CN106542540B - The method for synthesizing ERS-7 zeolite molecular sieves with line style polyquaternium organic formwork - Google Patents
The method for synthesizing ERS-7 zeolite molecular sieves with line style polyquaternium organic formwork Download PDFInfo
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- CN106542540B CN106542540B CN201610936682.6A CN201610936682A CN106542540B CN 106542540 B CN106542540 B CN 106542540B CN 201610936682 A CN201610936682 A CN 201610936682A CN 106542540 B CN106542540 B CN 106542540B
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- 239000010457 zeolite Substances 0.000 title claims abstract description 30
- 238000009415 formwork Methods 0.000 title claims abstract description 25
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 22
- 229920000289 Polyquaternium Polymers 0.000 title claims abstract description 21
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 11
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 18
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229910001388 sodium aluminate Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The present invention relates to molecular sieve preparation methods, it is desirable to provide a method of 7 zeolite molecular sieves of ERS are synthesized with line style polyquaternium organic formwork.Including step：Water, silicon source, silicon source, alkali source and template are mixed, is stirred until homogeneous, is subsequently placed in reaction kettle, the product of crystallization is through filtering, drying to get to the original powder of 7 zeolite molecular sieves of ERS.The present invention can not only greatly simplify the synthesis of organic formwork agent, and synthesize phase region to it and can carry out a wide range of broadening.It greatly reduces the difficulty for synthesizing this product, an excellent basis has been established in the application of product thus.Product maintains good crystallinity and purity, has good catalytic reaction activity, a kind of new thinking is provided for synthetic zeolite.
Description
Technical field
The invention belongs to molecular sieve preparation method, more particularly to a kind of novel line style polyquaternium organic formwork synthesizes ERS-
The method of 7 zeolite molecular sieves.
Background technology
Molecular sieve is widely used in being catalyzed, ion exchange because it has spacious structure and big surface area, inhales
It is attached with detach equal fields.In the synthesis of modern zeolite molecular sieve, zeolite molecular sieve conjunction is greatly facilitated in the use of organic formwork agent
At the development of chemistry.A big class template of the quaternary ammonium salt as synthesis zeolite, has synthesized panoramic zeolite
Structure, such as Beta, ZSM-5, ERS-7 etc..Wherein, ERS-7 is a kind of zeolite of one-dimensional octatomic ring structure, by Millini etc.
People reports for the first time.The synthesis of usual ERS-7 needs to use N, this organic formwork agent of N- dimethyl hydrogen oxyl ammoniums, in zeolite
Template process complexity (needing ion exchange at hydrogen-oxygen type) is not only synthesized in preparation process, but also synthesizes the phase of ERS-7 zeolites
Area is very narrow, and (only feed intake SiO2/Al2O3Pure phase can be just obtained for 25), it is easy to there is the generation of stray crystal.
Therefore, the method that Development of Novel simply synthesizes ERS-7 zeolites, while enabling it to synthesize phase region and widening significantly
It has very important significance.
Invention content
The technical problem to be solved by the present invention is to overcome deficiency in the prior art, provide one kind with line style polyquaternium
The method that organic formwork synthesizes ERS-7 zeolite molecular sieves.
To solve technical problem, solution of the invention is：
A kind of method synthesizing ERS-7 zeolite molecular sieves with line style polyquaternium organic formwork is provided, is included the following steps：
Water, silicon source, silicon source, alkali source and template are mixed, is stirred until homogeneous, is subsequently placed in reaction kettle, 130~
200 DEG C of crystallization 1d~10d, product are filtered, are dried to get to the original powder of ERS-7 zeolite molecular sieves；
The template is line style polyquaternium, and structural formula is shown below：
Controlling the additive amount of each reaction raw materials makes its molar ratio range be：15~50H2O∶SiO2: 0.0025~0.067
Al2O3: 0.1~0.5 (Na2O or K2O): 0.02~0.08 template.
In the present invention, source of aluminium is aluminum sulfate or sodium metaaluminate；Silicon source is the Ludox that dioxide-containing silica is 30%；
Alkali source is potassium hydroxide or sodium hydroxide.
Method the present invention also provides preparation for the line style polyquaternium template of ERS-7 zeolite molecular sieves synthesis,
Including step：Isosorbide-5-Nitrae-dibromobutane and N, N, N are weighed for 1: 1 according to molar ratio, N- tetramethyls-Putriscine are dissolved in second
In alcohol, then 12h is reacted under conditions of 80 DEG C of reflux under stiring；After reaction, ether is added into reaction product, produces
Raw white solid precipitation obtains line style polyquaternium template through filtering, drying.
Compared with prior art, the beneficial effects of the present invention are：
1, the present invention can not only greatly simplify the synthesis of organic formwork agent, and synthesize phase region to it and can carry out very big model
The broadening enclosed.It greatly reduces the difficulty for synthesizing this product, an excellent basis has been established in the application of product thus.
2, compared with prior art, the product that prepared by the present invention maintains good crystallinity and purity, has good
Catalytic reaction activity.
3, come synthesis zeolite, this is provided for synthetic zeolite for the design and exploitation of the invention by organic formwork agent
A kind of new thinking.
Description of the drawings
Fig. 1：The XRD spectra of the ERS-7 zeolites of line style polyquaternium organic formwork agent synthesis.
Fig. 2：The ERS-7 zeolite stereoscan photographs of line style polyquaternium organic formwork agent synthesis.
