CN108751221A - The method of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary - Google Patents
The method of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary Download PDFInfo
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- CN108751221A CN108751221A CN201810413258.2A CN201810413258A CN108751221A CN 108751221 A CN108751221 A CN 108751221A CN 201810413258 A CN201810413258 A CN 201810413258A CN 108751221 A CN108751221 A CN 108751221A
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- 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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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- 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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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Abstract
It is standby that the present invention relates to system with molecular sieve for preparing, it is desirable to provide the method for the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary.The method of this kind of floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieve of crystal seed auxiliary includes step：Water, alkali source, organic formwork agent, silicon source, the sources R and crystal seed are respectively placed in beaker, stirs evenly, is subsequently placed in reaction kettle, in 100~200 DEG C of crystallization 2h~10d, product filters, dries to get to Silicon-rich SSZ-13 zeolite molecular sieve original powders.Silicon-rich SSZ-13 zeolite molecular sieves prepared by the present invention, not only maintain good crystallinity and purity, have good catalytic reaction activity, and entire production process does not use the fluorine species of high poison, which reduces unnecessary losses in process of production.
Description
Technical field
The present invention relates to molecular sieve preparation fields, the more particularly to floride-free synthesis Silicon-rich SSZ-13 zeolite molecules of crystal seed auxiliary
The method of sieve.
Background technology
SSZ-13 zeolite molecular sieves are the silica-rich zeolites with three-dimensional octatomic ring pore passage structure, in NH3- SCR, MTO and A
It is had a wide range of applications during gas separation etc..
United States Patent (USP) US 4544538 makes public for the first time a kind of synthetic method of sial SSZ-13 zeolite molecular sieves.It uses
Organic formwork agent is N, N, N- trimethyl -1- adamantane ammoniums, and then the organic formworks such as choline chloride and benzyltrimethylammon.um
Agent is successfully applied in the building-up process of the zeolite molecular sieve.But these synthesis all carry out under alkaline condition, and
And the SSZ-13 zeolite molecular sieves of Silicon-rich cannot be obtained.Camblor professors seminar passes through under fluorine ion system condition for the first time
Control water has successfully synthesized total silicon SSZ-13 zeolite molecular sieves, but fluorine ion toxicity is big, is unfavorable for application.
Recently, Fan Wei professors seminar has synthesized total silicon SSZ-13 in non-fluorine system for the first time under conditions of Dry gel conversion method
A large amount of N is added in zeolite molecular sieve in synthesis, and N, N- trimethyls -1- adamantane ammonium is to form the template body of high concentration
System is the key that this total silicon SSZ-13 zeolite molecular sieves of synthesis.But this large amount of N of addition, N, N- trimethyl -1- adamantane
The method of ammonium considerably increases the synthesis cost of total silicon SSZ-13 zeolite molecular sieves.Obtained by this synthetic method of what is more important
To total silicon SSZ-13 zeolite molecules sieve structure its structure can be caused largely to cave in high-temperature roasting.
Invention content
It is a primary object of the present invention to overcome deficiency in the prior art, under the conditions of a kind of low template agent content is provided,
The method that Silicon-rich SSZ-13 zeolite molecular sieves are synthesized under non-fluorine system by crystal seed auxiliary.In order to solve the above technical problems, this
The solution of invention is：
A kind of method of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary is provided, following step is specifically included：
Water, alkali source, organic formwork agent, silicon source, the sources R and crystal seed are respectively placed in beaker, stirred evenly, is subsequently placed in anti-
It answers in kettle, in 100~200 DEG C of crystallization 2h~10d, product filters, dries to get to Silicon-rich SSZ-13 zeolite molecular sieve original powders
(Silicon-rich SSZ-13 zeolite molecular sieve original powders include total silicon, containing aluminium, boracic, iron content, containing gallium, titaniferous or stanniferous silicon substrate SSZ-13
Zeolite molecular sieve original powder)；
The alkali source uses sodium hydroxide；
The organic formwork agent refers to the N that mass concentration is 25%, N, and N- trimethyl -1- adamantyl quaternary ammonium salts are water-soluble
Liquid, and remember N, N, N- trimethyl -1- adamantyl quaternary ammonium salts are TMdaOH；
The silicon source uses solid silicone or Ludox, and (Ludox specifically uses mass concentration water-soluble for 30% Ludox
Liquid)；
The sources R refer to silicon source, boron source, source of iron, gallium source, titanium source or tin source；Silicon source uses aluminum sulfate or sodium metaaluminate, boron
Source uses boric acid, source of iron that ferric nitrate, gallium source is used to use gallium oxide, titanium source that butyl titanate, tin source is used to use butter of tin；
The crystal seed uses total silicon SSZ-13 zeolite molecular sieve crystal seeds；
Wherein, work as R2O3Refer to Al2O3、B2O3、Fe2O3Or Ga2O3When, each reaction raw materials additive amount meets molar ratio range：
H2O:SiO2:R2O3:Na2O:TMdaOH=5~15:1:0~0.01:0.05~0.5:0.02~0.2；Work as RO2Refer to TiO2Or
SnO2When, each reaction raw materials additive amount meets molar ratio range：H2O:SiO2:RO2:Na2O:TMdaOH=5~15:1:0~
0.01:0.05~0.5:0.02~0.2；The additive amount and SiO of crystal seed2Mass ratio be 1~10%.
