CN106268714A - A kind of preparation method of functionalized carbon nano-tube integral post - Google Patents

A kind of preparation method of functionalized carbon nano-tube integral post Download PDF

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CN106268714A
CN106268714A CN201610684936.XA CN201610684936A CN106268714A CN 106268714 A CN106268714 A CN 106268714A CN 201610684936 A CN201610684936 A CN 201610684936A CN 106268714 A CN106268714 A CN 106268714A
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carbon nano
integral post
column
tube
preparation
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刘海燕
李雪颖
白立改
闫宏远
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Hebei University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282—Porous sorbents
    • B01J20/285—Porous sorbents based on polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
    • B01J20/267—Cross-linked polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28011—Other properties, e.g. density, crush strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • 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
    • C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F210/14—Monomers containing five or more carbon atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/80—Aspects related to sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J2220/82—Shaped bodies, e.g. monoliths, plugs, tubes, continuous beds

Abstract

The invention discloses the preparation method of a kind of functionalized carbon nano-tube integral post, hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen and benzoyl peroxide are mixed, after ultrasonic disperse is uniform; add N; N dimethylaniline, is sufficiently mixed, and obtains polymer；Described polymer is poured in rustless steel gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached on high pressure pump, making of methanol flows rinses the polymer in column jecket mutually, obtains functionalized carbon nano-tube integral post.Integral post prepared by the present invention not only have that skeleton is stable, aperture big and uniformly, permeability is strong, post effect is high, can rapidly and efficiently separate the excellent properties such as small-molecule substance, but also have that preparation technology is simple, be easily achieved, favorable reproducibility, power consumption is low, operation application is convenient and the advantage such as low cost, is suitable to popularization and application in the separation of biological sample is analyzed.

