CN107673369A - A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure - Google Patents
A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure Download PDFInfo
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Abstract
The present invention relates to Zeolite synthesis field, specifically a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure.A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure of the present invention, adds the Chabazite zeolite seed crystals of preparation to synthesize the Chabazite zeolites of multi-stage porous in the gel of zeolite synthesis.Solve that micropore Chabazite zeolite molecular sieves duct is narrow and small, and mass transfer rate is slow, the low shortcoming of gas absorption amount, there is critically important practical value in catalysis, absorption and separation etc..
Description
Technical field
The present invention relates to Zeolite synthesis field, specifically a kind of Chabazite boilings synthesized with multi-stage artery structure
The method of stone molecular sieve.
Background technology
Chabazite is the zeolite for having CHA topological structures, has octatomic ring hole window（0.38nm*0.38nm）Three-dimensional
Pore canal system and relatively low skeletal density, silica alumina ratio 2-10, CHA type molecular sieve is with its unique pore passage structure and selects type selection
Property the characteristics of separate etc. and have broad application prospects in methanol preparing low carbon hydrocarbons and gas.
Chabazite belongs to pore zeolite, and smaller hole road is advantageous to the progress of shape selective catalysis, but is related to macromolecular at some
In the reaction of participation, relatively small duct is but unfavorable for reactant molecule and is diffused into the catalytic active center in micropore,
Also the macromolecular for being unfavorable for generation diffuses out from reaction center, so as to cause the generation of carbon deposit, have impact on zeolite catalysis
Energy and service life.On the other hand, the narrow and small duct of Chabazite molecular sieves make it that the religion of gas molecule diffusion rate is slow, is entering
When row gas absorption and separation, gas absorption equilibration time can be increased, reduce separating effect and production efficiency.Therefore, synthesis contains
The zeolitic material for having mesopore orbit structure turns into one due to that can improve the diffusion of material and improve catalyst activity
Study hotspot.
Preparing multi-orifice zeolite material mainly has the methods of zeolitic frameworks removing atom, template agent method.Wherein zeolitic frameworks
Middle abjection atom refers to that this sloughs the silicon atom or aluminium atom in share price using vapor, acid etching, alkaline etching etc..This method is fitted
It is wide with property, but be largely lost in using the zeolite micropore of the post processings such as vapor soda acid, crystallinity declines, skeleton defect increases.
Using template method porous zeotile refer to add in zeolite building-up process carbon black, activated carbon or surfactant,
The templates such as polymer, template is removed after zeolite synthesizes and can be obtained by porous zeotile.But use template
Prepared by method then can not really realize industrialized production due to high costs.
The content of the invention
The present invention prepares problems existing for porous zeotile to solve prior art, there is provided one kind synthesis has
The method of the Chabazite zeolite molecular sieves of multi-stage artery structure.
The present invention is achieved by the following technical solutions：A kind of Chabazite boilings synthesized with multi-stage artery structure
The method of stone molecular sieve, comprises the following steps：
(i) the synthesis of crystal seed
(1) the preparation of potassium metaaluminate
The mixture of distilled water, potassium hydroxide, aluminium hydroxide is heated to 343-363K and remains that the amount of distilled water is constant,
Until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) the preparation of CHA crystal seeds
By step (i)-(1) the potassium metaaluminate solution of middle gained mixed with water, be subsequently added into Ludox, stirring is until mixture becomes
Uniform shape, add Sr (NO3)210min is persistently stirred, mixture is transferred in the autoclave of polytetrafluoroethyllining lining,
423K reacts 5 days, after the completion for the treatment of crystallization, is repeatedly washed, filtered with distilled water, obtaining white powder after vacuum drying 5h under 423K
As crystal seed；
(ii) CHA synthesis
(1) the preparation of potassium metaaluminate
The mixture of distilled water, potassium hydroxide, aluminium hydroxide is heated to 343-363K and remains that the amount of distilled water is constant,
Until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) charging and aging
By step (ii)-(1) the potassium metaaluminate solution of middle gained mixed with water, be subsequently added into Ludox, after stirring until mixture become
Into uniform shape, Sr (NO are eventually adding3)2Lasting stirring, the aging 6-12h at a temperature of 293K-323K, forms gel；
(3) zeolite crystallization
Added in gel step (i)-(2) in after prepared crystal seed stirs 1 hour, mixture is transferred to polytetrafluoroethyllining lining
In autoclave, reaction temperature 393-423K, reaction time 6-12h, treat crystallization completion repeatedly washed, filtered with distilled water,
White powder i.e. Chabazite zeolite molecular sieves are obtained after being dried in vacuo 5h under 423K.