In the present invention, the N, N, N- trimethyl -1- adamantyl quaternary ammonium salts use N, N, N- trimethyl -1- adamantane
Ammonium hydroxide.
Compared with prior art, the beneficial effects of the invention are as follows：
1, Silicon-rich SSZ-13 zeolite molecular sieves prepared by the present invention, not only maintain good crystallinity and purity, have
Good catalytic reaction activity, and entire production process does not use the fluorine species of high poison, and which reduces producing
Unnecessary loss in journey.
2, the present invention makes zeolite molecular sieve skeleton structure stablize by roasting, and thermal stability is good.
3, inorganic raw material of the present invention is environmentally friendly, and price is less expensive, and since template usage amount is few,
Synthesis cost is greatly reduced, thus the present invention is of great significance in practical chemical production field.
Description of the drawings
Fig. 1 is the XRD spectra of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary.
Fig. 2 is the stereoscan photograph (low power) of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary.
Fig. 3 is the stereoscan photograph (high power) of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary.
Specific implementation mode
Present invention is further described in detail with specific implementation mode below in conjunction with the accompanying drawings：
The following examples can make the professional technician of this profession that the present invention be more fully understood, but not with any side
The formula limitation present invention.
Embodiment 1：Synthesize total silicon SSZ-13 zeolite molecular sieve crystal seeds
First, N, the N that the mass concentration for the Ludox that 12.13g mass concentrations are 30% being added drop-wise to 37.12g is 25%,
N- trimethyls -1- adamantane ammonium hydroxide (TMdaOH) aqueous solution stirs evenly and second alcohol and water is allowed to volatilize so that system
H2O/SiO2=3, the aqueous solution for the hydrofluoric acid that 1.33g mass concentrations are 45% is then added, and stir evenly.In 150 DEG C of crystallization
2d, that is, complete crystallization, product filter, and product is obtained after drying.The proportioning of reaction raw materials is as follows：H2O:SiO2:HF:TMdaOH=3:
1:0.5:0.5。
Embodiment 2：The floride-free synthesis total silicon SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 2.0g H2The N that O, 0.2g NaOH, 4g mass concentration are 25%, N, N- trimethyl -1- adamantane hydrogen-oxygens
Change ammonium (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir evenly, then by this gel
It is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters, and product is obtained after drying.Instead
Answer the proportioning of raw material as follows：H2O:SiO2:Na2O:TMdaOH=8:1:0.07:0.14.
It is the curve a in total silicon SSZ-13 zeolite molecular sieves such as Fig. 1, bone after roasting through its structure of X-ray diffraction analysis
Curve b in frame stable structure such as Fig. 1, and can be seen that uniform morphology is presented in synthesized product by stereoscan photograph
(low power), and the pattern of product is the cube (high power) of little crystal grain.Fig. 2, Fig. 3 are that crystal seed assists sweeping for floride-free sintetics
Retouch electromicroscopic photograph (SEM).
Embodiment 3：The floride-free high―temperature nuclei total silicon SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 0.14g NaOH, the N that 5.7g mass concentrations are 25%, N, N- trimethyl -1- adamantane ammonium hydroxide
(TMdaOH) aqueous solution, 2g solid silicones and 0.2g (10%) crystal seed are placed in beaker and stir evenly, and then add this gel
Enter in polytetrafluoroethylene (PTFE) stainless steel cauldron, 200 DEG C of crystallization 2h, that is, complete crystallizations, product filters, and product is obtained after drying.Reaction
The proportioning of raw material is as follows：H2O:SiO2:Na2O:TMdaOH=5:1:0.05:0.2.