Description

A kind of preparation method of functionalized carbon nano-tube integral post
Technical field
The present invention relates to the preparation method of high-efficiency liquid phase chromatography integral post, specifically a kind of functionalized carbon nano-tube is whole The preparation method of scapus.
Background technology
In recent years, along with the fast development of the ambits such as life sciences, environmental science, medical and health and chemical, The R and D of biological sample analysis, separation and purification technique become the focus of scientific research technical staff research.Wherein high-efficient liquid Phase chromatograph is a kind of very important method separating sample, and chromatographic column is the core of whole liquid chromatographic system, then, and section Grind worker by the performances such as Gao Zhuxiao, high sensitivity, high flux and rapidly and efficiently separation as exploitation chromatographic column key.
Integral post is that be prepared from by in-situ polymerization by mixture such as monomer, initiator, porogen is bar-shaped whole Body detached dowel.Integral post is as the new chromatographic separating medium developed rapidly in recent years, and it has permeability height, mechanical strength The advantages such as height, mass transfer velocity are fast and easily modified, are the most more and more applied, and have part integral post at present and achieve Commercialization.Theoretically, in preparation process, integral post surface by selecting different monomers or can be carried out by research staff Modify and obtain various types of integral post, to meet the high selectivity requirement of liquid chromatograph and electrochromatography.But it is true that specifically During research and development, selection and the proportioning thereof of each raw materials such as monomer whose, initiator, perforating agent are the most uncomfortable, its entirety obtained Post is it is possible to there will be particle packing structure, and pore diameter range distribution is wide, and internal structure heterogeneity is difficulty with bed pore structure equal Even unanimously and post effect is low, be applied to the separation of biological sample macromolecular substances more, and disengaging time is long, and separation efficiency is low, is difficult to Realize the separation analysis of small-molecule substance.Therefore, seek the new integral post that performance is the most excellent, prepare even structure, energy Enough rapidly and efficiently separate small-molecule substance, post effect integral post high, that disengaging time is short is the interior emphasis studied of whole industry, is also The trend of integral post property development.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of functionalized carbon nano-tube integral post, to solve existing entirety Rod structure is uneven, post low, the disengaging time length of effect, the problem that cannot separate small-molecule substance.
It is an object of the invention to be achieved through the following technical solutions: the preparation side of a kind of functionalized carbon nano-tube integral post Method, comprises the following steps:
Hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen and benzoyl peroxide are mixed Close, after ultrasonic disperse is uniform, adds DMA, be sufficiently mixed, obtain polymer；Described polymer is poured into stainless In steel gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached to high pressure In infusion pump, rinse the polymer in column jecket with methanol as mobile phase, obtain functionalized carbon nano-tube integral post；
Described hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen, benzoyl peroxide with N, the mass volume ratio of accelerine is: 0.1-0.6mg:0.51mL:0.48mL:0.51 mL:30mg:300 μ L.
Preferably, hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen, benzoyl peroxide Formyl and N, the mass volume ratio of accelerine is: 0.35-0.55mg:0.51mL:0.48mL:0.51mL:30mg: 300μL。
It is highly preferred that hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen, peroxidating Benzoyl and N, the mass volume ratio of accelerine is: 0.55mg:0.51mL:0.48mL:0.51mL:30mg:300 μ L。
Described porogen is that normal propyl alcohol and lauryl alcohol are by volume for the mixture of 1-10:1 composition；The most described positive third The volume ratio of alcohol and lauryl alcohol is 2.4-10:1, more preferably 2.4:1.
The column length of described rustless steel gc column tube is 50 mm, and internal diameter is 4.6 mm.
The innovation of the present invention is by have selected specific hydroxylating multi-walled carbon nano-tubes, octene, specific crosslinking The raw material such as agent, porogen and the proportioning of specified raw material and preparation process condition, make hydroxylating multi-walled carbon nano-tubes with embedding altogether Poly-mode embeds in polyalcohol integral pole so that the integral post of final preparation has that skeleton is stable, uniform pore diameter, permeability By force, post effect is high, can rapidly and efficiently separate the excellent properties such as small-molecule substance, extends the application of integral post.Additionally, this The preparation process condition of the integral post that invention provides is simple, be easily achieved, favorable reproducibility, low power consuming, operation application are convenient, cost Low, be suitable to popularization and application in the separation of biological sample is analyzed.
Accompanying drawing explanation
Fig. 1 is the internal morphology SEM figure of the integral post of embodiment 1 preparation.
Fig. 2 is the internal morphology SEM figure of the integral post of comparative example 1 preparation.
Fig. 3 is that the integral post of embodiment 1 preparation is at the chromatographic fractionation figure separating six kinds of Mixture of Benzene, toluene And Xylenes.
Fig. 4 is that the integral post of comparative example 1 preparation is at the chromatographic fractionation figure separating six kinds of Mixture of Benzene, toluene And Xylenes.
Fig. 5 is that the integral post of comparative example 2 preparation is at the chromatographic fractionation figure separating six kinds of Mixture of Benzene, toluene And Xylenes.