As the further improvement of technical solution of the present invention, step (i)-(1) with step (ii)-(1) middle distilled water, potassium hydroxide,
The mol ratio of aluminium hydroxide is 16.32:1.84:1.
As the further improvement of technical solution of the present invention, the amount of the material of Ludox is with SiO2Meter, step (i)-(2) with step
Suddenly (ii)-(2) middle Ludox, the mol ratio of strontium nitrate are 65-95：1.
Further improvement as technical solution of the present invention, it is preferred that step (i)-(2) with step (ii)-(2) middle Ludox, nitre
The mol ratio of sour strontium is 83：1.
As the further improvement of technical solution of the present invention, the amount of the material of potassium metaaluminate is with Al2O3Meter, the thing of Ludox
The amount of matter is with SiO2Meter, step (i)-(2) with step (ii)-(2) the mol ratio of middle potassium metaaluminate, water and Ludox be 0.14-
0.25：14：1.
Further improvement as technical solution of the present invention, it is preferred that step (i)-(2) with step (ii)-(2) middle potassium metaaluminate,
The mol ratio of water and Ludox is 0.17：14：1.
As the further improvement of technical solution of the present invention, step (ii)-(3) in the quality of crystal seed that is added be gelling
0.2 wt%-1wt% of amount.
Further improvement as technical solution of the present invention, it is preferred that step (ii)-(3) in the quality of crystal seed that is added be
The 0.5wt% of gel quality.
Further improvement as technical solution of the present invention, it is preferred that step (ii)-(3) middle reaction temperature 413K, reaction when
Between 8h.
Further improvement as technical solution of the present invention, it is preferred that step (ii)-(2) middle aging temperature be 303K, aging
Time is 8 hours.
A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure of the present invention, in zeolite
The Chabazite zeolite seed crystals of preparation are added in the gel of synthesis to synthesize the Chabazite zeolites of multi-stage porous.Solves micropore
Chabazite zeolite molecular sieves duct is narrow and small, and mass transfer rate is slow, the low shortcoming of gas absorption amount, in catalysis, absorption and separation etc.
Aspect has critically important practical value.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the XRD diffraction patterns for the Chabazite zeolite molecular sieves that embodiment 1 is prepared.
Fig. 2 is the 77K nitrogen adsorption isotherm figures for the Chabazite zeolite molecular sieves that embodiment 1 is prepared.The absorption
Curve belongs to IV type thermoisopleth, in 0.7 P0-1.0P0There is hysteresis loop, show to include slit-type in synthesized zeolitic material
It is mesoporous.
Fig. 3 is the graph of pore diameter distribution for the Chabazite zeolite molecular sieves that embodiment 1 is prepared.Can from the figure
Go out, the mesoporous of the zeolitic material of synthesized zeolite is mainly distributed on 40 and 60.
Fig. 4 is the 298K carbon dioxide adsorption thermoisopleths for the Chabazite zeolite molecular sieves that embodiment 1 is prepared.
Fig. 5 is the SEM figures for the Chabazite zeolite molecular sieves that embodiment 1 is prepared.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical scheme will be carried out below
Detailed description.Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are resulting on the premise of creative work is not made to be owned
Other embodiment, belong to the scope that the present invention is protected.
