CN110422855A - A kind of preparation method that Ti-beta molecular sieve is nanocrystalline - Google Patents
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline Download PDFInfo
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- CN110422855A CN110422855A CN201910678780.8A CN201910678780A CN110422855A CN 110422855 A CN110422855 A CN 110422855A CN 201910678780 A CN201910678780 A CN 201910678780A CN 110422855 A CN110422855 A CN 110422855A
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- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
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Abstract
The invention discloses a kind of preparation methods that Ti-beta molecular sieve is nanocrystalline, comprising: mixes 0.017~0.062g butyl titanate with the solution that the mass fraction of 4.21~18g tetraethyl ammonium hydroxide is 35%, mixed solution is made；Crystallizing treatment after mixing by the white carbon black of mixed solution and 0.8~7g after drying is carried out in 40~90 DEG C of at a temperature of 30~720min of drying again, obtains Crystallizing treatment product；To Crystallizing treatment product successively through supercooling, washing, drying, calcination processing, the Ti-beta molecular sieve that can be obtained high-crystallinity is nanocrystalline.Synthesis step of the invention is simple, without using crystal seed and introduce F ion, and can to prepare crystallization complete in a short time, the nanocrystalline good dispersion of Ti-beta molecular sieve prepared, particle diameter distribution is uniform, meanwhile, the structure directing agent and water consumption that this method synthesis process uses are small, therefore, this method also has many advantages, such as that at low cost, environmental pollution is small, is conducive to industrialized production.
Description
Technical field
The invention belongs to the nanocrystalline technical fields of molecular sieve, and in particular to a kind of preparation that Ti-beta molecular sieve is nanocrystalline
Method.
Background technique
Traditional zeolite have many advantages, such as uniform micropore, surface acid point abundant, large specific surface area, good hydrothermal stability, it is wide
It is general to be applied to absorption, heterogeneous catalysis, molecule separation etc..However, the aperture due to zeolite is usually less than 0.7nm, when being related to
When the catalyst of macromolecular reaction, the diffusion limitation in crystal is a problem very serious.Nanometer point can be prepared
Son sieve, shortens diffusion path length, to solve the problems, such as this.Nano molecular sieve has been widely used in adsorbent, more at present
The mutually traditional fields such as catalysis, molecule separation, but also by its application extension to microbiological fuel cell, chemical sensitisation, cosmetics
With the emerging fields such as food, optical device, biomedicine and drug delivery.
Nano molecular sieve generally uses conventional hydrothermal crystallization synthetic method to prepare, and the preparation relative to conventional micron zeolite synthesizes
Process is complicated, needs to introduce F ion or crystal seed, and water consumption is big and is difficult to that product is collected by filtration, and causes high production cost,
Wastewater treatment is difficult, is not easy to form large-scale production.
Summary of the invention
Place in view of the deficiency of the prior art, the present invention provides a kind of Ti-beta molecular sieve is nanocrystalline
Preparation method.
In order to achieve the above technical purposes, the present invention is realized by following technical scheme:
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline, comprising:
It is 35% by the mass fraction of 0.017~0.062g butyl titanate and 4.21~18g tetraethyl ammonium hydroxide
Solution mixing, is made mixed solution, then at a temperature of dry 30~720min by mixed solution at 40~90 DEG C；
After mixing by the white carbon black of mixed solution and 0.8~7g after drying, it is carried out under conditions of steam assists
Crystallizing treatment obtains Crystallizing treatment product；
To Crystallizing treatment product successively through supercooling, washing, drying, calcination processing, the Ti- of high-crystallinity can be obtained
Beta molecular sieve is nanocrystalline.
Further, after mixing butyl titanate with tetraethyl ammonium hydroxide solution, with stirring for 450~550r/min
It mixes speed, after stirring 1~for 24 hours, then in 40~90 DEG C of dry 30~720min, can be obtained mixed solution.
Further, the Crystallizing treatment carries out in hydrothermal reaction kettle, and is put into 1 in the kettle lining of the hydrothermal reaction kettle
The deionized water of~10ml.
Further, the mixture is put into the glassware of opening, and glassware is put into hydrothermal reaction kettle later
In kettle lining, and to prevent the water in hydrothermal reaction kettle kettle lining from entering in the glassware.
