 238000005893 bromination reaction Methods 0.000 claims description 5
- 229950000405 decamethonium Drugs 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- HLXQFVXURMXRPU-UHFFFAOYSA-L trimethyl-[10-(trimethylazaniumyl)decyl]azanium;dibromide Chemical compound [Br-].[Br-].C[N+](C)(C)CCCCCCCCCC[N+](C)(C)C HLXQFVXURMXRPU-UHFFFAOYSA-L 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- 159000000000 sodium salts Chemical class 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- 159000000013 aluminium salts Chemical class 0.000 claims description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- COLRBPHEBSHUAG-UHFFFAOYSA-L disodium bromide chloride Chemical group [Na+].[Na+].[Cl-].[Br-] COLRBPHEBSHUAG-UHFFFAOYSA-L 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 229960004249 sodium acetate Drugs 0.000 claims description 2
- 235000017281 sodium acetate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 229940001516 sodium nitrate Drugs 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims description 2
- 229940039790 sodium oxalate Drugs 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 230000003068 static effect Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000011027 product recovery Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 10
- 229910021536 Zeolite Inorganic materials 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 9
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 239000010457 zeolite Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 241001185310 Symbiotes <prokaryote> Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 238000006317 isomerization reaction Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000002152 alkylating effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a preparation method of a NU-85 molecular sieve, which comprises a crystallization material preparation process, a crystallization process and a crystallization product recovery treatment process, wherein the crystallization material preparation process is to mix an aluminum source, a silicon source, alkali, a template agent, inorganic salt, an EU-1 molecular sieve and water, and the EU-1 molecular sieve added in the crystallization material and SiO contained in the silicon source2The mass ratio of to (B) is 2.5 to 8.5. Compared with the prior art, the method can effectively shorten the crystallization time of the NU-85 molecular sieve and improve the production efficiency.
Description
Technical field
The present invention relates to a kind of preparation method of NU-85 molecular sieve.
Background technology
The NU-85 molecular sieve is a kind of supersiliceous zeolite molecular sieve of two-dimentional microvoid structure.Be the symbiote of EU-1 molecular sieve and NU-87 molecular sieve, EU-1 molecular sieve structure band links to each other with NU-87 molecular sieve structure band is staggered in its crystalline structure, in conjunction with tight.This structures shape of NU-85 molecular sieve it have the duct characteristic and the catalysis characteristics of two kinds of parent molecules sieve, this also makes it be widely used in the isomerization reaction and alkylated reaction of hydrocarbon polymer as catalyzer.
U.S. Pat 5385718 has proposed NU-85 molecular sieve and preparation method thereof the earliest with US6784334.Template used dose is C6 (HexBr
2), hydrothermal crystallizing is synthetic.Concrete compound method is following: aluminium source, alkali and inorganic salt are dissolved in process solution A in the portion water, template is dissolved in processes solution B in the portion water, the silicon source is dissolved in the water processes solution C; At first solution B is joined in the solution A, stir, then solution C is joined in the solution A, stir.Each molar ratio of material that adds is SiO
2/ Al
2O
3=25～40, Na
2O/SiO
2=0.025～0.5, R/SiO
2=0.02～1, H
2O/SiO
2=5～250, NaL/SiO
2=0～1, wherein R is the template C6, and NaL is a sodium salt.Crystallization temperature is 120～180 ℃, and crystallization time is more than 10 days.Can add crystal seed and shorten crystallization time, it can be NU-85 molecular sieve, NU-87 molecular sieve, EU-1 molecular sieve that institute adds crystal seed.Contained EU-1 molecular sieve is different with NU-87 molecular sieve ratio in the NU-85 molecular sieve that synthesizes under the different synthesis conditions.Temperature is very big to the synthetic influence of NU-85 molecular sieve, and when Tc was 200 ℃, the product that synthesizes was the EU-1 molecular sieve; When Tc was 180 ℃, what preferentially generate was the EU-1 molecular sieve, but product has shown the characteristic of NU-85 molecular sieve; When Tc was 160 ℃, the product that synthesizes was the NU-85 molecular sieve.Along with the reduction of Tc, product can be become the symbiote NU-85 molecular sieve of EU-1 molecular sieve and NU-87 molecular sieve by pure EU-1 molecular sieve.But temperature reduces, and crystallization time prolongs thereupon.So the crystallization time of General N U-85 molecular sieve is more than 18 days.
Summary of the invention
To the deficiency of prior art, the present invention provides a kind of NU-85 molecular sieve and preparation method thereof, and this method can effectively shorten the crystallization time of NU-85 molecular sieve.
