CN105732693A - Bisamide bond long carbon chain organosilane quaternary ammonium compound and preparation and application thereof - Google Patents
Bisamide bond long carbon chain organosilane quaternary ammonium compound and preparation and application thereof Download PDFInfo
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- CN105732693A CN105732693A CN201610196253.XA CN201610196253A CN105732693A CN 105732693 A CN105732693 A CN 105732693A CN 201610196253 A CN201610196253 A CN 201610196253A CN 105732693 A CN105732693 A CN 105732693A
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- 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
- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C01B39/38—Type ZSM-5
- C01B39/40—Type ZSM-5 using at least one organic template directing agent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
Abstract
The invention relates to a bisamide bond long carbon chain organosilane quaternary ammonium compound and preparation and application thereof. A structural formula of the compound is shown in the specification, wherein m is any integer from 1-18, n is any integer from 1-5, X is one of Cl<->, Br<-> and I<->. The preparation is as follows: adding N-methylimino diacetic acid, aliphatic amine, 1-hydroxy benzotriazole HOBT, carbodiimide EDCI and triethylamine in a solvent, stirring at room temperature to stay overnight, and purifying to obtain a bisamide chain intermediate; mixing the bisamide chain intermediate and haloalkyl trimethoxy silane, reacting, cooling, and washing to obtain the compound. The compound is applied to the preparation of a mesoporous ZSM-5 molecular sieve. A hierarchical porous zeolite molecular sieve prepared by the invention is capable of obviously improving the pore volume and specific surface area of the zeolite molecular sieve, and the aperture and pore volume of the hierarchical pores of the molecular sieve can be effectively regulated through the changing of carbon atom number of the diacyl aliphatic chain.
Description
Technical field
The invention belongs to quaternary ammonium compound and preparation thereof and application, particularly to a kind of bisamide bond distance's carbochain
Organosilan quaternary ammonium compound and preparation thereof and application.
Background technology
Zeolite molecular sieve is widely used in petrochemical industry and fine chemistry industry as catalyst, because of the adsorbing separation merit of its uniqueness
Can also be widely used in the field of engineering technology such as ion exchange, adsorbing separation, environmental conservation.But traditional zeolite molecular sieve is many
For micropore (aperture is less than 2nm), such aperture is difficult to be catalyzed the chemical reaction of macromole, and then micro-pore zeolite molecular sieve is greatly
The application of Journal of Molecular Catalysis field is restricted.Especially less and less in current Global Oil resource, in oil, heavy oil content is increasingly
Many, petroleum chemical industry is catalyzed in the urgent need to more wide-aperture catalyst.Also have the most emerging biological medicine, become more meticulous
The fields such as work carry out the chemical reaction of macromole and are also required to the utilization of new macroporous footpath catalyst.In this context, develop mesoporous
Being particularly important with practical of molecular sieve or even large pore molecular sieve.According to the world purely and applied chemistry community (IUPAC)
Classification: the aperture referred to as poromerics less than 2nm, aperture is in the referred to as mesoporous material of 2 to 50nm, aperture being referred to as more than 50nm
Large pore material.
Preparing mesopore molecular sieve and usually need to use template, New Mesoporous Molecular Sieves to be developed will develop new type formwork
Agent, surfactant is as conventional soft template, the research emphasis of still the most current new type formwork agent and focus.In preparation
During mesoporous material, the formation of mesoporous phase is had a significant impact by kind and the character of surfactant, even can change
The route of synthesis of reaction system.Cationic surfactant is a class important in surfactant, its hydrophilic group positively charged.
And the long chain alkyl ammonium salt of low-molecular-weight is the most frequently used cationic surfactant.But use long chain alkyl ammonium salt type
The mesoporous molecular sieve structure that cationic surfactant synthesizes as template is more single, and hole wall is relatively thin, dividing of its synthesis
Son sieve hydrothermal stability is poor, and then to develop novel quaternary cationic surfactant exactly to be solved for these problems
Problem.
Hierarchical zeolite molecular sieve, its duct model is synthesized for template with novel organosilicon quaternary ammonium salt surface active agent
Enclose and include micropore and mesoporous, even macropore.This kind of zeolite molecular sieve containing multistage pore canal is because having the character of its uniqueness with excellent
Gesture, being catalyzed, adsorb, the field such as separation is gathered around and is had wide practical use.