Further, the crystallization temperature of the Crystallizing treatment is 130~200 DEG C, and crystallization time is 20~48h.
Further, the carrying out washing treatment includes: to carry out centrifuge washing processing, washing times 1 to liquid gel product
~3 times, centrifugal rotational speed is 8000~12000r/min.
Further, the calcination temperature of the calcination processing is 500~600 DEG C, and calcination time is 6~12 hours.
Further, the nanocrystalline partial size of the Ti-beta molecular sieve is 40~110nm.
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline provided by the invention, synthesis step is simple, without using crystalline substance
Kind and introducing F ion, and the nanocrystalline dispersion of Ti-beta molecular sieve that crystallization is complete, prepares can be prepared in a short time
Property is good, and particle diameter distribution is uniform, meanwhile, the structure directing agent and water consumption that this method synthesis process uses are small, and therefore, this method is also
Have many advantages, such as that at low cost, environmental pollution is small, be conducive to industrialized production.
Detailed description of the invention
Fig. 1 is the nanocrystalline XRD diagram of the Ti-beta molecular sieve of the preparation of exemplary embodiment of the present 1；
Fig. 2 is the nanocrystalline SEM photograph of the Ti-beta molecular sieve of the preparation of exemplary embodiment of the present 1；
Fig. 3 is the nanocrystalline XRD diagram of the Ti-beta molecular sieve of the preparation of exemplary embodiment of the present 2；
Fig. 4 is the nanocrystalline SEM photograph of the Ti-beta molecular sieve of the preparation of exemplary embodiment of the present 2；
Fig. 5 is the nanocrystalline XRD diagram of the Ti-beta molecular sieve of the preparation of exemplary embodiment of the present 3；
Fig. 6 is the nanocrystalline SEM photograph of the Ti-beta molecular sieve of the preparation of exemplary embodiment of the present 3.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the preferred embodiment of the present invention
In attached drawing, technical solution in the embodiment of the present invention is further described in more detail.In the accompanying drawings, identical from beginning to end or
Similar label indicates same or similar element or element with the same or similar functions.Described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.The embodiments described below with reference to the accompanying drawings are exemplary, it is intended to
It is used to explain the present invention, and is not considered as limiting the invention.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without creative efforts, shall fall within the protection scope of the present invention.
The embodiment of the present invention is described in detail with reference to the accompanying drawing.
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline, includes the following steps:
It (1) is 35% by the mass fraction of 0.017~0.062g butyl titanate and 4.21~18g tetraethyl ammonium hydroxide
Solution mixing, with the mixing speed of 450~550r/min, after stirring 1~for 24 hours, then in 40~90 DEG C of dry 30~720min,
Mixed solution is made；
(2) after mixing by the white carbon black of mixed solution and 0.8~7g, mixture transfer is placed on to the glass of opening
In vessel, glassware is put into the hydrothermal reaction kettle kettle lining of the deionized water equipped with 1~10ml in kettle lining later, and to prevent
Only the water outside glassware enters in glassware；Under conditions of steam auxiliary, the temperature of hydrothermal reaction kettle is adjusted to 130~
200 DEG C, crystallization time is 20~48h, obtains Crystallizing treatment product；
It (3) is then 8000~12000r/ in centrifugal rotational speed by product to Crystallizing treatment product cooled to room temperature
Washing 1~3 time in the centrifuge of min, re-dry, finally 500~600 DEG C at a temperature of, calcine 6~12 in air atmosphere
Hour, the Ti-beta molecular sieve that can be obtained the high-crystallinity that partial size is 40~110nm is nanocrystalline.
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline provided by the invention, synthesis step is simple, without using crystalline substance
Kind and introducing F ion, and crystallization can be prepared in a short time completely (crystallization time is short, and most short 15h can be crystallized), preparation
The nanocrystalline good dispersion of Ti-beta molecular sieve out, particle diameter distribution is uniform, and by controlling crystallizing handle when state modulator
The nanocrystalline partial size of Ti-beta molecular sieve；Meanwhile it is different from traditional xerogel transformation method, a small amount of water is kept in reactant
It can make nanocrystalline quick formation, on the one hand prevent structure directing agent caused by being evaporated completely (tetraethyl ammonium hydroxide solution)
Loss, on the other hand a small amount of water helps to improve degree of supersaturation, is conducive to largely nucleation and crystal growth, and therefore, this method is closed
The structure directing agent and water consumption used at process is small, and then not only reduces the cost of this method, and also reduce to ring
The pollution in border, is conducive to industrialized production.
