CN109694089A - One-dimensional nano line VPI-8 molecular sieve and its synthetic method - Google Patents
One-dimensional nano line VPI-8 molecular sieve and its synthetic method Download PDFInfo
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Abstract
The present invention relates to a kind of one-dimensional nano line VPI-8 molecular sieve and its synthetic method, the technical problem to be solved is that provide it is a kind of before this without pattern reported in the literature be the VPI molecular sieve of one-dimensional nano line, and provide the synthetic method of corresponding molecular sieve.Duct orientation and pattern control are the importances in Zeolite synthesis field, the VPI-8 molecular sieve for synthesizing draw ratio > 100 of the invention, these nano wires VPI-8 molecular sieve constitutes 40-100 μm of diameter of fluffy reunion shape structure, it is effectively increased the porosity of molecular sieve, enhance its adsorption capacity and adsorption capacity, has good application prospect in the fields such as conventional catalyst reaction and light-catalyzed reaction.
Description
Technical field
The present invention relates to a kind of synthetic method of molecular sieve, more specifically a kind of one-dimensional nano line VPI-8 molecular sieve
And its synthetic method.
Background technique
Molecular sieve is that a kind of silicate material of crystallization is being urged due to some particularity in its structure and chemical property
Change, the fields such as absorption and ion exchange all have extensive use.Some molecular sieves can be obtained from nature, however, greatly
Part in the molecular sieve that catalytic field obtains practical application is obtained by artificial synthesized method.Hydrothermal synthesis method is
The method of most common synthesis of molecular sieve.A key factor for determining molecular sieve application performance is that its duct or cage cave are special
Sign, and these are characterized in being determined by the intrinsic crystal structure of molecular sieve, thus obtain the molecular sieve of new crystal structure for
It has very important significance for the application of developing molecular sieve.
VPI-8 molecular sieve is a kind of zinc si molecular sieves of better heat stability, belongs to VET family, has one-dimensional ten binary
Ring cellular structure has application potential in the cracking industry of petroleum macromolecular.VPI-8 molecular sieve earliest by Annen M.J. and
DavisM.E. equal synthesis.VPI-8 molecular sieve is reported in document (Microporous Mater, 1997,11:127-136)
Synthetic method has investigated the effect of zinc ion, alkali metal ion and organic ion in synthesis respectively.The molecular sieve of synthesis is
Corynebacterium, up to approximately 3 μm, draw ratio is 10 or so, and zinc silicon is than range 5 < Si/Zn < 100.Document (petroleum journal, 2004,20
(5): 27-31. the method using cheap TEABr for template synthesizing high-silicon zinc ratio VPI-8 molecular sieve) is reported, feed intake silicon
Zinc ratio between 10-50, product be it is rodlike, several microns to tens microns of length are differed, and draw ratio is still in 10 or so.
Nano wire is commonly known as a material, is commonly defined as being limited in 100nm hereinafter, on longitudinal direction in a kind of transverse direction
The one-dimentional structure that there is no limit.Patent (CN201410004146.3) reports a kind of Fe2O3/ Silicalite-1 molecular sieve is received
The synthetic method and application of rice noodles.The Sample Width of synthesis is 100~300nm, and length is greater than 5 μm.
So far, document there is no to be related to the synthesis of nano wire VPI-8 molecular sieve.
Summary of the invention
The technical problem to be solved by the present invention is to a kind of nano wire VPI-8 molecular sieve being not directed in the prior art and its
Synthetic method.
In order to solve the above technical problems, adopting the following technical scheme that
The present invention provides a kind of one-dimensional nano line VPI-8 molecular sieve, and the one-dimensional nano line VPI-8 molecular sieve is nano wire
The pure phase VPI-8 molecular sieve of shape, draw ratio > 100, the diameter of nano wire VPI-8 molecular sieve are 40-100nm.
In above-mentioned technical proposal, it is preferable that the diameter of the nano wire VPI-8 molecular sieve is 40-80nm.
In above-mentioned technical proposal, it is preferable that the nano wire VPI-8 molecular sieve constitutes 40-100 μm of diameter of fluffy reunion
Shape structure.
In above-mentioned technical proposal, it is preferable that the draw ratio is > 200
The present invention also provides a kind of methods of synthesizing one-dimensional nano wire VPI-8 molecular sieve, comprising the following steps:
A) according to 10SiO2: (0.05~0.5) ZnO:(0.5~4.5) alkaline matter A:(2.0~6.0) organic formwork agent
R:(0.0005~0.5) surfactant S:(100~400) H2The initial molar of O matches, by silicon source, zinc source, alkaline matter A,
Organic formwork agent R, surfactant S and water are uniformly mixed to get mixture；
B) by the mixture hydrothermal crystallizing, products therefrom is washed and is dried, and obtains one-dimensional nano line VPI-8 molecule
Sieve.
