CN109535316A - A kind of n-isopropyl acrylamide hydridization integral post and preparation method thereof - Google Patents
A kind of n-isopropyl acrylamide hydridization integral post and preparation method thereof Download PDFInfo
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- CN109535316A CN109535316A CN201811354539.1A CN201811354539A CN109535316A CN 109535316 A CN109535316 A CN 109535316A CN 201811354539 A CN201811354539 A CN 201811354539A CN 109535316 A CN109535316 A CN 109535316A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
A kind of n-isopropyl acrylamide hydridization integral post and preparation method thereof, comprising the following steps: capillary, which is carried out pretreatment, makes its inner wall surface with ethylene linkage；Siloxane crosslinker, silicone coupling agents, n-isopropyl acrylamide, polyethylene glycol, urea, aqueous acetic acid and initiator are mixed to get pre-polymerization liquid, wherein silicone coupling agents contain ethylene linkage and siloxane group, siloxane crosslinker contains multiple paradigmatic structures, and paradigmatic structure contains siloxane group；Capillary is placed in pre-polymerization liquid and enters pre-polymerization liquid in capillary, and the both ends of capillary are sealed, the inner wall and coupling agent of crosslinking agent and capillary occur ethylene linkage polymerization reaction and form skeleton structure, ring-opening reaction occurs for the alkenyl of coupling agent and n-isopropyl acrylamide simultaneously, obtains n-isopropyl acrylamide hydridization integral post.N-isopropyl acrylamide hydridization integral post made from method of the invention has hydrophobicity, and separating capacity is strong.
Description
Technical field
The present invention relates to substance separation technology field, more particularly to a kind of n-isopropyl acrylamide hydridization integral post and
Preparation method.
Background technique
In chemical substance separation technology field, as isolated core, chromatographic column plays critical effect.Presently the most
Common chromatographic column can be divided into positive and reverse chromatograms two major classes.Wherein the polarity of stationary phase is less than mobile phase in reverse-phase chromatography
Polarity, reverse-phase chromatography are widely used in the separation analysis of middle polarity and low pole compound.Divide from stationary phase angle, it can be with
It is divided into two class of packed column and integral post, integral post (monolith column) is considered as stationary phase of new generation, it is by list
Body, crosslinking agent, pore-foaming agent and initiator mixed solution caused in capillary column by in-situ heat or light initiation polymerization obtains
The cylinder with co-continuous porous structure arrived.Integral post has the characteristics that preparation is simple, structure is uniform, permeability is good, thus
Obtain very high separative efficiency.
Organic-inorganic hybridization monolithic column reported by Zou Hanfa seminar for the first time, by simultaneously using organic monomer and inorganic
Monomer is polymerize, so that obtain integral post and can obtain enough rigidity also and can guarantee to possess enough organo-functional groups,
To realize the unification of service life and separating capacity.Sol-gal process is due to being easy to obtain using aqueous polymerization method
Biggish specific surface area is obtained, thus is one of the prefered method for being prepared with machine inorganic hybridization integral post, is very suitable to have with preparation
There is the preparation of hydrophily hydridization integral post, but the water solubility of hydrophobic monomer limits it in the preparation of hydrophobicity hydridization integral post
Application.
Summary of the invention
Based on this, it is necessary to provide a kind of method for preparing hydrophobic hydridization integral post using sol-gal process.
First aspect present invention is related to a kind of preparation method of n-isopropyl acrylamide hydridization integral post, including following step
It is rapid:
A, capillary is carried out pretreatment makes its inner wall surface with ethylene linkage functional group；
B, siloxane crosslinker, silicone coupling agents, n-isopropyl acrylamide, urea, polyethylene glycol, acetic acid is water-soluble
Liquid and initiator are mixed to get pre-polymerization liquid, wherein the silicone coupling agents contain ethylene linkage and siloxy group, the siloxanes is handed over
Connection agent contains paradigmatic structure, and the paradigmatic structure is siloxane group；
C, it will be placed in the pre-polymerization liquid by pretreated capillary and enter the pre-polymerization liquid in the capillary,
And by the both ends of the capillary seal, the ethylene linkage of the silicone coupling agents respectively with the ethylene linkage on the inner wall of the capillary
Ethylene linkage polymerization reaction occurs for functional group and n-isopropyl acrylamide monomer, realizes that skeleton is fixed and monomer introduces, the silicon oxygen
Logical react with siloxane crosslinker generation condensation polymerization of the siloxy group of alkane coupling agent is connected to form skeleton structure, obtains the N-
N-isopropylacrylamide hydridization integral post.
