CN105271293A - Synthetic method of high-silicon zeolite - Google Patents
Synthetic method of high-silicon zeolite Download PDFInfo
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Abstract
The invention belongs to the technical field of microporous materials and particularly relates to a synthetic method of high-silicon zeolite. According to the synthetic method, glass powder is taken as a silicon source, crystalline-state aluminosilicate (zeolite), AlPO or SAPO (silicoaluminophosphate) molecular sieve, or a natural mineral molecular sieve crystal is taken as a seed crystal, alkylamine is taken as a structure-directing agent, accordingly, a reaction mixture is formed, and high-silicon MRE (ZSM-48), MFI (ZSM-5) and MTN (ZSM-39) zeolite molecular sieves are synthesized through a hydrothermal reaction under the guiding action of out-phase crystal nucleus. By means of the method, the synthetic reaction time can be shortened, generation of mixed crystal phases is avoided, the product purity is improved, and crystal grains of synthesized product zeolite have small sizes and are relatively uniformly distributed.
Description
Technical field
The invention belongs to micropore material technology field, be specifically related to the method for heterogeneous nucleation synthesizing high-silicon zeolitic material.
Background technology
Supersiliceous zeolite molecular sieve is important shape-selective catalyst and sorbent material.There are liquid water glass, silicon sol in the conventional silicon source of synthesizing high-silicon zeolite, solid-state Silica hydrogel, precipitated silica, white carbon black, Silicon-rich natural mineral kaolin, montmorillonite etc.Aluminium source is liquid aluminium salt, meta-aluminate, solid-state aluminum oxide, aluminium hydroxide, plan book diaspore etc.The report making silicon source synthetic zeolite of glass powder is very rare.Chemistry journal 2003 (61,2,251-255) He 2004 years (62,19, two sections of papers 1912-1916) report boracic micropore glass powder spontaneous generation MFI(ZSM-5 of vapour/solid state reaction in ethamine-water or methylamine-water mixing steam respectively) or TON(ZSM-22, CF-2) zeolite molecular sieve crystallization mechanism research.
Glass is common Silicon-rich or pure silicon dioxide solid material.Glass powder is often abandoned as solid waste in glass processing related industries, uses it as the silicon raw material of synthesizing high-silicon zeolite, has actual application value.Water glass, silicon sol that industrial synthesizing high-silicon zeolite is conventional, the silicon dioxide structure in solid-state Silica hydrogel, precipitated silica, white carbon black is all the poly-or poly silicate ion of unordered list or micelle.Typical silica gel be by elementary SiO2 silicon-oxy tetrahedron altogether oxygen summit amorphous micelle is assembled, interlinkage forms chain three-dimensional structure [work such as Xu Ruren, " molecular sieve and porous material chemistry " P347-348, Science Press in March, 2004].As shown in Figure 7.SiO2 in glass then forms the reticulated structure [Zhou Xiaodi etc. translate, " structural inorganic chemistry ", P109, People's Education Publishing House, in September, 1981 for day, the good work in paulownia mountain] of short range order.As shown in Figure 8.Obviously, take glass as the silicon source of synthesis zeolite, its crystallization principle and rule and be not quite similar with above-mentioned conventional silicon source.
The silicon dioxide structure of vitreous state is relatively stable, rebuilds formation crystallization of zeolites after destroying its structure, need use zeolite seed crystal assist and use organic amine be directed agents just likely.In the building-up reactions raw material that unbodied silicon source is formed, add the zeolite crystal of certain structure as crystal seed, the crystallization of this structure type zeolites can be promoted, shorten synthesising reacting time, avoid generating the little and distribution uniform of product Zeolite grain-size that stray crystal improves product purity, synthesis mutually.Different from this homophase crystal seed, also there is the patent report using out-phase zeolite seed crystal for the synthesis of ad hoc structure zeolite.As CN103429533 report BEA(Beta) zeolite seed crystal guiding amorphous silicon al reactant generation MTW(ZSM-12) zeolite.CN102659134 proposes with the zeolite with five oxygen ring structures, as Silicalite-1, ZSM5, ZSM-11, ZSM-35 make crystal seed synthesis MOR zeolite (mordenite).Crystal seed synthesis small-particle MOR zeolite made by CN102602957 report laminate structure zeolite such as FER, MWW or layer silicate such as MCM-50, ten silica layered silicates.USP6923949 report BEA(Beta) zeolite seed crystal is with N, N, N, N
,, N
,, N
,-vegolysen, 6-C6 bis-ammonium is directed agents, and white carbon black, silicon sol or silica gel are silicon source synthesis MRI(ZSM-48) zeolite.
