CN101007637A - Process for synthesizing MCM-56 molecular sieve - Google Patents
Process for synthesizing MCM-56 molecular sieve Download PDFInfo
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- CN101007637A CN101007637A CN 200610148803 CN200610148803A CN101007637A CN 101007637 A CN101007637 A CN 101007637A CN 200610148803 CN200610148803 CN 200610148803 CN 200610148803 A CN200610148803 A CN 200610148803A CN 101007637 A CN101007637 A CN 101007637A
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Abstract
The invention discloses a synthesizing method of MCM-56 molecular sieve in the inorganic chemical synthetic technical domain, which is characterized by the following: adopting MCM-22(p) as raw material; disposing through acid; sintering; obtaining the product as one number of MWW structural molecular sieve opened by US5, 362,697 firstly.
Description
Technical field
The present invention relates to a kind of synthetic method of MCM-56 molecular sieve, belong to the inorganic chemical synthesis technical field.
Background technology
The MCM-56 molecular sieve is a member in the MWW structure molecular screen family.This molecular sieve at first by Fung etc. at US5, open in 362,697.Because the MCM-56 molecular sieve has big specific surface area and many surface voids, thereby shows high catalytic activity in macromolecular catalyzed reaction.
At present the synthetic method of MCM-56 molecular sieve is substantially with US5, and disclosed process be basic in 362,697.Promptly control the generation of MCM-56 molecular sieve by the control crystallization condition.The crystalline phase of the shortcoming synthetic product MCM-56 molecular sieve of this method maximum is difficult to control, is easy to occur changeing brilliant, changes another MCM-49 molecular sieve in the MWW structure molecular screen family into.
Summary of the invention
In order to overcome the problem that background technology exists, purpose of the present invention provides a kind of synthetic method of MCM-56 molecular sieve.
For achieving the above object, the present invention by the following technical solutions: based on MCM-22 molecular sieve presoma, adopt acid solution to handle under the certain temperature condition, again through roasting, get the MCM-56 molecular sieve.MCM-22 molecular sieve presoma is exactly the MCM-22 molecular sieve that removes volatile material without roasting, is called MCM-22 (p) at present in the literature.Therefore MCM-22 molecular sieve presoma is promptly represented with MCM-22 (p) in this manual.In other words, technical scheme of the present invention is characterised in that, is raw material with MCM-22 (p), acid treatment MCM-22 (p), and roasting gets the MCM-56 molecular sieve.
The synthetic method of MCM-22 molecular sieve is more, as US 4,954,325, CN1686801, CN1789126, CN1535918 etc.In all synthetic methods, all be to synthesize MCM-22 (p) earlier, by operations such as conventional exchange, filtration, washing, roastings, obtain the MCM-22 molecular sieve then.Technical scheme of the present invention all is suitable for for the MCM-22 (p) by any method preparation.
Now describe technical scheme of the present invention in detail.
A kind of synthetic method of MCM-56 molecular sieve is characterized in that, is raw material with MCM-22 (p), operation steps:
The first step acid treatment MCM-22 (p)
Is that 0.1～6mol/l acid solution is 1 according to weight ratio with MCM-22 (p) with concentration: (5～100) preparation feedback mixture, described acid solution is mineral acid or organic acid, mineral acid is hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid, organic acid is formic acid, acetate, propionic acid or tartrate, ℃ processing is 10 minutes～3 days in room temperature～120, after filtration, washing, drying, acid-treated product;
Second one-step baking
The acid-treated product that the first step is obtained is in 400～600 ℃ of roastings 5～10 hours, product MCM-56 molecular sieve.
Technical scheme of the present invention is further characterized in that, in the first step, is that 0.5～3mol/l acidic solution is 1 according to weight ratio with MCM-22 (p) with concentration: (10～65) preparation feedback mixture, ℃ processing is 5～36 hours in room temperature～90.
Compare the advantage that the present invention has with background technology:
1. the inventive method has been avoided controlling the direct synthetic method that the MCM-56 molecular sieve forms by crystallization condition, adopts to form the stable MCM-22 molecular sieve presoma MCM-22 (p) of crystalline phase, the method for handling with acid solution then earlier.This method solves the unmanageable shortcoming of direct synthetic product crystalline phase effectively.
2. the inventive method process is simple, and no especial equipment requirements is easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the XRD spectra that embodiment 1 obtains product, with US 4,954, and the feature unanimity of the XRD spectra of 325 described MCM-56 molecular sieves.The product of embodiment 1 is exactly the MCM-56 molecular sieve.
Embodiment
All embodiment all operate by the operation steps of technique scheme.
Embodiment 1
Raw material MCM-22 (p) is according to US 4,954, and 325 described methods are synthetic.
The first step acid treatment MCM-22 (p)
With MCM-22 (p) and concentration is that 2 mol/l salpeter solutions are 1: 50 preparation feedback mixture according to weight ratio, under room temperature, handled 20 hours, after filtration, washing, drying, acid-treated product;
Second one-step baking
The acid-treated product that the first step is made is in 550 ℃ of roastings 8 hours, product MCM-56 molecular sieve.