The preparation method of n-isopropyl acrylamide hydridization integral post of the present invention, utilizes silicone coupling agents and N- isopropyl
Acrylamide free radical polymerization introduces hydrophobic isopropyl, and column bed is formed directly in capillary by crosslinking agent, makes
Obtain n-isopropyl acrylamide hydridization integral post.Obtained n-isopropyl acrylamide hydridization integral post hydrophobicity is good, mechanical strong
Degree is high, and this method is easy to operate, favorable reproducibility.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, the pre-polymerization liquid is placed at 0~5 DEG C and is made
With 1~4h, so that siloxane group occurs hydrolysis and generates polymerizable silicone hydroxyl.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, at 30~50 DEG C of the capillary with it is described
Pre-polymerization liquid effect 4~for 24 hours, so that the ethylene linkage polymerization reaction and the condensation reaction occur for the pre-polymerization liquid.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, the weight percent of the pre-polymerization liquid is formed
It is as follows: siloxane crosslinker 15~25%, silicone coupling agents 4~10%, n-isopropyl acrylamide 2~5%, urea 5~
8%, polyethylene glycol 4~9%, aqueous acetic acid 50~65% and initiator 0.05~0.1%.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, the molecular weight polyethylene glycol is greater than
1000, more optimized molecular weight polyethylene glycol is 2000.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, the silicone coupling agents are vinyl three
Methoxy silane.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, the siloxane crosslinker is tetramethoxy
Silane.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, step A passes through the side included the following steps
Method is implemented:
A1, the inner wall surface that capillary glass tube is successively handled with NAOH solution and hydrochloric acid solution, have its inner wall surface
Silicone hydroxyl；Then,
A2, the inner wall surface is handled with bifunctional reagent's 3- methacrylic acid oxygen propyl trimethoxy silicane, wherein
Condensation reaction occurs for the silicone hydroxyl on trimethoxy silane group and capillary tube inner wall surface, so that the inner wall surface be made to have
Ethylene linkage functional group.
In the preparation method of the above n-isopropyl acrylamide hydridization integral post, the initiator is two NSC 18620 salt of azo
Hydrochlorate.
Second aspect of the present invention is related to a kind of n-isopropyl acrylamide hydridization integral post, uses first aspect present invention
The preparation method is made.Its hydrophily is strong, high mechanical strength, the favorable reproducibility of product；Furthermore preparation method is simple, ring
Guarantor property is good.
Detailed description of the invention
Fig. 1 is the reaction mechanism figure of embodiment；
Fig. 2 is the scanning electron microscope (SEM) photograph for the n-isopropyl acrylamide hydridization entirety column section that embodiment obtains；
Fig. 3 is the column bed material (b) and N- isopropyl third for the n-isopropyl acrylamide hydridization integral post that embodiment obtains
The infrared spectrum of acrylamide monomer (a)；
Fig. 4 is the column back pressure for the n-isopropyl acrylamide hydridization integral post that embodiment obtains and the relationship of linear flow rate
Figure.
Fig. 5 is benzene compound separation chromatography in the n-isopropyl acrylamide hydridization integral post that embodiment obtains
Figure.
Fig. 6 is phenol compound separation chromatography in the n-isopropyl acrylamide hydridization integral post that embodiment obtains
Figure.
Fig. 7 is amino benzenes compounds separation chromatography in the n-isopropyl acrylamide hydridization integral post that embodiment obtains
Figure.