Fig. 6 is that the integral post of comparative example 3 preparation is at the chromatographic fractionation figure separating six kinds of Mixture of Benzene, toluene And Xylenes.
Detailed description of the invention
Example below is used for further describing the present invention, but limits the present invention the most in any form.
Embodiment 1
By the hydroxylating multi-walled carbon nano-tubes of 0.55mg, 0.51mL octene, 0.48mL TEGDMA, The benzoyl peroxide mixing of 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and 30mg, after ultrasonic disperse is uniform, adds 300 μ L DMA, be sufficiently mixed, obtain polymer；Described polymer is poured into the rustless steel of 50 mm × 4.6 mm I.D. In gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached to high pressure defeated On liquid pump, do flowing phase with methanol, flow velocity be 1mL/min pressure be 0.5Mpa, rinse the polymer 90min in column jecket, to obtain final product Functionalized carbon nano-tube integral post.
Embodiment 2
By the hydroxylating multi-walled carbon nano-tubes of 0.10mg, 0.51mL octene, 0.48mL TEGDMA, The benzoyl peroxide mixing of 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and 30mg, after ultrasonic disperse is uniform, adds 300 μ L DMA, be sufficiently mixed, obtain polymer；Described polymer is poured into the rustless steel of 50 mm × 4.6 mm I.D. In gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached to high pressure defeated On liquid pump, doing flowing phase with methanol, flow velocity is 1mL/min, rinses the polymer 90min in column jecket, obtains functionalized carbon nanometer Pipe integral post.
Embodiment 3
By the hydroxylating multi-walled carbon nano-tubes of 0.35mg, 0.51mL octene, 0.48mL TEGDMA, The benzoyl peroxide mixing of 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and 30mg, after ultrasonic disperse is uniform, adds 300 μ L DMA, be sufficiently mixed, obtain polymer；Described polymer is poured into the rustless steel of 50 mm × 4.6 mm I.D. In gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached to high pressure defeated On liquid pump, doing flowing phase with methanol, flow velocity is 1mL/min, rinses the polymer 90min in column jecket, obtains functionalized carbon nanometer Pipe integral post.
Embodiment 4
By the hydroxylating multi-walled carbon nano-tubes of 0.6mg, 0.51mL octene, 0.48mL TEGDMA, The benzoyl peroxide mixing of 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and 30mg, after ultrasonic disperse is uniform, adds 300 μ L DMA, be sufficiently mixed, obtain polymer；Described polymer is poured into the rustless steel of 50 mm × 4.6 mm I.D. In gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached to high pressure defeated On liquid pump, doing flowing phase with methanol, flow velocity is 1mL/min, rinses the polymer 90min in column jecket, obtains functionalized carbon nanometer Pipe integral post.
Comparative example 1
By 0.51mL octene, 0.48mL TEGDMA, 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and 30mg Benzoyl peroxide mixing, ultrasonic disperse uniformly after, add the DMA of 300 μ L, be sufficiently mixed, obtain polymerization Thing；Being poured into by described polymer in the rustless steel gc column tube of 50 mm × 4.6 mm I.D., 30 DEG C of reaction 3h, stainless steel colored Chromatographic column stigma is installed at the two ends of spectrum column jecket, is then attached on high pressure pump, does flowing phase with methanol, and flow velocity is 1mL/ Min, rinses the polymer 90min in column jecket, obtains integral post.
Comparative example 2
(1) by 0.55mg hydroxylating multi-walled carbon nano-tubes, 0.3mL octene, 0.4mL trimethylolpropane trimethacrylate, 0.1mL Ethyleneglycol dimethacrylate fat, 0.38mL lauryl alcohol, 0.08mL normal propyl alcohol and the mixing of 25mg benzoyl peroxide, ultrasonic disperse After Jun Yun, add the DMA of 150 μ L, and be sufficiently mixed, mixed liquor is poured into 50 mm × 4.6 mm I.D. Rustless steel gc column tube in, at 30 DEG C react 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, then Being connected on high pressure pump, do flowing phase with methanol, flow velocity is 1mL/min, rinses the polymer 90min in column jecket, to obtain final product Integral post A.
(2) similar with (1) under equal conditions, be not added with hydroxylating multi-walled carbon nano-tubes, 0.3mL octene, 0.4mL tri-hydroxyl first Base propane triacrylate, 0.1mL ethyleneglycol dimethacrylate fat, 0.38mL lauryl alcohol, 0.08mL normal propyl alcohol and 25mg mistake BP mixes, and after ultrasonic disperse is uniform, adds the DMA of 150 μ L, and is sufficiently mixed, by mixed liquor It is poured in the rustless steel gc column tube of 50 mm × 4.6 mm I.D., at 30 DEG C, reacts 3h, at the two of rustless steel gc column tube End installs chromatographic column stigma, is then attached on high pressure pump, and doing flow rate of mobile phase with methanol is 1mL/min, rinses post Polymer 90min in pipe, obtains integral post B.
Comparative example 3
(1) by 0.55mg hydroxylating multi-walled carbon nano-tubes, 0.51mL tetradecene, 0.48mL TEGDMA, 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and the mixing of 30mg benzoyl peroxide, after ultrasonic disperse is uniform, add 300 μ L's DMA, and be sufficiently mixed, mixed liquor is poured in the rustless steel gc column tube of 50 mm × 4.6 mm I.D., 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached on high pressure pump, use first Alcohol does flowing phase, and flow velocity is 1mL/min, rinses the polymer 90min in column jecket, obtains integral post C.
(2) similar with (1) be under equal conditions added without hydroxylating multi-walled carbon nano-tubes, then 0.51mL tetradecene, 0.48mL TEGDMA, 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and 30mg benzoyl peroxide are mixed Close, ultrasonic disperse uniformly after, add the DMA of 300 μ L, and be sufficiently mixed, mixed liquor is poured into 50 mm × In the rustless steel gc column tube of 4.6 mm I.D., 30 DEG C of reaction 3h, install chromatographic column at the two ends of rustless steel gc column tube Stigma, is then attached on high pressure pump, does flowing phase with methanol, and flow velocity is 1mL/min, rinses the polymer in column jecket 90min, obtains integral post D.