Embodiment 1
A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure, comprises the following steps：
(i) the synthesis of crystal seed
(1) the preparation of potassium metaaluminate
By 20g（1.11mol）Distilled water, 7g（0.125mol）Potassium hydroxide, 5.3g（0.068mol）The mixture of aluminium hydroxide
It is heated to 353K and remains that the amount of distilled water is constant, until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) the preparation of CHA crystal seeds
By step (i)-the 2ml potassium metaaluminate solution of (1) middle gained（With Al2O3Meter, 0.0034mol）With 5ml（0.28mol）Water mixes
Close, be subsequently added into 3ml（0.02mol）Ludox, stirring become uniform shape up to mixture, add 0.05g
（0.00024mol）Sr(NO3)210min is persistently stirred, mixture is transferred in the autoclave of polytetrafluoroethyllining lining,
423K reacts 5 days, after the completion for the treatment of crystallization, is repeatedly washed, filtered with distilled water, obtaining white powder after vacuum drying 5h under 423K
As crystal seed；
(ii) CHA synthesis
(1) the preparation of potassium metaaluminate
By 20g（1.11mol）Distilled water, 7g（0.125mol）Potassium hydroxide, 5.3g（0.068mol）The mixture of aluminium hydroxide
It is heated to 353K and remains that the amount of distilled water is constant, until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) charging and aging
By step (ii)-(1) the 2ml potassium metaaluminates solution of middle gained mixed with 5ml water, be subsequently added into 3ml Ludox, it is straight after stirring
Become uniform shape to mixture, be eventually adding 0.05g（0.00024mol）Sr(NO3)2Lasting stirring, the aging at a temperature of 303K
8h, form gel；
(3) zeolite crystallization
Added in gel step (i)-(2) in after prepared crystal seed stirs 1 hour, step (ii)-(3) in the matter of crystal seed that is added
Measure as the 0.5wt% of gel quality, mixture is transferred in the autoclave of polytetrafluoroethyllining lining, it is reaction temperature 423K, anti-
8h between seasonable, repeatedly washed after crystallization completion, filtered with distilled water, be dried in vacuo 5h under 423K after obtain white powder i.e.
Chabazite zeolite molecular sieves.
The specific surface area and pore volume for the Chabazite zeolite molecular sieves that the embodiment 1 of table 1 is prepared
| D-R specific surface areas | BET specific surface area | Langmuir specific surface areas | Micropore volume | Mesoporous pore volume |
| 601.68m2/g | 36.14m3/g m1/g | 51.23m2/g | 0.21cm3/g | 0.11cm3/g |
As shown in Table 1：The pore volume of synthesized zeolitic material intermediary hole accounts for the 34% of total pore volume, is a kind of zeolite material of multi-stage porous
Material.
Embodiment 2
A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure, comprises the following steps：
(i) the synthesis of crystal seed
(1) the preparation of potassium metaaluminate
By 20g（1.11mol）Distilled water, 7g（0.125mol）Potassium hydroxide, 5.3g（0.068mol）The mixture of aluminium hydroxide
It is heated to 343K and remains that the amount of distilled water is constant, until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) the preparation of CHA crystal seeds
By step (i)-the 1.3ml potassium metaaluminate solution of (1) middle gained（With Al2O3Meter, 0.0022mol）With 4ml（0.0.22mol）
Water mixes, and is subsequently added into 2.34ml（0.0156mol）Ludox, stirring become uniform shape up to mixture, add 0.05g
（0.00024mol）Sr(NO3)210min is persistently stirred, mixture is transferred in the autoclave of polytetrafluoroethyllining lining,
423K reacts 5 days, after the completion for the treatment of crystallization, is repeatedly washed, filtered with distilled water, obtaining white powder after vacuum drying 5h under 423K
As crystal seed；
(ii) CHA synthesis
(1) the preparation of potassium metaaluminate
By 20g（1.11mol）Distilled water, 7g（0.125mol）Potassium hydroxide, 5.3g（0.068mol）The mixture of aluminium hydroxide
It is heated to 353K and remains that the amount of distilled water is constant, until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) charging and aging
By step (ii)-(1) middle gained 1.3ml potassium metaaluminate solution（With Al2O3Meter, 0.0022mol）With 4ml（0.0.22mol）Water
Mixing, is subsequently added into 2.34ml（0.0156mol）Ludox, stirring become uniform shape up to mixture, add 0.05g
（0.00024mol）Sr(NO3)2Lasting stirring, the aging 12h at a temperature of 293K, forms gel；
(3) zeolite crystallization
Added in gel step (i)-(2) in after prepared crystal seed stirs 1 hour, step (ii)-(3) in the matter of crystal seed that is added
Measure as the 1wt% of gel quality, mixture is transferred in the autoclave of polytetrafluoroethyllining lining, reaction temperature 403K, reaction
Time 6h, repeatedly washed after crystallization completion, filtered with distilled water, be dried in vacuo 5h under 423K after obtain white powder i.e.