Summary of the invention
The object of the present invention is to provide that a kind of reaction times is short, product purity is high, grain-size is little and the supersiliceous zeolite synthetic method be evenly distributed.
The supersiliceous zeolite synthetic method that the present invention proposes, take glass powder as silicon source, out-phase nucleus is crystal seed, alkylamine is structure directing agent, anabolic reaction mixture, carry out hydro-thermal reaction by the guide effect of out-phase nucleus, synthesis obtains high silicon MRE(ZSM-48), MFI(ZSM-5) or MTN(ZSM-39) zeolite molecular sieve.
In the present invention, described out-phase nucleus is crystal form silico-aluminate (zeolite), aluminum phosphate (AlPO) or aluminium silicophosphate (SAPO) molecular sieve, or natural mineral molecular sieve crystal.
In the present invention, alkylamine used is ethamine (EA).
In the present invention, the structure type of described crystal form silico-aluminate (zeolite) is FER, MOR, FAU, CHA, EUO, BEA, LTA; Described aluminum phosphate (AlPO) or aluminium silicophosphate (SAPO) molecular sieve structure type are SAPO-34(CHA type structures), SAPO-RHO(RHO type structure), SAPO-5(AFI type structure) or crystallne phosphoric acid aluminium; The structure type of described natural mineral molecular sieve crystal is STI, HEU, sepiolite, kaolin or polynite.
In the present invention, the composition of described reaction mixture by mass:
Alkylamine: 1,
Na
2O：0.03~0.15，
SiO
2：0.7-1.5
H
2O：10-20
Out-phase nucleus (Seed): 0.04 ~ 0.1.
In the present invention, described hydrothermal temperature is 140-200 degree Celsius, and the reaction times is 24-100 hour, and preferable reaction temperature is 140-180 degree Celsius, and the reaction times is 24-72 hour.
The inventive method can shorten synthesising reacting time, avoids generating stray crystal and improves product purity mutually, the little and distribution uniform of the product Zeolite grain-size of synthesis.
Accompanying drawing explanation
Fig. 1 is synthetic product MTN X zeolite x ray diffration pattern x.
Fig. 2 is synthetic product MRE X zeolite x ray diffration pattern x.
Fig. 3 is synthetic product MFI X zeolite x ray diffration pattern x.
Fig. 4 is synthetic product MTN zeolite electron scanning micrograph.
Fig. 5 is synthetic product MRE zeolite electron scanning micrograph.
Fig. 6 is synthetic product MFI zeolite electron scanning micrograph.
Fig. 7 is typical silica gel three-dimensional structure diagram.
Fig. 8 is the SiO in glass
2form the reticulated structure diagram of short range order.
Embodiment
The present invention is further described below by embodiment.
Embodiment 1
Taking fused silica powder as silicon source, with ethamine (EA) for template, add FER(ferrierite) molecular sieve crystal (SAR=20) is crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05FER ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MTN zeolite crystal reaction product.
Embodiment 2
Being silicon source with fused silica powder, taking ethamine as template, add MOR(mordenite) molecular sieve crystal (SAR=13) is crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05MOR ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MTN zeolite crystal reaction product.
Embodiment 3
Being silicon source with fused silica powder, take ethamine as template, with FAU(high-silicon Y-Zeolite) molecular sieve crystal (SAR=90) is crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05FAU ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MRE zeolite crystal reaction product.
Embodiment 4
Being silicon source with fused silica powder, take ethamine as template, with CHA(SSZ-13) molecular sieve crystal (SAR=40) is crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05CHA ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MTN zeolite crystal reaction product.