Comparative example 4
By 0.55mg hydroxylating multi-walled carbon nano-tubes, 0.51mL octene, 0.48mL TEGDMA, 0.15mL lauryl alcohol, 0.36mL normal propyl alcohol and the mixing of 30mg benzoyl peroxide, after ultrasonic disperse is uniform, add 300 μ L's DMA, and be sufficiently mixed, mixed liquor is poured in the capillary tube of 25cm × 250 μm i.d., 30 DEG C of reaction 3h, Being then attached to pressurization capillary electric chromatogram, gained CNT integral post connects upper pressurization capillary electric chromatogram, then uses second Nitrile and water do flowing phase, and when flowing is 100% acetonitrile mutually, the flow velocity of pressurization capillary electric chromatogram is set to pressure during 0.05mL/min Power is 17.5Mpa, and pressure is excessive and flowing cannot be flowed out mutually in integral post, it is impossible to proceed next step experiment.
According to ordinary skill in the art means, the present invention, by the ratio of each component in feed change, regulates pressure Excessive phenomenon, as by changing one or more in the following manner, will the content of TEGDMA change into 0.36mL, the content of normal propyl alcohol is changed into 0.26mL, change the content of octene into 0.38mL, under same experiment condition, still So find that pressure is excessive and flowing cannot be flowed out mutually in integral post, it is impossible to proceed next step experiment.
The electron-microscope scanning experiment of material structure in embodiment 5 integral post post.
Material structure in the column jecket of integral post prepared by embodiment 1 and comparative example 1 is carried out electron-microscope scanning, its scanning result As depicted in figs. 1 and 2.Fig. 1 be embodiment 1 preparation integral post in the SEM figure of material, can be apparent from from figure finds out this Material aperture in the integral post of invention preparation is big, skeleton is more uniformly distributed, and Fig. 2 mesoporous is relatively small.
Integral post prepared by embodiment 6 present invention and the application of integral post separation sample prepared by comparative example
(1) integral post prepared by embodiment 1 being connected on high performance liquid chromatograph, its chromatographic condition is: flowing is 65% second mutually Nitrile 35% aqueous solution, flow velocity is 1 mL/min, and detection wavelength is 254 nm, and sample size: 10 μ L, with 6 kinds of Mixture of Benzene, toluene And Xylene (isophthalic Diphenol, benzene, chlorobenzene, naphthalene, fluorenes and anthracene) it is test sample.
Experimental result: its chromatographic isolation spectrogram such as Fig. 3, in figure, its peak sequence is followed successively by: 1, resorcinol；2, benzene；3、 Chlorobenzene；4, naphthalene；5, fluorenes；6, anthracene.
(2) integral post prepared by comparative example 1 being connected on high performance liquid chromatograph, its chromatographic condition is: flowing is mutually 53% acetonitrile 47% aqueous solution, flow velocity is 1 mL/min, and detection wavelength is 254 nm, and sample size: 10 μ L, with 6 kinds of Mixture of Benzene, toluene And Xylenes (resorcinol, benzene, chlorobenzene, naphthalene, fluorenes and anthracene) is test sample.
Experimental result: its chromatographic isolation spectrogram such as Fig. 4, in figure, peak sequence is followed successively by: 1, resorcinol；2, benzene；3, chlorine Benzene；4, naphthalene；5, fluorenes；6, anthracene.
(3) that comparative example 2 is prepared adds hydroxylating multi-walled carbon nano-tubes and is not added with hydroxylating multi-walled carbon nano-tubes integral post Being connected respectively on high performance liquid chromatograph, its chromatographic condition is all: flowing is 50% acetonitrile 50% aqueous solution mutually, and flow velocity is 1 ML/min, detection wavelength be 254 nm, sample size: 10 μ L, with 6 kinds of Mixture of Benzene, toluene And Xylenes (resorcinol, benzene, chlorobenzene, naphthalene, fluorenes and Anthracene) it is test sample.
Experimental result: its chromatographic isolation spectrogram such as Fig. 5, its peak sequence is followed successively by: 1, resorcinol；2, benzene；3, chlorobenzene； 4, naphthalene；5, fluorenes；6, anthracene.
(4) that comparative example 3 is prepared adds hydroxylating multi-walled carbon nano-tubes and is not added with hydroxylating multi-walled carbon nano-tubes integral post Being connected on high performance liquid chromatograph, its chromatographic condition is all: flowing is 65% acetonitrile 35% aqueous solution mutually, and flow velocity is 1 mL/ Min, detection wavelength is 254 nm, and sample size: 10 μ L, with 6 kinds of Mixture of Benzene, toluene And Xylenes (resorcinol, benzene, chlorobenzene, naphthalene, fluorenes and anthracene) For test sample.
Experimental result: its chromatographic isolation spectrogram such as Fig. 6, is followed successively by according to peak sequence in figure: 1, resorcinol；2, benzene； 3, chlorobenzene；4, naphthalene；5, fluorenes；6, anthracene.
Embodiment 7 present invention contrasts with the post effect of comparative example
The theoretical cam curve of this experiment can be according to this formula N=5.55 (tR/W0.5)/L records, and N is theoretical cam curve (plates/m), tRFor the retention time (min) of analyte, W0.5For half-peak breadth, L is column length.Calculate each the most respectively real Execute the theoretical cam curve of the benzene of example and comparative example.
Experimental result:
The post effect of the integral post that table 1 present invention is prepared with comparative example
The integral post prepared with comparative example by the present invention separates disengaging time and the comparison of post effect thereof of six kinds of Mixture of Benzene, toluene And Xylenes, Finding that integral post prepared by the present invention can separate small-molecule substance, and its separating effect is more preferable, post effect is higher, disengaging time Short, separation efficiency is high.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by described embodiment Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify, All should be the substitute mode of equivalence, within being included in protection scope of the present invention.