Chabazite zeolite molecular sieves.
Embodiment 3
A kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure, comprises the following steps：
(i) the synthesis of crystal seed
(1) the preparation of potassium metaaluminate
By 20g（1.11mol）Distilled water, 7g（0.125mol）Potassium hydroxide, 5.3g（0.068mol）The mixture of aluminium hydroxide
It is heated to 363K and remains that the amount of distilled water is constant, until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) the preparation of CHA crystal seeds
By step (i)-the 3.35ml potassium metaaluminates solution and 5.76ml of (1) middle gained（0.32mol）Water mixes, and is subsequently added into
3.42ml（0.023mol）Ludox, stirring become uniform shape up to mixture, add 0.05g（0.00024mol）Sr
(NO3)210min is persistently stirred, mixture is transferred in the autoclave of polytetrafluoroethyllining lining, 423K reacts 5 days, treats crystalline substance
It is crystal seed after the completion of change, repeatedly to be washed, filtered with distilled water, obtaining white powder after vacuum drying 5h under 423K；
(ii) CHA synthesis
(1) the preparation of potassium metaaluminate
By 20g（1.11mol）Distilled water, 7g（0.125mol）Potassium hydroxide, 5.3g（0.068mol）The mixture of aluminium hydroxide
It is heated to 353K and remains that the amount of distilled water is constant, until solution becomes as clear as crystal, room temperature cooling is stand-by；
(2) charging and aging
By step (ii)-the 3.35ml potassium metaaluminates solution and 5.76ml of (1) middle gained（0.32mol）Water mixes, and is subsequently added into
3.42ml（0.023mol）Ludox, stirring become uniform shape up to mixture, add 0.05g（0.00024mol）Sr
(NO3)2Lasting stirring, the aging 6h at a temperature of 323K, forms gel；
(3) zeolite crystallization
Added in gel step (i)-(2) in after prepared crystal seed stirs 1 hour, step (ii)-(3) in the matter of crystal seed that is added
Measure as the 0.2wt% of gel quality, mixture is transferred in the autoclave of polytetrafluoroethyllining lining, it is reaction temperature 393K, anti-
12h between seasonable, repeatedly washed after crystallization completion, filtered with distilled water, be dried in vacuo 5h under 423K after obtain white powder i.e.