Fig. 8 is benzoic acid derivative separation chromatography in the n-isopropyl acrylamide hydridization integral post that embodiment obtains
Figure.
Fig. 9 is that polycyclic arene compound separates color in the n-isopropyl acrylamide hydridization integral post that embodiment obtains
Spectrogram.
Figure 10 is perfluorochemical separation chromatogram in the n-isopropyl acrylamide hydridization integral post that embodiment obtains.
Figure 11 is that chlorophenol species compound separates color in the n-isopropyl acrylamide hydridization integral post that embodiment obtains
Spectrogram.
Specific embodiment
To facilitate the understanding of the present invention, a more comprehensive description of the invention is given in the following sections with reference to the relevant attached drawings.In attached drawing
Give preferred embodiment of the invention.But the invention can be realized in many different forms, however it is not limited to herein
Described embodiment.Purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Step S100: capillary, which is carried out pretreatment, makes its inner wall surface with ethylene linkage functional group.
Step S100 is by introducing bifunctional reagent 3- methacrylic acid oxygen propyl trimethoxy silicane (γ-
MAPS).Siloxy group is contained in one end of γ-MAPS, reacts with the silicone hydroxyl of quartz capillary wall, and the other end contains ethylene linkage function
Group.
The step of step S100 is specifically included in one of the embodiments: using NaOH solution, water, hydrochloric acid, water and methanol
It passes sequentially through capillary and washs 8~14h, drying.γ-MAPS solution is fitted into capillary and seals the both ends of capillary.
Capillary equipped with silane mixture liquid is placed in 8~14h of reaction at 60~70 DEG C.It is washed with methanol by capillary, dries up, obtain
To by pretreated capillary.
Wherein by capillary tube inner wall after NaOH solution is handled, the inner wall of capillary has silicone hydroxyl.The ethylene linkage of γ-MAPS
Activity is higher, is easy to polymerize with free radical and other surfaces derivatization reaction.
Specifically, the concentration of NaOH solution is 1mol/L.Specifically, the concentration of hydrochloric acid is 1mol/L.Specifically, γ-
MAPS solution is the mixed solution of the γ-MAPS that volume ratio is 1:1 and methanol.Specifically, drying is nitrogen in step S100
Drying.
Preferably, the capillary equipped with silane mixture liquid is placed at 60 DEG C and reacts 12h.
Step S200: by siloxane crosslinker, silicone coupling agents, n-isopropyl acrylamide, urea, polyethylene glycol,
Aqueous acetic acid and initiator mixing, low temperature stirs to get pre-polymerization liquid, wherein the coupling agent contains ethylene linkage and siloxy group, institute
It states crosslinking agent and contains paradigmatic structure, the paradigmatic structure is siloxane group；
Preferably, each component ratio is siloxane crosslinker 15~25%, silicone coupling agents 4~10%, N- isopropyl
Acrylamide 2~5%, urea 5~8%, polyethylene glycol 4~9%, aqueous acetic acid (0.1M) 50~65% and initiator 0.05
~0.1%.
Step S300: will be placed in pre-polymerization liquid by pretreated capillary and enter pre-polymerization liquid in capillary, and will
The both ends of capillary seal, and ethylene linkage occurs for the silicone hydroxyl and siloxane crosslinker on silicone coupling agents and capillary tube inner wall surface
Polymerization reaction forms skeleton structure, while the alkenyl of silicone coupling agents and n-isopropyl acrylamide generation free radical polymerization are anti-
It answers, obtains n-isopropyl acrylamide hydridization integral post.
Preferably, will by pretreated capillary at 30~50 DEG C with the pre-polymerization liquid effect 4~for 24 hours so that in advance
The ethylene linkage polymerization reaction and the condensation polymerization occur for poly- liquid.It is furthermore preferred that will be by pretreated capillary and pre-polymerization liquid
12h is acted in 40 DEG C to guarantee the abundant progress of ethylene linkage polymerization reaction and condensation polymerization.
It further includes washing step before coming into operation that n-isopropyl acrylamide hydridization integral post is obtained in step S300.