Embodiment 4：The floride-free high―temperature nuclei total silicon SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 4.2g H2The N that O, 1.4g NaOH, 0.57g mass concentration are 25%, N, N- trimethyl -1- adamantane
Ammonium hydroxide (TMdaOH) aqueous solution, 6.64g Ludox and 0.02g (1%) crystal seed are placed in beaker and stir evenly, and then will
This gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 100 DEG C of crystallization 10d, that is, complete crystallizations, and product filters, and is obtained after drying
Product.The proportioning of reaction raw materials is as follows：H2O:SiO2:Na2O:TMdaOH=15:1:0.5:0.02.
Embodiment 5：The floride-free synthesizing high-silicon aluminium ratio SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 2.0g H2O,0.18g NaOH,0.078g NaAlO2, the N that 4g mass concentrations are 25%, N, N- front threes
Base -1- adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir
It is even, then this gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters, and dries
Product is obtained after dry.The proportioning of reaction raw materials is as follows：H2O:SiO2:Al2O3:Na2O:TMdaOH=8:1:0.01:0.07:0.14.
Embodiment 6：The floride-free synthesizing high-silicon aluminium ratio SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 2.0g H2O,0.2g NaOH,0.11g Al2(SO4)3·18H2N, the N that O, 4g mass concentration are 25%,
N- trimethyls -1- adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker
It stirs evenly, then this gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product
It filters, product is obtained after drying.The proportioning of reaction raw materials is as follows：H2O:SiO2:Al2O3:Na2O:TMdaOH=8:1:0.005:
0.07:0.14。
Embodiment 7：The floride-free synthesis boracic SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 2.0g H2O,0.2g NaOH,0.01g H3BO3, the N that 4g mass concentrations are 25%, N, N- trimethyls-
1- adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir evenly,
Then this gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters, drying
After obtain product.The proportioning of reaction raw materials is as follows：H2O:SiO2:B2O3:Na2O:TMdaOH=8:1:0.005:0.07:0.14.
Embodiment 8：The floride-free synthesis iron content SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 2.0g H2O, 0.2g NaOH, 0.13g ferric nitrate, the N that 4g mass concentrations are 25%, N, N- trimethyls-
1- adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir evenly,
Then this gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters, drying
After obtain product.The proportioning of reaction raw materials is as follows：H2O:SiO2:Fe2O3:Na2O:TMdaOH=8:1:0.005:0.07:0.14.
Embodiment 9：The floride-free synthesis zeolite molecular sieves of SSZ-13 containing gallium of crystal seed auxiliary
First, by 2.0g H2O,0.2g NaOH,0.03g Ga2O3, the N that 4g mass concentrations are 25%, N, N- trimethyls-
1- adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir evenly,
Then this gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters, drying
After obtain product.The proportioning of reaction raw materials is as follows：H2O:SiO2:Ga2O3:Na2O:TMdaOH=8:1:0.005:0.07:0.14.
Embodiment 10：The floride-free synthesizing titanium-containing SSZ-13 zeolite molecular sieves of crystal seed auxiliary
First, by 2.0g H2O, 0.2g NaOH, 0.11g butyl titanate, the N, N, N- tri- that 4g mass concentrations are 25%
Methyl-1-adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir
Uniformly, then this gel being added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters,
Product is obtained after drying.The proportioning of reaction raw materials is as follows：H2O:SiO2:TiO2:Na2O:TMdaOH=8:1:0.005:0.07:
0.14。
Embodiment 11：Crystal seed auxiliary is floride-free to synthesize stanniferous SSZ-13 zeolite molecular sieves
First, by 2.0g H2O, 0.2g NaOH, 0.087g butter of tin, the N that 4g mass concentrations are 25%, N, N- front threes
Base -1- adamantane ammonium hydroxide (TMdaOH) aqueous solution, 2g solid silicones and 0.1g (5%) crystal seed are placed in beaker and stir
It is even, then this gel is added in polytetrafluoroethylene (PTFE) stainless steel cauldron, 160 DEG C of crystallization 1d, that is, complete crystallizations, product filters, and dries
Product is obtained after dry.The proportioning of reaction raw materials is as follows：H2O:SiO2:SnO2:Na2O:TMdaOH=8:1:0.005:0.07:
0.14。
The above is only several case study on implementation of the present invention, not does limitation in any form to the present invention,
Although the present invention is disclosed as above with preferable case study on implementation, however, it is not intended to limit the invention, any skill for being familiar with this profession
Art personnel, without departing from the scope of the present invention, when structure and technology contents using the disclosure above make it is a little
Change or be modified to the equivalence enforcement cases of equivalent variations.But every content without departing from technical solution of the present invention, foundation
The technical spirit of the present invention still belongs to the present invention to any simple modification, equivalent change and modification made by the above case study on implementation
In technical proposal scope.