In above-mentioned technical proposal, it is preferable that silicon source includes being selected from silica solution, solid silicone, gas-phase silica, and amorphous two
At least one of silica or organic silicone grease.
In above-mentioned technical proposal, it is preferable that zinc source includes being selected from zinc oxide, zinc acetate, zinc nitrate, zinc chloride or zinc oxalate
At least one of.
In above-mentioned technical proposal, it is preferable that alkaline matter A includes being selected from lithia, sodium oxide molybdena, potassium oxide, lithium hydroxide,
At least one of sodium hydroxide or potassium hydroxide.
In above-mentioned technical proposal, it is preferable that organic formwork agent R includes being selected from tetramethylammonium hydroxide, tetraethyl hydroxide
Ammonium, tetrapropylammonium hydroxide, at least one of 4 bromide, tetraethylammonium bromide or 4-propyl bromide.
In above-mentioned technical proposal, it is preferable that surfactant S include selected from cetyl trimethylammonium bromide (CTAB) and
At least one of polyethylene glycol.
In above-mentioned technical proposal, it is preferable that the initial molar proportion of mixture is 10SiO2: (0.05~0.3) ZnO:
(0.5~3.0) alkaline matter A:(2.0~6.0) organic formwork agent R:(0.2~0.5) surfactant S:(100~400)
H2O。
In above-mentioned technical proposal, it is preferable that mixture hydrothermal crystallizing 50~200 hours at 130~200 DEG C.It is more excellent
Selection of land, at 160~180 DEG C, hydrothermal crystallizing 80~140 hours.
The method of synthesizing one-dimensional nano wire VPI-8 molecular sieve provided by the present invention, it is living using organic formwork agent and surface
Property agent synergistic effect, the pure phase VPI-8 molecular sieve that pattern is nanometer threadiness can be effectively synthesized, the pattern of synthetic sample more advises
It is whole, draw ratio, draw ratio > 100 are improved, nano wire VPI-8 molecular sieve constitutes 40-100 μm of diameter of fluffy reunion shape structure.
Meanwhile silicon zinc is than adjustable extent largest extension to 200.
Detailed description of the invention
Fig. 1 is obtained X-ray diffraction (XRD) figure of sample by embodiment 1.
Fig. 2 is obtained scanning electron microscope (SEM) figure of sample by embodiment 1.
Fig. 3 is obtained scanning electron microscope (SEM) figure of sample by embodiment 1.
Fig. 4 is obtained scanning electron microscope (SEM) figure of sample by embodiment 1.
Fig. 5 is obtained scanning electron microscope (SEM) figure of sample by comparative example 1.
The present invention will be further described below by way of examples, but the protection scope being not intended to limit the present invention.
Specific embodiment
[embodiment 1]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 96 hours, after reaction after washing, drying,
Through XRD identify product be pure phase VPI-8 molecular sieve, SEM as the result is shown product be one-dimensional nano line, 60~80nm of diameter, length >
10 μm, draw ratio > 200.
[embodiment 2]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 milligrams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, and gained is mixed
Close the mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.0005CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 132 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, product is one-dimensional nano line to SEM as the result is shown, has a little amorphous phase, directly
40~80nm of diameter, length > 5 μm, draw ratio > 100.
[embodiment 3]
By 0.21 gram of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.05ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 120 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, product is one-dimensional nano line, 80~100nm of diameter, length to SEM as the result is shown
> 10 μm, draw ratio > 100.
[embodiment 4]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 160 DEG C crystallization 140 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, product is one-dimensional nano line, 60~100nm of diameter, length to SEM as the result is shown
> 10 μm, draw ratio > 100.
[embodiment 5]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 180 DEG C crystallization 80 hours, after reaction after washing, drying,
Through XRD identify product be pure phase VPI-8 molecular sieve, SEM as the result is shown product be one-dimensional nano line, 40~80nm of diameter, length >
10 μm, draw ratio > 100.
[embodiment 6]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 140 DEG C crystallization 160 hours, after reaction after washing, drying,
It identifies that principal product is VPI-8 molecular sieve through XRD, is mixed with a small amount of quartzy phase stray crystal, principal product is 1-dimention nano to SEM as the result is shown
Line, 40~100nm of diameter, length > 10 μm, draw ratio > 100.
[embodiment 7]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 34.0 grams of water, the white carbon black that 3.40 grams of CTAB and 12.44g dioxide-containing silica is 90% are uniformly mixed, institute
Obtain the mol ratio of mixture are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 96 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, product is one-dimensional nano line, 60~100nm of diameter, length to SEM as the result is shown
> 10 μm, draw ratio > 100.
[embodiment 8]
By 0.88 gram of two oxalic acid hydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 96 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, product is one-dimensional nano line, 60~100nm of diameter, length to SEM as the result is shown
> 10 μm, draw ratio > 100.