Preferably, the condition of washing is successively to pass sequentially through capillary douche with methanol, water, is dried up.The effect of washing is removal capillary
Remaining reactant and polynary pore-foaming agent urea, polyethylene glycol and 0.1mol/ aqueous acetic acid, different to obtain porous N- in pipe
Propylacrylamide hydridization integral post.
The preparation method of n-isopropyl acrylamide hydridization integral post of the present invention, utilizes silicone coupling agents and N- isopropyl
Acrylamide free radical polymerization introduces isopropyl, and column bed is formed directly in capillary by siloxane crosslinker, and N- is made
N-isopropylacrylamide hydridization integral post.Obtained n-isopropyl acrylamide hydridization integral post hydrophobicity is good, high mechanical strength,
And this method is easy to operate, favorable reproducibility.
The following are specific embodiments.
Capillary is passed sequentially through with the NaOH solution of 1mol/L, water, the hydrochloric acid of 1mol/L, water and methanol and washs 12h, uses nitrogen
Air-blowing is dry.γ-MAPS solution γ-the MAPS and methanol of 1:1 (volume ratio be) is fitted into capillary and with silicon rubber by capillary
The both ends of pipe seal.Capillary equipped with silane mixture liquid is placed in water-bath 12h at 60 DEG C.It is washed with methanol by capillary
30min is washed, with being dried with nitrogen, is obtained by pretreated capillary.
By PEG100000.175g, urea 0.145g, aqueous acetic acid (0.1M) 1.35mL, 450 μ L of tetramethoxy-silicane,
Vinyltrimethoxysilane 150 μ L, n-isopropyl acrylamide 80mg stir hydrolysis after mixing each component and at 0 DEG C
4h is reacted into clear pre-polymerization liquid.
30cm will be cut by pretreated capillary, pre-polymerization liquid will be sucked in capillary；After pre-polymerization liquid fills capillary,
The both ends of capillary are used into silicone rubber seal.
Capillary equipped with pre-polymerization liquid is placed in water-bath 12h at 40 DEG C, successively passes sequentially through capillary with water, methanol
It rinses, drying obtains n-isopropyl acrylamide hydridization integral post.
Implementation column schematic diagram is as shown in Figure 1.
Structural characterization (1)
Electronic Speculum test is scanned to the section for the n-isopropyl acrylamide hydridization integral post that embodiment obtains, is obtained
The scanning electron microscope (SEM) photograph of embodiment is as shown in Figure 2.
The n-isopropyl acrylamide hydridization integral post that embodiment obtains, column bed continuous uniform, and there is porous structure,
Illustrate that its permeability is good.
Structural characterization (2)
Column bed material (curve b) and the N- isopropyl third for the n-isopropyl acrylamide hydridization integral post that embodiment is obtained
(curve a) carries out Fourier infrared spectrum analysis to acrylamide respectively, obtains infrared spectrum 3, and wherein abscissa is Wavenumber
Wave number, unit cm-1, ordinate be Transmittance light transmittance, unit %, as shown in Figure 5.
A and B is compared it is found that wherein in the flexible vibration that 1689cm-1 and 1563cm-1 are respectively carbonyl and N-H in amide groups
It is dynamic；Wherein 3290cm-1 is the N-H stretching vibration of Hydrogenbond, and 1387cm-1 and 1367cm-1 are different on N-isopropylacrylamide
Symmetrical deformation vibration lotus root on propyl closes division and is formed bimodal.Proof has been successfully introduced into different in the preparation process of integral post
Propylacrylamide monomer.
Performance characterization
The mechanical strength of integral post affects its use time and separating effect.Respectively using acetonitrile and water as mobile phase,
Column length is the hydridization integral post of 10cm, and using the method for nanoliter liquid chromatogram, it is whole to have investigated n-isopropyl acrylamide hydridization
The relationship of the column back pressure (Back-pressure, unit psi) and linear flow rate (Flow rate, unit are μ L/min) of column
Figure, as shown in Figure 4.Under test conditions, the column pressure of n-isopropyl acrylamide hydridization integral post is as the increase of flow velocity is in line
Property increase, column pressure with tool linear flow rate have good linear relationship (R2> 0.999), show that the n-isopropyl acrylamide is miscellaneous
Changing integral post has good mechanical strength and stability.