Summary of the invention
The technical problem to be solved is to provide a kind of bisamide bond distance's carbochain organosilan quaternary ammonium salt chemical combination
Thing and preparation thereof and application, the present invention prepares hierarchical zeolite molecular sieve prepared by the present invention can significantly improve zeolite molecular sieve
Pore volume and specific surface area, can the hole of effective Molecular regulator sieve multistage pore canal by changing the carbon atom number of bisamide base chain
Footpath and pore volume, it is also possible to by changing rubbing of quaternary cationics and the silicon source in zeolite molecular sieve synthesis mother liquid
You are than the pattern regulating and controlling hierarchical zeolite molecular sieve.
A kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound of the present invention, described structural formula of compound is:
Wherein, m=1-18 arbitrary integer, n=1-5 arbitrary integer, X-For Cl-、Br-、I-In one.
A kind of preparation method of bisamide bond distance's carbochain organosilan quaternary ammonium compound of the present invention, including:
(1) by N-methyliminodiacetic acid, fatty amine, I-hydroxybenzotriazole HOBT, carbodiimides EDCI, triethylamine
Add in solvent, then stirred overnight at room temperature, purify, obtain bisamide chain intermediate；Wherein N-methylene imine oxalic acid, fat
Amine, the mol ratio of HOBT, EDCI is 1:2.0-3.0:2.0-2.5:2.0-2.5；
(2) above-mentioned bisamide chain intermediate and alkylhalide group trimethoxy silane are mixed, at 90-130 DEG C, react 12-
24h, is cooled to room temperature, washing, obtains bisamide bond distance's carbochain organosilan quaternary ammonium compound；Wherein in the middle of bisamide chain
The mol ratio of body and alkylhalide group trimethoxy silane is 1:1.0-2.0.
In described step (1), fatty amine isWherein any positive integer of m=1-18.
Described step (1) purifies particularly as follows: by saturated sodium bicarbonate, ethyl acetate, use normal hexane weight after ether washing
Crystallization.
In described step (1), solvent is dimethylformamide or oxolane.
In described step (2), the molecular formula of alkylhalide group trimethoxy silane is:Wherein X be Cl,
One in Br, I, n=1-5 arbitrary integer.
A kind of application of bisamide bond distance's carbochain organosilan quaternary ammonium compound of the present invention, it is characterised in that: institute
State bisamide bond distance's carbochain organosilan quaternary ammonium compound for the preparation containing mesoporous ZSM-5 molecular sieve, particularly as follows:
(1), under the conditions of 20-25 DEG C, silicon source, aluminum source and water are mixed to homogeneously, then under the conditions of continuously stirred,
Adding micropore template, be stirred for homogeneously, obtain the mother solution of zeolite molecular sieve synthesis, being subsequently adding bisamide bond distance's carbochain has
Machine organosilane quaternary ammonium salt compounds, stirring 1-3h mixing, obtain mixed system；Wherein silicon source, aluminum source, micropore template, double acyl
Amine bond distance's carbochain organosilan quaternary ammonium compound, the mol ratio of water are 1-100:1:20-48:0.01-8:800-5000；
(2) above-mentioned mixed system is carried out constant temperature stirring, obtain white gels, then carry out crystallization, quenching, sucking filtration, wash
Wash to neutrality, be dried, calcining, obtain hierarchical zeolite molecular sieve containing mesoporous ZSM-5 molecular sieve.
One or more during silicon source is silicate class, sodium silicate crystal, waterglass, Ludox in described step (1)；Aluminum
Source is one or more in sodium metaaluminate, aluminum sulfate, aluminum nitrate, aluminum chloride and aluminum isopropylate.；Micropore template is tetramethyl
One in base ammonium bromide, tetraethylammonium bromide, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide and TPAOH or
Several.In described step (1), speed of agitator is 260-350r/min.
In described step (2), constant temperature stirring is: under the conditions of 20-25 DEG C, speed of agitator is 360-450r/min, mixing time
For 2-3h.Crystallization in described step (2) particularly as follows: containing politef bushing pipe confined reaction autoclave in, 140-170
Crystallization 3-96h at DEG C；It is dried and is: under the conditions of 80-120 DEG C, be dried 10-20h；Calcining calcines 10-15h at 400-600 DEG C.