[embodiment 9]
By 1.02 grams of acetic acid dihydrate zinc, 2.24 grams of sodium hydroxides, 43.99 gram 25% of tetraethyl ammonium hydroxide is molten
Liquid, 51.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixture
Mol ratio are as follows:
10SiO2: 0.25ZnO:3.0NaO:4.0TEAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 96 hours, after reaction after washing, drying,
It identifies that product main phase is VPI-8 molecular sieve through XRD, there is a small amount of quartzy phase.Product is one-dimensional nano line to SEM as the result is shown, directly
80~100nm of diameter, length > 10 μm, draw ratio > 100.
[embodiment 10]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 60.72 gram 25% of tetrapropyl hydroxide
Ammonium salt solution, 34.0 grams of water, 3.40 grams of CTAB and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, gained mixing
The mol ratio of object are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TPAOH:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 96 hours, after reaction after washing, drying,
It identifies that product main phase is VPI-8 molecular sieve through XRD, there is a small amount of quartzy phase.Product is one-dimensional nano line to SEM as the result is shown, directly
80~100nm of diameter, length > 10 μm, draw ratio > 100.
[embodiment 11]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water, 1.68 grams of polyethylene glycol (PEG300) and the mixing of 21.54 milliliter 40% of silicon sol solution are equal
It is even, the mol ratio of gained mixture are as follows:
10SiO2: 0.25ZnO:3.0LiO:4.0TEAOH:0.3PEG300:300H2O
By said mixture move into reaction kettle in 180 DEG C crystallization 96 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, product is one-dimensional nano line, 60~100nm of diameter, length to SEM as the result is shown
> 10 μm, draw ratio > 100.
[comparative example 1]
By 4.08 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 43.99 gram 25% of tetraethyl hydroxide
Ammonium salt solution, 51.0 grams of water and 21.54 milliliter 40% of silicon sol solution are uniformly mixed, the mol ratio of gained mixture
Are as follows:
10SiO2: ZnO:3.0LiO:4.0TEAOH:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 120 hours, after reaction after washing, drying,
Identify that product is pure phase VPI-8 molecular sieve through XRD, principal product is rodlike to SEM as the result is shown.
[comparative example 2]
By 1.02 grams of acetic acid dihydrate zinc, 2.35 gram of one hydronium(ion) lithia, 51.0 grams of water, 3.40 grams of CTAB with
And 21.54 milliliter 40% of silicon sol solution is uniformly mixed, the mol ratio of gained mixture are as follows:
10SiO2: 0.25ZnO:3.0LiO:0.5CTAB:300H2O
By said mixture move into reaction kettle in 170 DEG C crystallization 96 hours, after reaction after washing, drying,
Identify that product is amorphous phase through XRD.
Claims (10)
1. a kind of one-dimensional nano line VPI-8 molecular sieve, which is characterized in that the one-dimensional nano line VPI-8 molecular sieve is nano wire
The pure phase VPI-8 molecular sieve of shape, draw ratio > 100.
2. a kind of method of synthesizing one-dimensional nano wire VPI-8 molecular sieve, comprising the following steps:
A) according to 10SiO2: (0.05~0.5) ZnO:(0.5~4.5) alkaline matter A:(2.0~6.0) organic formwork agent R:
(0.0005~0.5) surfactant S:(100~400) H2The initial molar of O matches, and by silicon source, zinc source, alkaline matter A, has
Machine template R, surfactant S and water are uniformly mixed to get mixture；
B) by the mixture hydrothermal crystallizing, products therefrom is washed and is dried, and obtains one-dimensional nano line VPI-8 molecular sieve.
3. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that silicon source includes
Selected from silica solution, solid silicone, gas-phase silica, at least one of amorphous silica or organic silicone grease.
4. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that zinc source includes
Selected from least one of zinc oxide, zinc acetate, zinc nitrate, zinc chloride or zinc oxalate.
5. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that alkaline matter A
Including being selected from lithia, sodium oxide molybdena, potassium oxide, lithium hydroxide, at least one of sodium hydroxide or potassium hydroxide.
6. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that organic formwork
Agent R includes being selected from tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide, 4 bromide, tetrem bromide
Change at least one of ammonium or 4-propyl bromide.
7. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that surface-active
Agent S includes being selected from least one of cetyl trimethylammonium bromide and polyethylene glycol.
8. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that mixture
Initial molar proportion is 10SiO2: (0.05~0.5) ZnO:(0.5~4.5) alkaline matter A:(2.0~6.0) organic formwork agent
R:(0.0005~0.5) surfactant S:(100~400) H2O。
9. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that mixture exists
Hydrothermal crystallizing 50~200 hours at 130~200 DEG C.
10. the method for synthesizing one-dimensional nano wire VPI-8 molecular sieve according to claim 2, which is characterized in that nanometer wire length
Diameter ratio > 100.
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