Separating capacity is to measure the index of the final new energy of integral post, in order to investigate obtained n-isopropyl acrylamide
The hydrophilic separating capacity of hydridization integral post, using 95% acetonitrile solution mobile phase the most respectively to ucleosides, phenolic compound, alkali
Base class, amides compound have carried out separate evaluation to it.As shown in figures 5-8, respectively alkylbenzene, phenol, phenyl amines,
Benzoic acids, multiring aromatic hydrocarbon, perfluorochemical, chlorophenol species separating resulting, the results showed that, four class compounds are in gained entirety
Have on column and be effectively maintained ability, and good separation, peak type is symmetrical.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of n-isopropyl acrylamide hydridization integral post, which comprises the following steps:
A, capillary is carried out pretreatment makes its inner wall surface with ethylene linkage functional group；
B, by siloxane crosslinker, silicone coupling agents, n-isopropyl acrylamide, urea, polyethylene glycol, aqueous acetic acid and
Initiator is mixed to get pre-polymerization liquid, wherein the silicone coupling agents contain ethylene linkage and siloxy group, the siloxane crosslinker
Containing paradigmatic structure, the paradigmatic structure is siloxane group；
C, it will be placed in the pre-polymerization liquid by pretreated capillary and enter the pre-polymerization liquid in the capillary, and will
The both ends of the capillary seal, the ethylene linkage of the silicone coupling agents respectively with the ethylene linkage function on the inner wall of the capillary
Ethylene linkage polymerization reaction occurs for group and n-isopropyl acrylamide monomer, realizes that skeleton is fixed and monomer introduces, the siloxanes is even
The siloxy group for joining agent is connected to form skeleton structure by reacting with siloxane crosslinker generation condensation polymerization, and it is different to obtain the N-
Propylacrylamide hydridization integral post.
2. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that by institute
It states pre-polymerization liquid and is placed in 1~4h of effect at 0~5 DEG C, so that siloxane group occurs hydrolysis and generates polymerizable silicone hydroxyl.
3. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that by institute
State by pretreated capillary at 30~50 DEG C with pre-polymerization liquid effect 4~for 24 hours so that described in the pre-polymerization liquid occurs
Ethylene linkage polymerization reaction and condensation polymerization reaction.
4. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that described
The weight percent composition of pre-polymerization liquid is as follows:
Siloxane crosslinker 15~25%, silicone coupling agents 4~10%, n-isopropyl acrylamide 2~5%, urea 5~
8%, polyethylene glycol 4~9%, aqueous acetic acid 50~65% and initiator 0.05~0.1%.
5. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that described
Siloxane crosslinker is tetramethoxy-silicane.
6. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that described
Silicone coupling agents are vinyltrimethoxysilane.
7. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that described
Molecular weight polyethylene glycol is greater than 1000.
8. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that wherein
Step A is implemented by method comprising the following steps:
A1, the inner wall surface that capillary glass tube is successively handled with NAOH solution and hydrochloric acid solution make its inner wall surface with silicon hydroxyl
Base；Then,
A2, the inner wall surface is handled with bifunctional reagent's 3- methacrylic acid oxygen propyl trimethoxy silicane, wherein front three
Condensation reaction occurs for the silicone hydroxyl on oxysilane group and capillary tube inner wall surface, to make the inner wall surface with ethylene linkage
Functional group.
9. the preparation method of n-isopropyl acrylamide hydridization integral post according to claim 1, which is characterized in that described
Initiator is azo-bis-isobutyrate hydrochloride.
10. a kind of n-isopropyl acrylamide hydridization integral post, which is characterized in that it is according to claim 1~9 described in any one
The preparation method of n-isopropyl acrylamide hydridization integral post be prepared.
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