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Preparation method of inorganic nanoparticle/polymer-based composite monolithic column

A technology of inorganic nanoparticles and polymers, applied in separation methods, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve the problems of easy agglomeration and thermodynamic instability, and achieve scientific and reasonable preparation methods and long service life. , the effect of improving dispersion

Inactive Publication Date: 2015-11-04
HEBEI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing an inorganic nanoparticle / polymer-based composite monolithic column, to develop a monolithic column of a new material, and to solve the problem of thermodynamic instability and easy occurrence of existing inorganic nanoparticles used to prepare monolithic columns. reunion problem

Method used

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  • Preparation method of inorganic nanoparticle/polymer-based composite monolithic column
  • Preparation method of inorganic nanoparticle/polymer-based composite monolithic column
  • Preparation method of inorganic nanoparticle/polymer-based composite monolithic column

Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) Using the mixed acid reflux oxidation method, prepare a mixed acid solution with concentrated nitric acid (mass ratio concentration of 98%) and concentrated sulfuric acid (mass ratio concentration of 65%) at a volume ratio of 1:3, and take 2.0g of nano-diamonds into a 150mL flask , then add 80mL of the mixed acid solution, disperse under ultrasonic conditions for 30 min, reflux at 135°C for 8 h under magnetic stirring, centrifuge (12000 rpm, 10 min), discard the supernatant, wash three times with absolute ethanol, 110 Dry at ℃ for 24 hours to obtain carboxylated nano-diamonds;

[0023] (2) Take 1.0 g of dried carboxylated nanodiamonds in a flask, add 40 mL of thionyl chloride, add 100 μL of dimethylformamide as a catalyst, ultrasonically disperse for 1 h, and reflux at 90 ° C for 4 h under magnetic stirring , centrifuge the reacted mixed solution (12000 rpm, 10min), discard the supernatant, wash 4 times with tetrahydrofuran to obtain acyl chloride nanodiamonds; put ...

Embodiment 2

[0027] (1) Using the mixed acid reflux oxidation method, prepare a mixed acid solution with concentrated nitric acid and concentrated sulfuric acid at a volume ratio of 1:3, take 2.0g of nano-diamonds into a 150mL flask, then add 60mL of the mixed acid solution, and disperse under ultrasonic conditions for 35 minutes. Reflux at 135°C for 10 h under magnetic stirring, centrifuge (12000 rpm, 10 min), discard the supernatant, wash with absolute ethanol three times, and dry at 110°C for 24 h to obtain carboxylated nano-diamonds;

[0028] (2) Take 1.0 g of dried carboxylated nanodiamonds in a flask, add 30 mL of thionyl chloride, add 100 μL of dimethylformamide as a catalyst, ultrasonically disperse for 1 h, and reflux at 90 ° C for 5 h under magnetic stirring , centrifuge the reacted mixed solution (12000 rpm, 10min), discard the supernatant, wash 4 times with tetrahydrofuran to obtain acyl chloride nano-diamonds; put the acyl chloride nano-diamonds into 40mL of anhydrous tetrahydr...

Embodiment 3

[0032] (1) Using the mixed acid reflux oxidation method, prepare a mixed acid solution with concentrated nitric acid and concentrated sulfuric acid at a volume ratio of 1:3.5, take 2.0 g of nano-diamonds into a 150 mL flask, then add 100 mL of the mixed acid solution, and disperse under ultrasonic conditions for 40 min. Reflux at 145°C for 8 h under magnetic stirring, centrifuge (12,000 rpm, 10 min), discard the supernatant, wash with absolute ethanol three times, and dry at 110°C for 24 h to obtain carboxylated nano-diamonds;

[0033] (2) Take 1.0 g of carboxylated nano-diamond after drying in a flask, add 50 mL of thionyl chloride, add 100 μL of dimethylformamide as a catalyst, ultrasonically disperse for 1 h, and reflux at 90 ° C for 6 h under magnetic stirring , centrifuge the reacted mixed solution (12000 rpm, 10min), discard the supernatant, wash 4 times with tetrahydrofuran to obtain acyl chloride nanodiamonds; put the prepared acyl chloride nanodiamonds into 40mL of anh...

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Abstract

The invention discloses a preparation method of an inorganic nanoparticle / polymer-based composite monolithic column. The method comprises the following steps: (a) concentrated nitric acid and concentrated sulfuric acid are mixed; nano-diamond is added; a reflux reaction is carried out, and drying is carried out, such that carboxylated nano-diamond is obtained; (b) the carboxylated nano-diamond is mixed with thionyl chloride; a catalyst is added; ultrasonic treatment and a reflux reaction are carried out; centrifugation is carried out; and washing is carried out, such that acyl chlorinated nano-diamond is obtained; (c) the acyl chlorinated nano-diamond is mixed with anhydrous propenol and pyridine; a reflux reaction is carried out; centrifugation is carried out; and washing and drying are carried out, such that a polymerization monomer is obtained; (d) the polymerization monomer, glycol diacrylate, dodecanol, and benzoyl peroxide are mixed; and ultrasonic treatment is carried out; N,N-dimethylaniline is added, and the mixture is well mixed; the mixture is poured into a stainless steel column; a reaction is carried out under room temperature; a high-pressure delivery pump is connected; and flushing and drying are carried out, such that the inorganic nanoparticle / polymer-based composite monolithic column is obtained. The method has the advantages of simple process, mild reaction condition and good operability. The prepared monolithic column has uniform framework and pore size and good separation performance. The monolithic column is suitable for separating relatively complex samples.

Description

technical field [0001] The invention relates to a preparation method of an online solid-phase extraction monolithic column, in particular to a preparation method of an inorganic nanoparticle / polymer-based composite monolithic column. Background technique [0002] Monolithic column is a continuous stationary phase obtained by in-situ polymerization in a chromatographic column by an organic or inorganic polymerization method. It has the advantages of simple preparation, fast separation speed, good reproducibility, low back pressure, and excellent porosity. Advantages, so as to achieve efficient and rapid separation of samples. With the maturity of monolithic column preparation technology, monolithic column materials used in HPLC separation and analysis have developed rapidly and become a new generation of chromatographic separation materials. However, there are fewer types of material matrices and polymerization systems in the column, which limits its popularization and applic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/20B01D15/22
Inventor 刘海燕王凤青闫宏远
Owner HEBEI UNIVERSITY
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