Embodiment 5
Being silicon source with fused silica powder, take ethamine as template, with EUO zeolite (SSZ-47) molecular sieve crystal (SAR=30) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05EUO ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, reaction product after filtration, is washed, dry, obtain the mixed crystal of MTN zeolite and MFI zeolite crystal.
Embodiment 6
Being silicon source with fused silica powder, take ethamine as template, with the super steady Y of USY() molecular sieve crystal (SAR=8) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05USY ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 7
Being silicon source with fused silica powder, take ethamine as template, with LTA(NaA zeolite) molecular sieve crystal (SAR=2) is crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05LTA ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 8
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=360) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MRE zeolite crystal reaction product.
Embodiment 9
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=117) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MTN zeolite crystal reaction product.
Embodiment 10
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=50) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MTN zeolite crystal reaction product.
Embodiment 11
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=50) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 160 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, reaction product after filtration, is washed, dry, obtain the mixed crystal of MTN zeolite crystal and MRE zeolite crystal.
Embodiment 12
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=390) for crystal seed, according to EA:0.05Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MRE zeolite crystal reaction product.
Embodiment 13
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=390) for crystal seed, according to EA:0.03Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, reaction product after filtration, is washed, dry, obtain the mixed crystal of MRE crystal and MTN zeolite crystal.
Embodiment 14
Being silicon source with fused silica powder, take ethamine as template, with MFI molecular sieve crystal (SAR=20) for crystal seed, according to EA:0.05Na
2o:SiO
2: 12H
2o:0.05MFI ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 140 DEG C of baking ovens, hydro-thermal reaction 70h under self-generating pressure, reaction product after filtration, is washed, dry, obtain the mixed crystal of MRE zeolite crystal and MFI zeolite crystal.
Embodiment 15
Being silicon source with fused silica powder, take ethamine as template, with powdery Al
2o
3for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05Al
2o
3ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 16
Being silicon source with fused silica powder, take ethamine as template, with SAPO-34 molecular sieve crystal for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05SAPO-34 ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 17
Being silicon source with fused silica powder, take ethamine as template, with SAPO-5 molecular sieve crystal for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05SAPO-5 ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 18
Being silicon source with fused silica powder, take ethamine as template, with SAPO-RHO crystal for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05SAPO-RHO ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 19
Being silicon source with fused silica powder, take ethamine as template, with ALPO
4crystal is crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05ALPO
4ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 20
Being silicon source with fused silica powder, take ethamine as template, with natural STI (stilbite) molecular sieve crystal (SAR=10) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05STI ratio mixes, and this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain the mixed crystal of MRE zeolite crystal and MF zeolite crystal reaction product.
Embodiment 21
Being silicon source with fused silica powder, take ethamine as template, with natural HEU zeolite (clinoptilolite) molecular sieve crystal (SAR=10) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05HEU ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 180 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 22
Being silicon source with fused silica powder, take ethamine as template, with natural sepiolite (HP) molecular sieve fiber crystal (silicon magnesium atom is than 0.75) for crystal seed, according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05HP ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 160 DEG C of baking ovens, hydro-thermal reaction 24h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 23
Being silicon source with fused silica powder, take ethamine as template, with kaolin (KO) for crystal seed (SAR=2.0), according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05KO ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 140 DEG C of baking ovens, hydro-thermal reaction 72h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Embodiment 24
Being silicon source with fused silica powder, take ethamine as template, with polynite (MO) for crystal seed (SAR=4.0), according to EA:0.1Na
2o:SiO
2: 12H
2o:0.05MO ratio mixes, and puts into the withstand voltage reactor of stainless steel to 100ml capacity, this reactor is placed in 140 DEG C of baking ovens, hydro-thermal reaction 65h under self-generating pressure, and after filtration, washing, dries, obtain MFI zeolite crystal reaction product.
Claims (6)
1. the synthetic method of a supersiliceous zeolite, it is characterized in that, take glass powder as silicon source, out-phase nucleus is crystal seed, alkylamine is structure directing agent, anabolic reaction mixture, carries out hydro-thermal reaction by the guide effect of out-phase nucleus, and synthesis obtains high silicon MRE(ZSM-48), MFI(ZSM-5) or MTN(ZSM-39) zeolite molecular sieve.