Claims (2)
1. a kind of method of the floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary, which is characterized in that specifically include following
Step：
Water, alkali source, organic formwork agent, silicon source, the sources R and crystal seed are respectively placed in beaker, stirs evenly, is subsequently placed in reaction kettle
In, in 100~200 DEG C of crystallization 2h~10d, product filters, dries to get to Silicon-rich SSZ-13 zeolite molecular sieve original powders；
The alkali source uses sodium hydroxide；
The organic formwork agent refer to mass concentration be 25% N, N, N- trimethyl -1- adamantyl quaternary ammonium salt aqueous solutions, and
Remember that N, N, N- trimethyl -1- adamantyl quaternary ammonium salts are TMdaOH；
The silicon source uses solid silicone or Ludox；
The sources R refer to silicon source, boron source, source of iron, gallium source, titanium source or tin source；Silicon source uses aluminum sulfate or sodium metaaluminate, boron source to adopt
With boric acid, source of iron uses ferric nitrate, gallium source to use gallium oxide, titanium source that butyl titanate, tin source is used to use butter of tin；
The crystal seed uses total silicon SSZ-13 zeolite molecular sieve crystal seeds；
Wherein, work as R2O3Refer to Al2O3、B2O3、Fe2O3Or Ga2O3When, each reaction raw materials additive amount meets molar ratio range：H2O:
SiO2:R2O3:Na2O:TMdaOH=5~15:1:0~0.01:0.05~0.5:0.02~0.2；Work as RO2Refer to TiO2Or SnO2
When, each reaction raw materials additive amount meets molar ratio range：H2O:SiO2:RO2:Na2O:TMdaOH=5~15:1:0~0.01:
0.05~0.5:0.02~0.2；The additive amount and SiO of crystal seed2Mass ratio be 1~10%.
2. a kind of method of floride-free synthesis Silicon-rich SSZ-13 zeolite molecular sieves of crystal seed auxiliary according to claim 1, special
Sign is that the N, N, N- trimethyl -1- adamantyl quaternary ammonium salts use N, N, N- trimethyl -1- adamantane ammonium hydroxide.
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| CN110040743A (en) * | 2019-04-25 | 2019-07-23 | 太原理工大学 | A kind of coal ash for manufacturing for SSZ-13 molecular sieve method |
| CN110240175A (en) * | 2019-07-16 | 2019-09-17 | 吉林大学 | A kind of method of hydro-thermal free-floride synthesis pure silicon CHA molecular sieve |
| CN110357121A (en) * | 2019-08-02 | 2019-10-22 | 太原理工大学 | A kind of preparation method of little crystal grain nanometer hierarchical pore SSZ-13 molecular sieve |
| CN110950355A (en) * | 2019-11-18 | 2020-04-03 | 复旦大学 | Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity |
| CN110950356A (en) * | 2019-12-12 | 2020-04-03 | 吉林大学 | Preparation method of CHA type molecular sieve |
| CN114920265A (en) * | 2022-05-26 | 2022-08-19 | 嘉兴学院 | Method for rapidly preparing all-silicon SSZ-13 zeolite by using guide agent method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110040743A (en) * | 2019-04-25 | 2019-07-23 | 太原理工大学 | A kind of coal ash for manufacturing for SSZ-13 molecular sieve method |
| CN110240175A (en) * | 2019-07-16 | 2019-09-17 | 吉林大学 | A kind of method of hydro-thermal free-floride synthesis pure silicon CHA molecular sieve |
| CN110357121A (en) * | 2019-08-02 | 2019-10-22 | 太原理工大学 | A kind of preparation method of little crystal grain nanometer hierarchical pore SSZ-13 molecular sieve |
| CN110357121B (en) * | 2019-08-02 | 2022-09-09 | 太原理工大学 | Preparation method of small-grain nano hierarchical pore SSZ-13 molecular sieve |
| CN110950355A (en) * | 2019-11-18 | 2020-04-03 | 复旦大学 | Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity |
| CN110950355B (en) * | 2019-11-18 | 2022-10-11 | 复旦大学 | Preparation method of W-SSZ-13 zeolite with high crystallinity and high hydrophobicity |
| CN110950356A (en) * | 2019-12-12 | 2020-04-03 | 吉林大学 | Preparation method of CHA type molecular sieve |
| CN114920265A (en) * | 2022-05-26 | 2022-08-19 | 嘉兴学院 | Method for rapidly preparing all-silicon SSZ-13 zeolite by using guide agent method |
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