Specific implementation mode
Embodiment 1：The synthesis of line style polyquaternium organic formwork agent
Molar ratio according to Isosorbide-5-Nitrae-dibromobutane and N, N, N, N- tetramethyls-Putriscine is 1: 1, weighs 10g Isosorbide-5-Nitraes-
Dibromobutane and 15g N, N, N, N- tetramethyl-Putriscines are dissolved in 50ml ethyl alcohol, and setting temperature is 80 DEG C and is returned
Stream stirs 12h, and after reaction, into reaction product, addition ether is precipitated with regard to producible white solid, through filtering, drying
It can be obtained required template.
Embodiment 2：Line style polyquaternium organic formwork agent synthesizes ERS-7 zeolites
By 8.12g H2O, 0.065g NaAlO2, 0.3g NaOH, 0.65g organic formwork agent (T, structure such as Fig. 1) and
The Ludox of 3.32g dioxide-containing silicas 30%, which is placed in beaker, to stir evenly, this gel is then added to polytetrafluoroethylene (PTFE)
In stainless steel cauldron, 160 DEG C of crystallization 5d, that is, complete crystallizations, product filters, and product is obtained after drying.Reaction raw materials are matched such as
Under：
35H2O:SiO2:0.017Al2O3:0.23Na2O:0.04T
Through X-ray diffraction analysis, its structure is to belong to the ERS-7 zeolite molecular sieves (Fig. 1) of ESV, and pass through scanning electricity
Mirror photo can be seen that synthesized product pellet size is higher than more uniform and purity, as shown in Fig. 2.
Embodiment 3：Line style polyquaternium organic formwork agent high―temperature nuclei ERS-7 zeolites
By 12.67g H2O, 0.028g Al2(SO4)3·18H2O, 0.13g NaOH, 0.65g organic formwork agent (T, structure
Such as Fig. 1) and the Ludox of 3.32g dioxide-containing silicas 30% be placed in beaker and stir evenly, then this gel is added to
In polytetrafluoroethylene (PTFE) stainless steel cauldron, 200 DEG C of crystallization 1d, that is, complete crystallizations, product filters, and product is obtained after drying.Reaction is former
The proportioning of material is as follows：
50H2O:SiO2:0.0025Al2O3:0.1Na2O:0.04T
Embodiment 4：Line style polyquaternium organic formwork agent low temperature synthesizes ERS-7 zeolites
By 2.17g H2O, 0.26g NaAlO2, 0.54g NaOH, 0.33g organic formwork agent (T, structure such as Fig. 1) and
The Ludox of 3.32g dioxide-containing silicas 30%, which is placed in beaker, to stir evenly, this gel is then added to polytetrafluoroethylene (PTFE)
In stainless steel cauldron, 130 DEG C of crystallization 10d, that is, complete crystallizations, product filters, and product is obtained after drying.The proportioning of reaction raw materials
It is as follows：
15H2O:SiO2:0.067Al2O3:0.5Na2O:0.02T
Embodiment 5：Line style polyquaternium organic formwork agent synthesizes ERS-7 zeolites
By 8.12g H2O, 0.028g Al2(SO4)3·18H2(T, structure is as schemed for O, 0.35g KOH, 1.3g organic formwork agent
1) and the Ludox of 3.32g dioxide-containing silicas 30% is placed in beaker and stirs evenly, this gel is then added to poly- four
In vinyl fluoride stainless steel cauldron, 160 DEG C of crystallization 5d, that is, complete crystallizations, product filters, and product is obtained after drying.Reaction raw materials
Proportioning is as follows：
35H2O:SiO2:0.025Al2O3:0.16K2O:0.08T
Embodiment 6：Line style polyquaternium organic formwork agent synthesizes ERS-7 zeolites
By 8.12g H2O, 0.065g NaAlO2, 0.6g NaOH, 0.65g organic formwork agent (T, structure such as Fig. 1) and
The Ludox of 3.32g dioxide-containing silicas 30%, which is placed in beaker, to stir evenly, this gel is then added to polytetrafluoroethylene (PTFE)
In stainless steel cauldron, 160 DEG C of crystallization 5d, that is, complete crystallizations, product filters, and product is obtained after drying.Reaction raw materials are matched such as
Under：
35H2O:SiO2:0.017Al2O3:0.47Na2O:0.04T
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 (3)
1. a kind of method synthesizing ERS-7 zeolite molecular sieves with line style polyquaternium organic formwork, which is characterized in that including following
Step：
Water, silicon source, silicon source, alkali source and template are mixed, is stirred until homogeneous, is subsequently placed in reaction kettle, at 130~200 DEG C
Crystallization 1d~10d, product are filtered, are dried to get to the original powder of ERS-7 zeolite molecular sieves；
The template is line style polyquaternium, and structural formula is shown below：
Controlling the additive amount of each reaction raw materials makes its molar ratio range be：15~50H2O∶SiO2: 0.0025~0.067Al2O3∶
0.1~0.5Na2O or K2O: 0.02~0.08 template.
2. according to the method described in claim 1, it is characterized in that, source of aluminium is aluminum sulfate or sodium metaaluminate；Silicon source is two
The Ludox that silica content is 30%；Alkali source is potassium hydroxide or sodium hydroxide.
3. the method for preparing the line style polyquaternium template for the synthesis of ERS-7 zeolite molecular sieves, which is characterized in that including step
Suddenly：Isosorbide-5-Nitrae-dibromobutane and N, N, N are weighed for 1: 1 according to molar ratio, N- tetramethyls-Putriscine dissolve in ethanol, so
Afterwards 12h is reacted under conditions of 80 DEG C of reflux under stiring；After reaction, be added ether into reaction product, generation it is white
Color solid precipitation obtains line style polyquaternium template through filtering, drying.
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