Claims (5)

1. the preparation method of a functionalized carbon nano-tube integral post, it is characterised in that comprise the following steps:
Hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen and benzoyl peroxide are mixed Close, after ultrasonic disperse is uniform, adds DMA, be sufficiently mixed, obtain polymer；Described polymer is poured into stainless In steel gc column tube, 30 DEG C of reaction 3h, install chromatographic column stigma at the two ends of rustless steel gc column tube, are then attached to high pressure In infusion pump, making of methanol flows rinses the polymer in column jecket mutually, obtains functionalized carbon nano-tube integral post；
Described hydroxylating multi-walled carbon nano-tubes, octene, TEGDMA, porogen, benzoyl peroxide with N, the mass volume ratio of accelerine is: 0.1-0.6mg:0.51mL:0.48mL:0.51 mL:30mg:300 μ L.
The preparation method of functionalized carbon nano-tube integral post the most according to claim 1, it is characterised in that described hydroxylating Multi-walled carbon nano-tubes, octene, TEGDMA, porogen, benzoyl peroxide and N, accelerine Mass volume ratio be: 0.35-0.55mg:0.51mL:0.48mL:0.51 mL:30mg:300 μ L.
The preparation method of functionalized carbon nano-tube integral post the most according to claim 1 and 2, it is characterised in that described cause Hole agent is the mixture of normal propyl alcohol and lauryl alcohol.
The preparation method of functionalized carbon nano-tube integral post the most according to claim 3, it is characterised in that described normal propyl alcohol It is 1-10:1 with the volume ratio of lauryl alcohol.
The preparation method of functionalized carbon nano-tube integral post the most according to claim 1 and 2, it is characterised in that described not The column length of rust steel gc column tube is 50 mm, and internal diameter is 4.6 mm.
CN201610684936.XA 2016-08-18 2016-08-18 A kind of preparation method of functionalized carbon nano-tube integral post Pending CN106268714A (en)

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CN107596734A (en) * 2017-10-24 2018-01-19 河北大学 A kind of preparation method of graphite oxide alkene polymer continuous bed, using and a kind of method of separation and concentration phytosterol
CN110376321A (en) * 2019-07-30 2019-10-25 河北大学 A method of polymer continuous bed and ursolic acid on-line preconcentration for on-line preconcentration purifying ursolic acid purify
CN113860290A (en) * 2021-10-22 2021-12-31 广西壮族自治区海洋环境监测中心站 Modified carbon nano tube and application thereof in chromatographic separation
CN115594887A (en) * 2022-12-13 2023-01-13 广东粤港澳大湾区黄埔材料研究院（Cn） Preparation method of modified carbon nanotube and application of modified carbon nanotube in tire tread rubber

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