The XRD spectra of product MCM-56 molecular sieve as shown in Figure 1.
Embodiment 2～6
Implementation process except for the following differences, all the other are all with embodiment 1:
The first step acid treatment MCM-22 (p)
Reaction mixture weight proportion and treatment condition:
Embodiment 2 MCM-22 (p): 6 mol/l nitric acid=1: 20, room temperature treatment 36 hours;
Embodiment 3 MCM-22 (p): 0.5mol/l phosphoric acid=1: 90, handled 36 hours for 80 ℃;
Embodiment 4 MCM-22 (p): 2mol/l hydrochloric acid=1: 50, handled 3 hours for 120 ℃;
Embodiment 5 MCM-22 (p): 2mol/l sulfuric acid=1: 50, handled 10 hours for 50 ℃;
Embodiment 6 MCM-22 (p): 4mol/l acetate=1: 30, handled 72 hours for 80 ℃;
The XRD spectra of product and Fig. 1's is similar.
Embodiment 7
Raw material MCM-22 (p) is synthetic according to the described method of CN1686801.
Implementation process except for the following differences, all the other are all with embodiment 1:
The XRD spectra of product and Fig. 1's is similar.
Embodiment 8
Implementation process except for the following differences, all the other are all with embodiment 7:
The first step acid treatment MCM-22 (p)
MCM-22 (p): 0.1mol/l nitric acid=1: 20, room temperature treatment 36 hours;
The XRD spectra of product and Fig. 1's is similar.
Embodiment 9
Implementation process except for the following differences, all the other are all with embodiment 7:
The first step acid treatment MCM-22 (p)
MCM-22 (p): 0.1mol/l sulfuric acid=1: 20, handled 24 hours for 50 ℃;
The XRD spectra of product and Fig. 1's is similar.
Implementation process except for the following differences, all the other are all with embodiment 7:
The first step acid treatment MCM-22 (p)
MCM-22 (p): 2mol/l phosphoric acid=1: 20, handled 24 hours for 70 ℃;
XRD spectra and Fig. 1 of product are similar.
Embodiment 11
Implementation process except for the following differences, all the other are all with embodiment 7:
The first step acid treatment MCM-22 (p)
MCM-22 (p): 2mol/l tartrate=1: 20, handled 24 hours for 60 ℃;
XRD spectra and Fig. 1 of product are similar.
Embodiment 12
Implementation process except for the following differences, all the other are all with embodiment 7:
The first step acid treatment MCM-22 (p)
MCM-22 (p): 2mol/l formic acid=1: 20, handled 24 hours for 50 ℃;
XRD spectra and Fig. 1 of product are similar.
Method of the present invention is particularly suitable for being used for preparing the MCM-56 molecular sieve.
Claims (2)
1, a kind of synthetic method of MCM-56 molecular sieve is characterized in that, is raw material with MCM-22 (p), operation steps:
The first step acid treatment MCM-22 (p)
Is that 0.1～6mol/l acid solution is 1 according to weight ratio with MCM-22 (p) with concentration: (5～100) preparation feedback mixture, described acid solution is mineral acid or organic acid, mineral acid is hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid, organic acid is formic acid, acetate, propionic acid or tartrate, ℃ processing is 10 minutes～3 days in room temperature～120, after filtration, washing, drying, acid-treated product;
Second one-step baking
The acid-treated product that the first step is obtained is in 400～600 ℃ of roastings 5～10 hours, product MCM-56 molecular sieve.
2, the synthetic method of MCM-56 molecular sieve according to claim 1, it is characterized in that, in the first step, be that 0.5～3mol/l acidic solution is 1 according to weight ratio with MCM-22 (p) with concentration: (10～65) preparation feedback mixture, ℃ processing is 5～36 hours in room temperature～90.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818917A (en) * | 2014-02-20 | 2014-05-28 | 河南科技大学 | Preparation method for zeolite with bactericidal activity |
| CN106517231A (en) * | 2015-09-15 | 2017-03-22 | 中国石油化工股份有限公司 | Synthetic method for MCM-56 molecular sieve |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8704023B2 (en) | 2008-07-28 | 2014-04-22 | Exxonmobil Chemical Patents Inc. | Molecular sieve composition EMM-13, a method of making and a process of using the same |
| JP5476379B2 (en) | 2008-07-28 | 2014-04-23 | エクソンモービル・ケミカル・パテンツ・インク | Novel molecular sieve composition EMM-12, process for its production and process for its use |
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2006
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818917A (en) * | 2014-02-20 | 2014-05-28 | 河南科技大学 | Preparation method for zeolite with bactericidal activity |
| CN103818917B (en) * | 2014-02-20 | 2016-01-20 | 河南科技大学 | A kind of preparation method with fungicidal activity zeolite |
| CN106517231A (en) * | 2015-09-15 | 2017-03-22 | 中国石油化工股份有限公司 | Synthetic method for MCM-56 molecular sieve |
| CN106517231B (en) * | 2015-09-15 | 2018-11-20 | 中国石油化工股份有限公司 | The synthetic method of MCM-56 molecular sieve |
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