Chabazite zeolite molecular sieves.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
- A kind of 1. method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure, it is characterised in that including as follows Step：(i) the synthesis of crystal seed(1) the preparation of potassium metaaluminateThe mixture of distilled water, potassium hydroxide, aluminium hydroxide is heated to 343-363K and remains that the amount of distilled water is constant, Until solution becomes as clear as crystal, room temperature cooling is stand-by；(2) the preparation of CHA crystal seedsBy step (i)-(1) the potassium metaaluminate solution of middle gained mixed with water, be subsequently added into Ludox, stirring is until mixture becomes Uniform shape, add Sr (NO3)210min is persistently stirred, mixture is transferred in the autoclave of polytetrafluoroethyllining lining, 423K reacts 5 days, after the completion for the treatment of crystallization, is repeatedly washed, filtered with distilled water, obtaining white powder after vacuum drying 5h under 423K As crystal seed；(ii) CHA synthesis(1) the preparation of potassium metaaluminateThe mixture of distilled water, potassium hydroxide, aluminium hydroxide is heated to 343-363K and remains that the amount of distilled water is constant, Until solution becomes as clear as crystal, room temperature cooling is stand-by；(2) charging and agingBy step (ii)-(1) the potassium metaaluminate solution of middle gained mixed with water, be subsequently added into Ludox, after stirring until mixture become Into uniform shape, Sr (NO are eventually adding3)2Lasting stirring, the aging 6-12h at a temperature of 293K-323K, forms gel；(3) zeolite crystallizationAdded in gel step (i)-(2) in after prepared crystal seed stirs 1 hour, mixture is transferred to polytetrafluoroethyllining lining In autoclave, reaction temperature 393-423K, reaction time 6-12h, treat crystallization completion repeatedly washed, filtered with distilled water, White powder i.e. Chabazite zeolite molecular sieves are obtained after being dried in vacuo 5h under 423K.
- 2. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 1, Characterized in that, step (i)-(1) with step (ii)-(1) middle distilled water, potassium hydroxide, aluminium hydroxide mol ratio be 16.32: 1.84:1。
- 3. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 1, Characterized in that, the amount of the material of Ludox is with SiO2Meter, step (i)-(2) with step (ii)-mole of (2) middle Ludox, strontium nitrate Than being 65-95：1.
- 4. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 3, Characterized in that, preferable, step (i)-(2) with step (ii)-(2) middle Ludox, strontium nitrate mol ratio be 83：1.
- 5. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 1, Characterized in that, the amount of the material of potassium metaaluminate is with Al2O3Meter, the amount of the material of Ludox is with SiO2Meter, step (i)-(2) with step Suddenly (ii)-(2) the mol ratio of middle potassium metaaluminate, water and Ludox be 0.14-0.25：14：1.
- 6. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 5, Characterized in that, preferable, step (i)-(2) with step (ii)-(2) the mol ratio of middle potassium metaaluminate, water and Ludox be 0.17： 14：1.
- 7. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 1, Characterized in that, step (ii)-(3) in the quality of crystal seed that is added be gel quality 0.2 wt%-1wt%.
- 8. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 7, Characterized in that, preferable, step (ii)-(3) in the quality of crystal seed that is added be gel quality 0.5wt%.
- 9. a kind of method for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 1, Characterized in that, preferable, step (ii)-(3) middle reaction temperature 413K, reaction time 8h.
- A kind of 10. side for synthesizing the Chabazite zeolite molecular sieves with multi-stage artery structure according to claim 1 Method, it is characterised in that it is preferable, step (ii)-(2) middle aging temperature be 303K, ageing time is 8 hours.
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Cited By (2)
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| US11247911B2 (en) | 2018-05-03 | 2022-02-15 | Sabic Global Technologies B.V. | SDA-free synthesis of chabazite (CHA) zeolite and uses thereof |
| US20220266228A1 (en) * | 2019-08-02 | 2022-08-25 | Basf Corporation | Chabazite synthesis method including organic and inorganic structure directing agents and chabazite zeolite with flake-like morphology |
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| CN101492168A (en) * | 2009-03-09 | 2009-07-29 | 广东工业大学 | Method of manufacturing kalium-strontium modified silicon-zirconium molecular sieve |
| CN102378739A (en) * | 2009-04-02 | 2012-03-14 | 雪佛龙美国公司 | Method for preparing cha-type molecular sieves using novel structure directing agents |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11247911B2 (en) | 2018-05-03 | 2022-02-15 | Sabic Global Technologies B.V. | SDA-free synthesis of chabazite (CHA) zeolite and uses thereof |
| US20220266228A1 (en) * | 2019-08-02 | 2022-08-25 | Basf Corporation | Chabazite synthesis method including organic and inorganic structure directing agents and chabazite zeolite with flake-like morphology |
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