Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Capillary monolithic column for separating benzologues and preparation method of capillary monolithic column

A technology of capillary monolithic columns and homologues, which is applied in the fields of analytical chemistry and environmental analysis, can solve problems such as difficult and efficient use of MOFs materials, and achieve good stability and good separation effect

Active Publication Date: 2019-01-18
HUBEI NORMAL UNIV
View PDF4 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are several problems in this method of embedding MOFs materials: First, due to the high surface energy and strong van der Waals force of MOFs materials, MOFs materials are prone to aggregation and separation.
Secondly, with the embedding method, most of the MOFs materials will be wrapped into the aggregated particles of the monolithic column, which makes it difficult to efficiently utilize the unique properties of MOFs materials

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Capillary monolithic column for separating benzologues and preparation method of capillary monolithic column
  • Capillary monolithic column for separating benzologues and preparation method of capillary monolithic column
  • Capillary monolithic column for separating benzologues and preparation method of capillary monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 Preparation of a capillary monolithic column for the separation of benzene homologues

[0024] 1. Synthesis of MOF-5:

[0025] 1. Using the classic hot solvent method, a certain amount of Zn(NO 3 ) 2 ·6H 2 O and H 2 BDC (terephthalic acid) is mixed, dissolved in an appropriate amount of DMF, shaken vigorously for 30 minutes and placed in a high-temperature and high-pressure reactor. After reacting at 120°C for 24 hours, the product was suction-filtered and washed three times with DMF, each time 15 mL, to remove unreacted reactants. Use CH again 2 Cl 2 (dichloromethane) for one day to remove the DMF in the guest molecule. Finally, the prepared MOF-5 was vacuum-dried at 120°C for 24 hours to obtain a white solid, which was characterized by XRD, SEM, and infrared.

[0026] Table 1 raw material consumption

[0027]

[0028] 2. The XRD spectrum of the prepared MOF-5 material is as follows figure 2 shown. It can be seen from the figure that the charac...

experiment example 1

[0044] Experimental example 1 Stability analysis of a capillary monolithic column used for separation of benzene homologues

[0045] When methanol is used as the mobile phase, the flow rate is from 0.02mL·min -1 to 0.06mL·min -1 There is a nice linear relationship between back pressure and flow rate, indicating that the permeability does not change with flow rate as in Figure 6 shown. When water is used as the mobile phase, the flow rate and back pressure also have a linear relationship and the R value reaches 0.99. Figure 7 shown. Bring the data into the permeability formula to calculate the permeability K as the following table:

[0046] Table 4-Physical data of each substance

[0047]

experiment example 2

[0048] Experimental example 2 detects the separation effect of homologues of benzene

[0049] 1. Connect the monolithic capillary column MOF-5@ploy(GMA-co-EDMA) (experimental group) and monolithic capillary column poly(GMA-co-EDMA) (control group) to HPLC (FL2200) respectively. The mobile phase was 75% methanol / 25% water, and the ultraviolet spectrum was used as the detector, and the flow rate was 0.02mL·min-1. Take 10 microliters each of 1% toluene (methanol:toluene=99:1, v / v), 1% benzene (methanol:benzene=99:1, v / v), 0.5% phenol (MeOH:Phenol=199: 1, v / v) Shake well in a centrifuge tube. Inject 20 μL of the mixed solution with a sampler and detect it with a 245nm ultraviolet detector.

[0050] 2. If Figure 8 As shown, the GMA-EDMA monolithic column without immobilized MOF-5 (control group) did not have any separation ability for the mixed solution, and only one peak appeared.

[0051] 3. If Figure 9 As shown, the monolithic column of immobilized MOF-5 material (experim...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a capillary monolithic column for separating benzologues and a preparation method of the capillary monolithic column. The preparation method comprises the following steps: dissolving GCC in ethanol, thus obtaining a mixed solution, adding a given amount of the mixed solution into a sample bottle with MOF-5, and injecting obtained suspension into a ploy(GMA-co-EDMA) monolithic column activated by ethylenediamine, thus obtaining the capillary monolithic column MOF-5@ploy(GMA-co-EDMA). The MOF-5 is solid loaded onto the surface of the GMA-EDMA monolithic column by virtue of a surface covalent solid loading method, MOF-5 is dispersed in the DCC and ethanol mixed solution, the epoxy functional group on the surface of the PMMA is opened by virtue of the ethylenediamine, the MOF-5 is covalently immobilized onto the surface of the polymer in the monolithic column, the MOF-5 is covalently connected with the monolithic column, so that the gathering and separation phenomenon of the MOFs material can be avoided, and the properties of the MOFs material can be prevented from being severely influenced.

Description

technical field [0001] The invention relates to the technical fields of analytical chemistry and environmental analysis, in particular to a capillary integral column for separating benzene homologues and a preparation method thereof. Background technique [0002] Solid phase microextraction (SPME) is a new type of sample pretreatment technology, which was first proposed by the Pawliszyn research group in Canada in 1989. This technology integrates sampling, extraction, enrichment and sample injection, does not consume solvents, and can be used online with other instruments. It has developed rapidly in less than 20 years, and various types of extraction media have emerged continuously. . The basic principle of SPME is to immobilize the coating material with adsorption function on the surface of a certain matrix fiber by physical or chemical methods, make direct or indirect contact with the sample, enrich and concentrate the target analyte, and combine it with The sample inje...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): B01D15/10
CPCB01D15/10
Inventor 吴帅宾谢一铭
Owner HUBEI NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com