The preparation method of NU-85 molecular sieve of the present invention; Comprise crystallization material process for preparation, crystallization process and crystallization product recycling process; Described crystallization material process for preparation is that aluminium source, silicon source, alkali, template, inorganic salt, EU-1 molecular sieve and water are mixed, contained SiO in EU-1 molecular sieve that adds in the crystallization material and the silicon source
2Mass ratio be 2.5～8.5, the composition of the aluminium source in the crystallization material, silicon source, alkali, template, inorganic salt and water by the mol ratio of oxide compound or salt is:
SiO
2/Al
2O
3＝45～65；
R/SiO
2＝0.1～0.22；
Na
2O/SiO
2＝0.1～0.2；
H
2O/SiO
2＝42～55；
NaL/SiO
2＝0.059～0.098；
R is a template bromination decamethonium, and NaL is a sodium salt, can be sodium-chlor, Sodium Bromide, SODIUMNITRATE, sodium-acetate, sodium oxalate, is preferably sodium-chlor.
Described aluminium source can be preferably sodium aluminate for one or more the mixture in aluminium salt, aluminate, aluminum oxide, white lake or the aluminium colloidal sol; Said silicon source can be preferably silicon sol for white carbon black, silicon sol, water glass or tetraethoxy etc.
Described EU-1 molecular sieve, its silica alumina ratio (SiO
2/ Al
2O
3Mol ratio) be 20～35.The EU-1 molecular sieve can be through roasting, also can be unfired, preferably passes through the EU-1 molecular sieve of roasting.
Described crystallization process crystallization temperature is 160～200 ℃, and crystallization time is 1～10 day, and crystallization pressure is the autogenous pressure under the crystallization temperature.Crystallization process can adopt static crystallization, also can adopt dynamic crystallization, the preferred latter.Dynamic crystallization generally adopts the mode of stirring to carry out, stirring velocity be generally 150～800rpm (rev/min).The dynamic crystallization temperature is preferably 160～190 ℃ of following crystallization 3～8 days.
The NU-85 molecular sieve of the inventive method preparation can be applied to field of petrochemical industry, is a kind of good catalytic material, and it is at alkylating aromatic hydrocarbon, and aspects such as aromatics isomerization and methane aromatizing and alkane hydroisomerizing all have good catalytic performance.
The inventive method has been used the EU-1 molecular sieve in crystallization material process for preparation.The EU-1 molecular sieve is structurally extremely similar with the NU-85 molecular sieve a kind of molecular sieve, and it also possesses the characteristics of nanocrystal simultaneously.The inventive method is fully used the characteristics of the nanocrystal of EU-1 type molecular sieve; Make it in crystallization material process for preparation, decompose, form the secondary structure unit of a large amount of EUO type molecular sieves; And these structural units also are the structural units of NU-85 molecular sieve; With these secondary structure units is directed agents, and sial in the crystallization material and bromination decamethonium are incorporated in the skeleton of NU-85 molecular sieve.The inventive method has effectively shortened the crystallization time of NU-85 molecular sieve, has reduced preparation cost, has improved production efficiency.Though the bromination decamethonium is not the conventional template agent of synthetic NU-85 molecular sieve, in the synthetic material system of the inventive method, effectively promoted the synthetic of NU-85 molecular sieve, obtained beyond thought technique effect.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) spectrogram of the molecular sieve of the embodiment of the invention 1 preparation.
Fig. 2 is the ESEM picture of the molecular sieve of the embodiment of the invention 1 preparation.
Embodiment
Further specify the present invention program and effect below by embodiment.
Embodiment 1
Configuration solution 1: with 2.61gNaAlO
2, 4.37gNaOH, 2.57gNaCl, 31.37gDecBr
2(bromination decamethonium) joins 300mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol (is contained SiO
245g, down with) join 267mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 125gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 160 ℃, 8 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 150rpm, and the XRD spectra of product and ESEM picture are seen Fig. 1 and Fig. 2.
Embodiment 2
Configuration solution 1: with 3.73gNaAlO
2, 6.48gNaOH, 4.30gNaCl, 69.01gDecBr
2Join 350mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 250mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 375gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 190 ℃, 3 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 800rpm.
Embodiment 3
Configuration solution 1: with 2.98gNaAlO
2, 8.96gNaOH, 3.38gNaCl, 45.76gDecBr
2Join 400mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 342mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 268gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 180 ℃, 6 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 250rpm.
