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A kind of sol-gel matrix capillary monolithic column and preparation method thereof

A capillary monolithic column and sol-gel technology, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve problems such as increased entropy, chaotic molecular motion, and complex actions, and achieve improved efficiency, tight combination, and heavy effect of guarantee

Active Publication Date: 2018-04-20
HENAN INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Another point of view is that the effect of microwaves on chemical reactions is very complicated. On the one hand, the reactant molecules absorb microwave energy, which increases the speed of molecular motion, resulting in chaotic molecular motions, resulting in an increase in entropy; in addition, the effect of microwaves on polar molecules, Forcing it to move in accordance with the action of the electromagnetic field leads to an increase in entropy. Therefore, the mechanism of microwave action on chemical reactions cannot be described only by the microwave heating effect.

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  • A kind of sol-gel matrix capillary monolithic column and preparation method thereof
  • A kind of sol-gel matrix capillary monolithic column and preparation method thereof
  • A kind of sol-gel matrix capillary monolithic column and preparation method thereof

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Embodiment Construction

[0021] The present invention will be described in detail below in conjunction with specific embodiments.

[0022] Experimental procedure

[0023] Reagents: methacryloxypropyltrimethoxysilane, sodium hydroxide, hydrochloric acid, methanol, toluene, sodium dodecylsulfonate, tris(Tris), acetonitrile, naphthalene, toluene, thiourea , Benzene, biphenyl.

[0024] making process:

[0025] 2.1 Preparation of polymerization solution: 1150 μL of methacryloxypropyltrimethoxysilane and 300 μL of 0.12M hydrochloric acid were stirred at room temperature for 30 minutes in the dark to obtain a monomer solution. Then, 800 μL of toluene and 50 mg of SDS (sodium dodecylsulfonate) were added to 200 μL of the monomer solution, and stirred at room temperature for 30 minutes to obtain a toluene-monomer solution mixture containing SDS.

[0026] 2.2 Capillary pretreatment: (1) sequentially use 0.1M NaOH, H 2 O, 0.1M HCl solution rinsed for 0.5h, and then rinsed with water to pH = 7; (2) rinsed wit...

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Abstract

The invention discloses a sol-gel matrix capillary integral column and a preparation method thereof. The preparation method is as follows: fill the polymerization solution into a 10 cm alkenylated capillary tube and conduct microwave polymerization for 14.5 minutes at a temperature of 80° C. and a power of 700 W. The invention prepares the sol-gel capillary monolithic column by in-situ polymerization in the capillary through a temperature-controlled microwave synthesizer. The chromatographic performance of the prepared monolithic column was evaluated under the separation mode of pressure electrochromatography (P-CEC). The four substances of thiourea, naphthalene, toluene and biphenyl were separated by baseline, and the lowest theoretical plate height of naphthalene was It can reach 1.83μm. Compared with the experimental results of the ordinary microwave method, the theoretical plate number of naphthalene increased from 10000 / m to 54794 / m, which greatly improved the separation column efficiency of the compound. The results of scanning electron microscopy show that the monolithic sol-gel capillary column prepared by temperature-controlled microwave has uniform material distribution in the tube and is closely combined with the inner wall of the capillary.

Description

technical field [0001] The invention relates to capillary monolithic column technology, in particular to a sol-gel matrix capillary monolithic column and a preparation method thereof. Background technique [0002] Capillary electrochromatography (CEC) is a micro-column liquid chromatography separation technique driven by electroosmotic flow. It combines the high selectivity of high performance liquid chromatography (HPLC) with the high efficiency of capillary electrophoresis (CE), and is a new type of micro-separation technology. It has the characteristics of fast separation and less consumption of samples and reagents. It is not only used for the separation and analysis of ionic compounds, but also for the separation and analysis of neutral compounds. [0003] Capillary column is the core of capillary electrochromatography separation and analysis, and the preparation of capillary column is the key of capillary electrochromatography. Capillary electrochromatographic colum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/22B01D15/20B01J20/281B01J20/30G01N30/60
CPCB01D15/20B01D15/22B01J20/281B01J2220/84B01J2220/86G01N30/6078
Inventor 张裕平许明录龚文君陈娜张毅军陈军李英杨靖华涂剑秋
Owner HENAN INST OF SCI & TECH
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