In described step (2), hierarchical zeolite molecular sieve belongs to MFI type structure Si-Al zeolite.
The BET surface area of described hierarchical zeolite molecular sieve is 200～1000m2g-1, BJH aperture is 2～20nm, hole
Appearance is 0.2～1.0cm3g-1。
The present invention relates to series bisamide bond distance carbochain organosilicone quaternary ammonium salt compounds preparation method and application.Such is changed
Compound, with series fatty amine as raw material, reacts to obtain bisamide chain intermediate, bisamide chain intermediate with N-methylene imine oxalic acid
Target product series bisamide chain organosilicon quaternary ammonium salt is obtained with alkylhalide group trimethoxy silane quaterisation.
The present invention contains the zeolite molecular sieve of multistage pore canal with series bisamide chain organosilicon quaternary ammonium salt for new template agent preparation,
Its multistage pore canal includes micropore, mesoporous, even macropore.This hierarchical zeolite molecular sieve has bigger pore volume and specific surface
Long-pending, pore-size distribution is homogeneous, and its multistage pore canal can be suitably used for different size of Journal of Molecular Catalysis, adsorbs and separate.And also by
Change aperture and the pore volume of the carbon atom number energy effective Molecular regulator sieve multistage pore canal of bisamide bond distance's carbochain, by change
Quaternary cationics regulates and controls multistage pore canal with the mol ratio of the silicon dioxide in zeolite molecular sieve synthesis mother liquid
The pattern of zeolite molecular sieve.
Beneficial effect
Hierarchical zeolite molecular sieve prepared by the present invention can significantly improve pore volume and the specific surface area of zeolite molecular sieve, logical
Cross aperture and the pore volume of the carbon atom number energy effective Molecular regulator sieve multistage pore canal changing bisamide bond distance's carbochain, it is also possible to
Regulate and control multistage by the mol ratio of change quaternary cationics with the silicon source in zeolite molecular sieve synthesis mother liquid
The pattern of duct zeolite molecular sieve；
The zeolite molecular sieve containing multistage pore canal of the present invention because having character and the advantage of its uniqueness, catalysis, absorption,
Separate, biology, medicine and other fields are gathered around and are had wide practical use.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the hierarchical pore MFI structural zeolite molecular sieve that embodiment 4 prepares；
Fig. 2 is that the nitrogen absorption under low temperature-desorption isothermal of the hierarchical pore MFI structural zeolite molecular sieve that embodiment 4 prepares is bent
Line；
Fig. 3 is the graph of pore diameter distribution of the hierarchical pore MFI that embodiment 4 prepares；
Fig. 4 is the scanning electron microscope (SEM) photograph of the hierarchical pore MFI that embodiment 4 prepares；
Fig. 5 is the transmission electron microscope picture of the hierarchical pore MFI that embodiment 4 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
Bisamide chain organosilicone quaternary ammonium salt compounds, its chemical structural formula is:
Wherein X-For I-, n=3, m=12.
Preparation method: be sequentially added into 0.68gN-methyliminodiacetic acid in 150mL there-necked flask, 1.97g tetradecy lamine,
1.225g1-hydroxybenzotriazole (HOBT), 1.773g carbodiimides (EDCI), 1.27mL triethylamine, 100mL DMF room temperature
(25 DEG C) are stirred overnight.50mL saturated sodium bicarbonate solution is poured in there-necked flask reactant liquor, has white solid to separate out, filter
Obtain white solid, wash with 20mL DMF solution every time, wash three times, wash three with 20mL saturated sodium bicarbonate solution afterwards
Secondary, then wash three times by 20mL ethyl acetate, finally washed once with 20mL ether, the white solid obtained uses normal hexane weight again
Crystallization obtains pure intermediate, puts into the midbody product drying pure in vacuum drying oven.
In 50mL round-bottomed flask, add above-mentioned intermediate 0.8g, 3-iodine propyl trimethoxy silicane 0.56g, be slowly heated
To 100 DEG C, react 12h, after reaction terminates, naturally cool to room temperature, wash repeatedly with normal hexane solvent, obtain above-mentioned bisamide chain
Organosilicone quaternary ammonium salt compounds.