2. the synthetic method of supersiliceous zeolite according to claim 1, is characterized in that, described out-phase nucleus is crystal form silico-aluminate, aluminum phosphate or aluminium silicophosphate molecular sieve, or natural mineral molecular sieve crystal.
3. the synthetic method of supersiliceous zeolite according to claim 1, is characterized in that, alkylamine used is ethamine.
4. the synthetic method of supersiliceous zeolite according to claim 2, is characterized in that, the structure type of described crystal form silico-aluminate is FER, MOR, FAU, CHA, EUO, BEA or LTA; Described aluminum phosphate or aluminium silicophosphate molecular sieve structure type are SAPO-34, SAPO-RHO, SAPO-5 or crystallne phosphoric acid aluminium; The structure type of described natural mineral molecular sieve crystal is STI, HEU, sepiolite, kaolin or polynite.
5. the synthetic method of supersiliceous zeolite according to claim 1, is characterized in that, the composition of described reaction mixture is by mass:
Alkylamine: 1,
Na
2O：0.03~0.15，
SiO
2：0.7-1.5
H
2O：10-20
Out-phase nucleus: 0.04 ~ 0.1.
6. the synthetic method of supersiliceous zeolite according to claim 1, is characterized in that, described hydrothermal temperature is 140-200 degree Celsius, reaction times 24-100 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044792A (en) * | 2016-05-31 | 2016-10-26 | 南开大学 | SAPO-34 molecular-sieve preparing method simultaneously using crystal microporous aluminum phosphite NKX-6 as phosphorus source and aluminum source |
| CN106082266A (en) * | 2016-05-31 | 2016-11-09 | 南开大学 | The method that two kinds of microporous crystals coordinate conversion to prepare SAPO 34 molecular sieve |
| CN111762796A (en) * | 2020-07-04 | 2020-10-13 | 复榆(张家港)新材料科技有限公司 | Preparation method of zeolite with BEA structure |
| CN114873602A (en) * | 2022-03-30 | 2022-08-09 | 南京大学 | Novel phosphorus-silicon molecular sieve material named NPS-2 and preparation method thereof |
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| CN1930083A (en) * | 2004-03-05 | 2007-03-14 | 埃克森美孚研究工程公司 | Synthesis of ZSM-48 crystals with heterostructural, non ZSM-48, seeding |
| CN102530986A (en) * | 2012-01-10 | 2012-07-04 | 复旦大学 | Method for producing MFI type zeolites |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1930083A (en) * | 2004-03-05 | 2007-03-14 | 埃克森美孚研究工程公司 | Synthesis of ZSM-48 crystals with heterostructural, non ZSM-48, seeding |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106044792A (en) * | 2016-05-31 | 2016-10-26 | 南开大学 | SAPO-34 molecular-sieve preparing method simultaneously using crystal microporous aluminum phosphite NKX-6 as phosphorus source and aluminum source |
| CN106082266A (en) * | 2016-05-31 | 2016-11-09 | 南开大学 | The method that two kinds of microporous crystals coordinate conversion to prepare SAPO 34 molecular sieve |
| CN106044792B (en) * | 2016-05-31 | 2018-03-09 | 南开大学 | A kind of crystalline microporous aluminium phosphite NKX 6 prepares the molecular sieve methods of SAPO 34 as phosphorus source and silicon source simultaneously |
| CN111762796A (en) * | 2020-07-04 | 2020-10-13 | 复榆(张家港)新材料科技有限公司 | Preparation method of zeolite with BEA structure |
| CN114873602A (en) * | 2022-03-30 | 2022-08-09 | 南京大学 | Novel phosphorus-silicon molecular sieve material named NPS-2 and preparation method thereof |
| CN114873602B (en) * | 2022-03-30 | 2023-06-06 | 南京大学 | Phosphorus-silicon molecular sieve material named NPS-2 and preparation method thereof |
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