Embodiment 1
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline, includes the following steps:
(1) 0.017g butyl titanate is mixed with the solution that the mass fraction of 4.21g tetraethyl ammonium hydroxide is 35%,
With the mixing speed of 500r/min, after stirring 12h, then the dry 120min in 70 DEG C of baking oven, mixed solution is made；
(2) after mixing by the white carbon black of mixed solution and 0.8g, mixture transfer is placed on to the vierics of opening
In ware, glassware is put into the hydrothermal reaction kettle kettle lining of the deionized water equipped with 4ml in kettle lining later, and to prevent glass
Water outside vessel enters in glassware；Under conditions of steam auxiliary, the temperature of hydrothermal reaction kettle is adjusted to 160 DEG C, crystallization
Time is 20h, obtains Crystallizing treatment product；
(3) to Crystallizing treatment product cooled to room temperature, then by product centrifugal rotational speed be 10000r/min from
Washing 2 times in scheming, re-dry, finally 580 DEG C at a temperature of, calcine 12 hours in air atmosphere, can be obtained partial size
Ti-beta molecular sieve for the high-crystallinity for being about 100nm is nanocrystalline.
It will be seen from figure 1 that there is the appearance of beta characteristic peak, it was demonstrated that Ti-beta is successfully crystallized, figure it is seen that Ti-
The pattern of beta is complete, and particle diameter distribution is uniform, substantially in 100nm or so.
Embodiment 2
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline, includes the following steps:
(1) 0.04g butyl titanate is mixed with the solution that the mass fraction of 8.42g tetraethyl ammonium hydroxide is 35%,
With the mixing speed of 450r/min, after stirring 11h, then the dry 180min in 65 DEG C of baking oven, mixed solution is made；
(2) after mixing by the white carbon black of above-mentioned mixed solution and 6g, it is moved into vial, is transferred to later
In 50ml hydrothermal reaction kettle kettle lining, 4ml deionized water is added in reaction kettle lining, and prevent the water outside vial from entering vial
In, temperature of reaction kettle is adjusted, makes mixed solution at 155 DEG C, crystallization 48h obtains Crystallizing treatment product；
(3) to Crystallizing treatment product cooled to room temperature, then by product in the centrifugation that centrifugal rotational speed is 8000r/min
Washing 1 time in machine, re-dry, finally 500 DEG C at a temperature of, calcine 6 hours in air atmosphere, can be obtained partial size is
The Ti-beta molecular sieve of the high-crystallinity of 50nm or so is nanocrystalline.
From figure 3, it can be seen that there is the appearance of beta characteristic peak, it was demonstrated that Ti-beta is successfully crystallized, from fig. 4, it can be seen that Ti-
The pattern of beta is complete, and particle diameter distribution is uniform, substantially in 50nm or so.
Embodiment 3
A kind of preparation method that Ti-beta molecular sieve is nanocrystalline, includes the following steps:
(1) 0.062g butyl titanate is mixed with the solution that the mass fraction of 10g tetraethyl ammonium hydroxide is 35%, with
The mixing speed of 550r/min, after stirring for 24 hours, then the dry 720min in 90 DEG C of baking oven, mixed solution is made；
(2) after mixing by the white carbon black of mixed solution and 7g, mixture transfer is placed on to the glassware of opening
In, glassware is put into the hydrothermal reaction kettle kettle lining of the deionized water equipped with 4ml in kettle lining later, and to prevent vierics
Water outside ware enters in glassware；Under conditions of steam auxiliary, the temperature of hydrothermal reaction kettle is adjusted to 165 DEG C, when crystallization
Between for for 24 hours, obtain Crystallizing treatment product；
(3) to Crystallizing treatment product cooled to room temperature, then by product centrifugal rotational speed be 12000r/min from
Washing 3 times in scheming, re-dry, finally 600 DEG C at a temperature of, calcine 12 hours in air atmosphere, can be obtained partial size
The Ti-beta molecular sieve of about 100 nanometers of high-crystallinity is nanocrystalline.
