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SPME extracting fiber of porous organic framework coating and preparation method of SPME extracting fiber

A technology of organic framework and extraction fiber, which is applied in the field of porous organic framework coated SPME extraction fiber and its preparation, can solve the problem of no aromatic type, etc., and achieve the effect of high specific surface area

Pending Publication Date: 2019-04-16
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no aromatic covalent organic framework material in the prior art, so it is of great significance to develop an aromatic covalent organic framework material that has a strong ability to enrich aromatic and amino target substances.

Method used

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  • SPME extracting fiber of porous organic framework coating and preparation method of SPME extracting fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of preparation method of the SPME extraction fiber of porous organic framework coating, comprises the following steps:

[0036] (1) Under nitrogen protection, add anhydrous aluminum chloride (3.5mmol) into a 100mL round bottom flask, and then inject 40mL of anhydrous CHCl 3 , and stirred at 60 °C for 3 hours.

[0037] (2) Dissolve 1,3,5-triphenylamine (1.5mmol) in 20mL anhydrous CHCl 3 .

[0038] (3) Inject the solution of step 2 into the system of step 1, and stir and react at 60° C. for 24 hours.

[0039] (4) After the reaction is completed, and the temperature of the system is lowered to room temperature, filter and wash with hydrochloric acid (1mol L -1 ), methanol, and acetone to wash and clean the product 3 times. Subsequently, the product was subjected to Soxhlet extraction with ethanol, tetrahydrofuran and chloroform in sequence, and the extraction time was 2 days.

[0040] (5) PAF-41 was obtained under vacuum at 80°C for 12 hours.

[0041] (6) Soak...

Embodiment 2

[0046] A kind of preparation method of the SPME extraction fiber of porous organic framework coating, comprises the following steps:

[0047] (1) Under the protection of nitrogen, anhydrous FeCl 3 (4.5mmol) was added to a 100mL round bottom flask, followed by injection of 40mL of anhydrous CHCl 3 , and stirred at 60 °C for 3 hours.

[0048] (2) Dissolve 1,3,5-triphenylamine (1.5mmol) in 20mL anhydrous CHCl 3 .

[0049] (3) Inject the solution of step 2 into the system of step 1, and stir and react at 60° C. for 24 hours.

[0050] (4) After the reaction is completed, and the temperature of the system is lowered to room temperature, filter and wash with hydrochloric acid (1mol L -1 ), methanol, and acetone to wash and clean the product 3 times. Subsequently, the product was subjected to Soxhlet extraction with ethanol, tetrahydrofuran and chloroform in sequence, and the extraction time was 2 days.

[0051] (5) PAF-41 was obtained under vacuum at 80°C for 12 hours.

[0052...

Embodiment 3

[0057] A kind of preparation method of the SPME extraction fiber of porous organic framework coating, comprises the following steps:

[0058] (1) Under the protection of nitrogen, the anhydrous CuCl 2 (0.8mmol) was added to a 200mL round bottom flask, followed by injection of 40mL of anhydrous CHCl 3 , and stirred at 75 °C for 3 hours.

[0059] (2) Dissolve 1,3,5-triphenylamine (10mmol) in 50mL anhydrous CHCl 3 .

[0060] (3) Inject the solution of step 2 into the system of step 1, and stir and react at 70° C. for 72 hours.

[0061] (4) After the reaction is finished, and the temperature of the system drops to room temperature, filter and wash with hydrochloric acid (3mol·L -1 ), methanol, and acetone to wash and clean the product 3 times. Subsequently, the product was subjected to Soxhlet extraction with ethanol, tetrahydrofuran and chloroform in sequence, and the extraction time was 1 day.

[0062] (5) PAF-41 was obtained under vacuum at 80°C for 12 hours.

[0063] (6...

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Abstract

The invention relates to SPME extracting fiber of a porous organic framework coating and a preparation method of the SPME extracting fiber. The SPME extracting fiber comprises a fiber carrier and a coating attached to the surface of the carrier, carrier fiber is base fiber with the surface subjected to hydroxylation, one end of the carrier fiber is coated with a coating material, and the coating material is a mixture of PAF-41 and glue. The PAF-41 is a porous organic framework material with a uniform micropore structure, a high specific surface area and a high aromatic property, the structurecharacteristics of the porous organic framework material have good affinity to fragrant volatile substances, the extracting efficiency of SPME can be improved, and therefore the sensitivity of targetdetection is improved.

Description

technical field [0001] The invention belongs to the technical field of sample analysis pretreatment, is an interdisciplinary subject of analytical chemistry and material chemistry, and specifically relates to a SPME extraction fiber with a porous organic skeleton coating and a preparation method thereof. Background technique [0002] Solid-phase microextraction (Solid-phase microextraction, SPME) technology is a sample pretreatment technology that integrates sampling, extraction, concentration and sample injection. It has been widely used in environmental engineering, biological engineering, pharmaceutical engineering and food engineering. The core of SPME technology lies in the extraction fiber (or extraction fiber), and the quality of the extraction fiber depends on the enrichment efficiency, selectivity and stability of the analyte by the extraction coating. Currently, commercialized SPME fibers are expensive and limited in variety. , The main components of the coating ar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08
CPCB01D15/08B01J20/22B01J20/28023B01J20/30
Inventor 李忠月张玉霞刘昆赵瑞奇
Owner YANTAI UNIV
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