Embodiment 2
Bisamide chain organosilicone quaternary ammonium salt compounds, its chemical structural formula is:
Wherein X-For I-, n=3, m=10.
Preparation method: be sequentially added into 0.68gN-methyliminodiacetic acid in 150mL there-necked flask, 1.67g lauryl amine,
1.225g1-hydroxybenzotriazole (HOBT), 1.773g carbodiimides (EDCI), 1.27mL triethylamine, 100mL DMF room temperature
(25 DEG C) are stirred overnight.50mL saturated sodium bicarbonate solution is poured in there-necked flask reactant liquor, has white solid to separate out, filter
Obtain white solid, wash with 20mL DMF solution every time, wash three times, wash three with 20mL saturated sodium bicarbonate solution afterwards
Secondary, then wash three times by 20mL ethyl acetate, finally washed once with 20mL ether, the white solid obtained uses normal hexane weight again
Crystallization obtains pure intermediate, puts into the midbody product drying pure in vacuum drying oven.
In 50mL round-bottomed flask, add above-mentioned intermediate 0.8g, 3-iodine propyl trimethoxy silicane 0.61g, be slowly heated
To 100 DEG C, react 12h, after reaction terminates, naturally cool to room temperature, wash repeatedly with normal hexane solvent, obtain above-mentioned bisamide chain
Organosilicone quaternary ammonium salt compounds.
Embodiment 3
Bisamide chain organosilicone quaternary ammonium salt compounds, its chemical structural formula is:
Wherein X-For I-, n=3, m=8.
Preparation method: be sequentially added into 0.68gN-methyliminodiacetic acid in 150mL there-necked flask, 1.47g ten amine,
1.225g1 hydroxybenzotriazole (HOBT), 1.773g carbodiimides (EDCI), 1.27mL triethylamine, 100mL DMF room temperature
(25 DEG C) are stirred overnight.50mL saturated sodium bicarbonate solution is poured in there-necked flask reactant liquor, has white solid to separate out, filter
Obtain white solid, wash with 20mL DMF solution every time, wash three times, wash three with 20mL saturated sodium bicarbonate solution afterwards
Secondary, then wash three times by 20mL ethyl acetate, finally washed once with 20mL ether, the white solid obtained uses normal hexane weight again
Crystallization obtains pure intermediate, puts into the midbody product drying pure in vacuum drying oven.
In 50mL round-bottomed flask, add above-mentioned intermediate 0.8g, 3-iodine propyl trimethoxy silicane 0.66g, be slowly heated
To 100 DEG C, react 12h, after reaction terminates, naturally cool to room temperature, wash repeatedly with normal hexane solvent, obtain above-mentioned bisamide chain
Organosilicone quaternary ammonium salt compounds.
Embodiment 4
The synthesis of hierarchical pore MFI structural zeolite molecular sieve: add aluminum source aluminum isopropylate. (AIP) in 250mL there-necked flask
0.08g, water 54.01g, micropore template TPAOH (TPAOH, 25%w/w) 4.10g.Mechanical agitation is to (the most about
Half an hour), add silicon source tetraethyl orthosilicate (TEOS) 4.19g, continue to stir to homogeneous (about 1h), then drip season in example 2
Ammonium salt 0.35g (0.0005mol), continues stirring two hours, obtains white gels.Gel is put in autoclave in 150 DEG C of crystallization
72h, crystallization is the most neutral with distilled water wash sucking filtration the most afterwards, obtains white solid, puts into 100 DEG C of baking 3h in baking oven, places into horse
Not 600 DEG C of calcining 5h in stove.Obtaining multi-stage porous MFI structure zeolite molecular sieve, its BET surface area is 386m2g-1, BJH aperture is
3.8nm, pore volume is 0.21cm3g-1。
The XRD figure spectrum of this hierarchical pore MFI structural zeolite molecular sieve is as it is shown in figure 1, result shows the degree of crystallinity of ZSM-5 very
Good, belong to typical ZSM-5 lattice.
Nitrogen absorption under low temperature-desorption isothermal curve is as in figure 2 it is shown, result shows relative pressure is more than 0.4MPa when bright
Explict occurrence hysteresis loop, has illustrated a large amount of irregular mesoporous generation.