Embodiment 4
Configuration solution 1: with 3.25gNaAlO
2, 9.23gNaOH, 2.84gNaCl, 34.89gDecBr
2Join 350mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 250mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 312gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 175 ℃, 7 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 300rpm.
Embodiment 5
Configuration solution 1: with 3.77gNaAlO
2, 9.65gNaOH, 3.32gNaCl, 36.54gDecBr
2Join 350mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 280mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 345gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 180 ℃, 6 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 210rpm.
Embodiment 6
Configuration solution 1: with 2.89gNaAlO
2, 8.36gNaOH, 3.82gNaCl, 55.65gDecBr
2Join 400mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 250mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 335gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 180 ℃, 5 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 250rpm.
Embodiment 7
Configuration solution 1: with 2.88gNaAlO
2, 7.63gNaOH, 3.38gNaCl, 47.32gDecBr
2Join 350mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 250mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 364gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 180 ℃, 7 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 200rpm.
Embodiment 8
Configuration solution 1: with 3.53gNaAlO
2, 9.43gNaOH, 3.94gNaCl, 60.58gDecBr
2Join 400mlH
2Among the O, under whipped state, mix.
Configuration solution 2: the 125ml silicon sol is joined 340mlH
2Among the O, under whipped state, mix.
Solution 2 is joined in the solution 1, under whipped state, mix, and add the 364gEU-1 molecular sieve, process gel as crystal seed.
The gained gel is packed in the 1L synthesis reactor, and in 185 ℃, 4 days postcooling of crystallization through filtration, washing, dry zeolite product, are NU-85 molecular sieve through the crystalline phase analysed preparation to room temperature under the 250rpm.
Claims (7)
1. the preparation method of a NU-85 molecular sieve; Comprise crystallization material process for preparation, crystallization process and crystallization product recycling process; It is characterized in that: crystallization material process for preparation is that aluminium source, silicon source, alkali, template, inorganic salt, EU-1 molecular sieve and water are mixed, contained SiO in EU-1 molecular sieve that adds in the crystallization material and the silicon source
2Mass ratio be 2.5～8.5, the composition of the aluminium source in the crystallization material, silicon source, alkali, template, inorganic salt and water by the mol ratio of oxide compound or salt is:
SiO
2/Al
2O
3＝45～65；
R/SiO
2＝0.1～0.22；
Na
2O/SiO
2＝0.1～0.2；
H
2O/SiO
2＝42～55；
NaL/SiO
2＝0.059～0.098；
R is a template bromination decamethonium, and NaL is a sodium salt.
2. according to the described method of claim 1, it is characterized in that: sodium salt is sodium-chlor, Sodium Bromide, SODIUMNITRATE, sodium-acetate or sodium oxalate.
3. according to the described method of claim 1, it is characterized in that: the aluminium source is one or more the mixture in aluminium salt, aluminate, aluminum oxide, white lake or the aluminium colloidal sol; The silicon source is white carbon black, silicon sol, water glass or tetraethoxy.
4. according to the described method of claim 1, it is characterized in that: the SiO of EU-1 molecular sieve
2/ Al
2O
3Mol ratio is 20～35.
5. according to the described method of claim 1, it is characterized in that: the crystallization temperature of crystallization process is 160～200 ℃, and crystallization time is 1～10 day, and crystallization pressure is the autogenous pressure under the crystallization temperature.
6. according to claim 1 or 5 described methods, it is characterized in that: crystallization process adopts static crystallization, perhaps adopts dynamic crystallization.
7. according to the described method of claim 6, it is characterized in that: the mode that dynamic crystallization adopt to stir is carried out, and the dynamic crystallization temperature was 160～190 ℃ of following crystallization 3～8 days.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496643A (en) * | 2019-09-03 | 2019-11-26 | 太原大成环能化工技术有限公司 | A kind of isomerization of C-8 aromatics catalyst crystal seed assistant preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058195A (en) * | 1990-06-21 | 1992-01-29 | 帝国化学工业公司 | Zeolite |
-
2010
- 2010-10-13 CN CN 201010509200 patent/CN102442678B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058195A (en) * | 1990-06-21 | 1992-01-29 | 帝国化学工业公司 | Zeolite |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110496643A (en) * | 2019-09-03 | 2019-11-26 | 太原大成环能化工技术有限公司 | A kind of isomerization of C-8 aromatics catalyst crystal seed assistant preparation method |
| CN110496643B (en) * | 2019-09-03 | 2022-04-12 | 太原大成环能化工技术有限公司 | Auxiliary preparation method of carbon octa-arene isomerization catalyst seed crystal |
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