From fig. 5, it can be seen that there is the appearance of beta characteristic peak, it was demonstrated that Ti-beta is successfully crystallized, from fig. 6, it can be seen that Ti-
The pattern of beta is complete, and particle diameter distribution is uniform, substantially in 100nm or so.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (8)
1. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline characterized by comprising
The solution for being 35% by the mass fraction of 0.017~0.062g butyl titanate and 4.21~18g tetraethyl ammonium hydroxide
Mixing, is made mixed solution, then at a temperature of dry 30~720min by mixed solution at 40~90 DEG C；
After mixing by the white carbon black of mixed solution and 0.8~7g after drying, crystallization is carried out under conditions of steam assists
Processing obtains Crystallizing treatment product；
To Crystallizing treatment product successively through supercooling, washing, drying, calcination processing, it can be obtained Ti-beta points of high-crystallinity
Son sieve is nanocrystalline.
2. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 1, which is characterized in that by titanium
After sour four butyl esters are mixed with tetraethyl ammonium hydroxide solution, with the mixing speed of 450~550r/min, stir 1~for 24 hours after, then
In 40~90 DEG C of dry 30~720min, mixed solution can be obtained.
3. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 1, which is characterized in that the crystalline substance
Change processing to carry out in hydrothermal reaction kettle, and is put into the deionized water of 1~10ml in the kettle lining of the hydrothermal reaction kettle.
4. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 3, which is characterized in that described mixed
It closes object to be put into the glassware of opening, glassware is put into hydrothermal reaction kettle kettle lining later, and to prevent hydro-thermal reaction
Water in kettle kettle lining enters in the glassware.
5. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 1, which is characterized in that the crystalline substance
The crystallization temperature for changing processing is 130~200 DEG C, and crystallization time is 20~48h.
6. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 1, which is characterized in that described to wash
Wash processing include: to liquid gel product carry out centrifuge washing processing, washing times be 1~3 time, centrifugal rotational speed be 8000~
12000r/min。
7. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 1, which is characterized in that described to forge
The calcination temperature for burning processing is 500~600 DEG C, and calcination time is 6~12 hours.
8. a kind of preparation method that Ti-beta molecular sieve is nanocrystalline according to claim 1, the Ti-beta molecular sieve
Nanocrystalline partial size is 40~110nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439756A (en) * | 2020-04-07 | 2020-07-24 | 福州大学 | Preparation method of cascade pore heteroatom M-Beta molecular sieve |
| CN113264558A (en) * | 2021-04-15 | 2021-08-17 | 大连理工大学盘锦产业技术研究院 | Fe3O4Preparation method and application of/Silicate-1 molecular sieve nanocrystalline composite material |
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| US9108190B1 (en) * | 2012-09-12 | 2015-08-18 | University Of Massachusetts | Rapid synthesis of beta zeolites |
| CN109467099A (en) * | 2019-01-08 | 2019-03-15 | 福州大学 | A kind of preparation method of nanoscale pure silicon step hole Beta molecular sieve |
| CN109850914A (en) * | 2019-04-15 | 2019-06-07 | 福州大学 | A kind of preparation method of the nanoscale without aluminium Ti-Beta molecular sieve |
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| US9108190B1 (en) * | 2012-09-12 | 2015-08-18 | University Of Massachusetts | Rapid synthesis of beta zeolites |
| CN109467099A (en) * | 2019-01-08 | 2019-03-15 | 福州大学 | A kind of preparation method of nanoscale pure silicon step hole Beta molecular sieve |
| CN109850914A (en) * | 2019-04-15 | 2019-06-07 | 福州大学 | A kind of preparation method of the nanoscale without aluminium Ti-Beta molecular sieve |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111439756A (en) * | 2020-04-07 | 2020-07-24 | 福州大学 | Preparation method of cascade pore heteroatom M-Beta molecular sieve |
| CN113264558A (en) * | 2021-04-15 | 2021-08-17 | 大连理工大学盘锦产业技术研究院 | Fe3O4Preparation method and application of/Silicate-1 molecular sieve nanocrystalline composite material |
| CN113264558B (en) * | 2021-04-15 | 2023-08-22 | 大连理工大学盘锦产业技术研究院 | Fe (Fe) 3 O 4 Preparation method and application of silica-1 molecular sieve nanocrystalline composite material |
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