BJH graph of pore diameter distribution is as shown in Figure 3, it is seen that aperture is mainly distributed on 4nm, for macropore range.
The scanning electron microscope of Fig. 4, Fig. 5 and transmission electron microscope are clearly visible the convex-concave of sample surfaces and rise and fall, from transmission electron microscope limit
Edge can be observed the crystalline structure on surface.
Embodiment 5
The synthesis of hierarchical pore MFI structural zeolite molecular sieve: add aluminum source aluminum isopropylate. (AIP) in 250mL there-necked flask
0.08g, water 54.64g, micropore template TPAOH (TPAOH, 25%w/w) 4.09g.Mechanical agitation is to (the most about
Half an hour), add silicon source tetraethyl orthosilicate (TEOS) 4.18g, continue to stir to homogeneous (about 1h), then drip season in example 1
Ammonium salt 0.36g (0.0005mol), continues stirring two hours, obtains white gels.Gel is put in autoclave in 150 DEG C of crystallization
72h, crystallization is the most neutral with distilled water wash sucking filtration the most afterwards, obtains white solid, puts into 100 DEG C of baking 3h in baking oven, places into horse
Not 600 DEG C of calcining 5h in stove.Obtaining multi-stage porous MFI structure zeolite molecular sieve, its BET surface area is 392m2g-1, BJH aperture is
3.81nm, pore volume is 0.25cm3g-1。
The x-ray diffraction pattern of product has the feature of Fig. 1；Nitrogen absorption under low temperature-desorption isothermal curve has the feature of Fig. 2；
Pore-size distribution has the feature of Fig. 3；Stereoscan photograph has the feature of Fig. 4；Transmission electron microscope photo has the feature of Fig. 5.
Embodiment 6
The synthesis of hierarchical pore MFI structural zeolite molecular sieve: add aluminum source aluminum isopropylate. (AIP) in 250mL there-necked flask
0.08g, water 54.64g, micropore template TPAOH (TPAOH, 25%w/w) 4.08g.Mechanical agitation is to (the most about
Half an hour), add silicon source tetraethyl orthosilicate (TEOS) 4.18g, continue to stir to homogeneous (about 1h), then drip season in example 3
Ammonium salt 0.41g (0.0005mol), continues stirring two hours, obtains white gels.Gel is put in autoclave in 150 DEG C of crystallization
72h, crystallization is the most neutral with distilled water wash sucking filtration the most afterwards, obtains white solid, puts into 100 DEG C of baking 3h in baking oven, places into horse
Not 600 DEG C of calcining 5h in stove.Obtaining multi-stage porous MFI structure zeolite molecular sieve, its BET surface area is 397m2g-1, BJH aperture is
3.93nm, pore volume is 0.21cm3g-1。
Embodiment 7
The synthesis of hierarchical pore MFI structural zeolite molecular sieve: add aluminum source aluminum isopropylate. (AIP) in 250mL there-necked flask
0.08g, water 54.64g, micropore template TPAOH (TPAOH, 25%w/w) 4.08g.Mechanical agitation is to (the most about
Half an hour), add silicon source tetraethyl orthosilicate (TEOS) 4.18g, continue to stir to homogeneous (about 1h), then drip season in example 3
Ammonium salt 0.8g (0.001mol), continues stirring two hours, obtains white gels.Gel is put in autoclave in 150 DEG C of crystallization
72h, crystallization is the most neutral with distilled water wash sucking filtration the most afterwards, obtains white solid, puts into 100 DEG C of baking 3h in baking oven, places into horse
Not 600 DEG C of calcining 5h in stove.Obtaining multi-stage porous MFI structure zeolite molecular sieve, its BET surface area is 454m2g-1, BJH aperture is
2.9nm, pore volume is 0.34cm3g-1。
The x-ray diffraction pattern of product has the feature of Fig. 1；Nitrogen absorption under low temperature-desorption isothermal curve has the feature of Fig. 2；
Pore-size distribution has the feature of Fig. 3；Stereoscan photograph has the feature of Fig. 4；Transmission electron microscope photo has the feature of Fig. 5.
Claims (10)
1. bisamide bond distance's carbochain organosilan quaternary ammonium compound, it is characterised in that: described structural formula of compound is:
Wherein, m=1-18 arbitrary integer, n=1-5 arbitrary integer, X-For Cl-、Br-、I-In one.
2. a preparation method for bisamide bond distance's carbochain organosilan quaternary ammonium compound as claimed in claim 1, bag
Include:
(1) N-methyliminodiacetic acid, fatty amine, I-hydroxybenzotriazole HOBT, carbodiimides EDCI, triethylamine are added
In solvent, then stirred overnight at room temperature, purify, obtain bisamide chain intermediate；Wherein N-methylene imine oxalic acid, fatty amine,
The mol ratio of HOBT, EDCI is 1:2.0-3.0:2.0-2.5:2.0-2.5；
(2) above-mentioned bisamide chain intermediate and alkylhalide group trimethoxy silane are mixed, at 90-130 DEG C, react 12-24h, cold
But to room temperature, washing, obtain bisamide bond distance's carbochain organosilan quaternary ammonium compound；Wherein bisamide chain intermediate and halogen
The mol ratio of alkyl trimethoxysilane is 1:1.0-2.0.
The preparation method of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 2,
It is characterized in that: in described step (1), fatty amine isWherein any positive integer of m=1-18.
The preparation method of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 2,
It is characterized in that: described step (1) purifies particularly as follows: by saturated sodium bicarbonate, ethyl acetate, use normal hexane after ether washing
Recrystallization.
The preparation method of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 2,
It is characterized in that: in described step (1), solvent is dimethylformamide or oxolane.
The preparation method of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 2,
It is characterized in that: in described step (2), the molecular formula of alkylhalide group trimethoxy silane is:Wherein X is
One in Cl, Br, I, n=1-5 arbitrary integer.
7. an application for bisamide bond distance's carbochain organosilan quaternary ammonium compound as claimed in claim 1, its feature
It is: described bisamide bond distance's carbochain organosilan quaternary ammonium compound is for the preparation containing mesoporous ZSM-5 molecular sieve, specifically
For:
(1) under the conditions of 20-25 DEG C, by silicon source, aluminum source and water mix and blend, it is subsequently adding micropore template, stirring, add double acyl
Amine bond distance's carbochain organosilan quaternary ammonium compound, stirring mixing, obtain mixed system；Wherein silicon source, aluminum source, micropore template
Agent, bisamide bond distance's carbochain organosilan quaternary ammonium compound, the mol ratio of water are 1-100:1:20-48:0.01-8:800-
5000；
(2) above-mentioned mixed system being carried out constant temperature stirring, obtain white gels, then carry out crystallization, quenching, sucking filtration, washing is extremely
Neutrality, is dried, and calcining obtains containing mesoporous ZSM-5 molecular sieve.
The application of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 7, it is special
Levy and be: one or more during silicon source is silicate class, sodium silicate crystal, waterglass, Ludox in described step (1)；Aluminum
Source is one or more in sodium metaaluminate, aluminum sulfate, aluminum nitrate, aluminum chloride and aluminum isopropylate.；Micropore template is tetramethyl
One in base ammonium bromide, tetraethylammonium bromide, Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide and TPAOH or
Several.
The application of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 7, it is special
Levy and be: in described step (2), constant temperature stirring is: under the conditions of 20-25 DEG C, speed of agitator is 360-450r/min, mixing time
For 2-3h.
The application of a kind of bisamide bond distance's carbochain organosilan quaternary ammonium compound the most according to claim 7, it is special
Levy and be: crystallization in described step (2) particularly as follows: containing politef bushing pipe confined reaction autoclave in, 140-170
Crystallization 3-96h at DEG C；It is dried and is: under the conditions of 80-120 DEG C, be dried 10-20h；Calcining calcines 10-15h at 400-600 DEG C.
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| CN109234217A (en) * | 2018-06-29 | 2019-01-18 | 安徽瑞赛生化科技有限公司 | Produce the immobilization and its application of 2,5- furandicarboxylic acid recombination engineering bacteria |
| CN110240612A (en) * | 2019-07-17 | 2019-09-17 | 南京神奇科技开发有限公司 | A kind of novel quaternary ammonium compound and its preparation method and application |
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| CN110240612B (en) * | 2019-07-17 | 2022-01-25 | 南京神奇科技开发有限公司 | Novel quaternary ammonium salt compound and preparation method and application thereof |
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