Preparation method of perfluorooctane sulfonic acid molecularly imprinted adsorbent on porous ceramic surface

A technology of perfluorooctane sulfonic acid and porous ceramics, applied in chemical instruments and methods, adsorption water/sewage treatment, other chemical processes, etc., can solve the uneven distribution of imprinted sites, reduce the utilization rate of imprinted sites, and templates Leakage mechanical properties and other issues, to achieve the effect of short elution time, excellent mechanical stability, good physical and chemical stability

Inactive Publication Date: 2019-03-15
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The device required by this method is simple and universal, but there are usually the following problems: (1) The controllability is poor during the grinding process, and some irregular particles are inevitably generated, and some imprinted spots are destroyed at the same time
The qualified particles obtained after sieving are generally less than 50%, resulting in obvious waste; (2) there are too deep embedding of template molecules, difficulty in elution, template leakage and low mechanical properties; (3) uneven distribution of imprinted sites , some of them are located above the particle pores, and their mass transfer rate is faster, while others are embedded in the polymer body, which is affected by steric hindrance, has poor accessibility, and the rate of recombining template molecules is slow, thereby reducing the number of imprinted sites. Utilization of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of porous ceramics: In the grinder, add ceramic powder: 40g, attapulgite powder: 40g, carbon powder: 10g, phenolic resin: 10g, turn on the grinder, grind for 30 minutes, take it out and place it at 90°C Dry in an oven for 8 hours, then place in a high-temperature furnace at 900°C for 6 hours, cool to room temperature, and grind to powder to obtain porous ceramic powder with a particle size between 40 and 60 mesh;

[0024] (2) Preparation of aminated porous ceramic powder: In the reactor, add ethanol: 76 mL, γ-aminopropyltriethoxysilane: 25 g, porous ceramic powder: 15 g, keep the temperature at 65±2°C, Stirring and reflux reaction for 4 h, after the reaction is completed, the solid-liquid separation, washing with ethanol, drying, to obtain aminated porous ceramic powder;

[0025] (3) Preparation of perfluorooctane sulfonic acid molecularly imprinted adsorbent on porous ceramic surface: In the reactor, add N,N-dimethylformamide: 66mL, succinimide: 18g, pe...

Embodiment 2

[0027] (1) Preparation of porous ceramics: In the grinder, add ceramic powder: 42g, attapulgite powder: 38g, carbon powder: 8g, phenolic resin: 12g, turn on the grinder, grind for 30 min, take it out and place it at 90°C Dry in an oven for 8 hours, then place in a high-temperature furnace at 900°C for 6 hours, cool to room temperature, and grind to powder to obtain porous ceramic powder with a particle size between 40 and 60 mesh;

[0028] (2) Preparation of aminated porous ceramic powder: In the reactor, add ethanol: 78mL, γ-aminopropyltriethoxysilane: 22g, porous ceramic powder: 16g, keep the temperature at 65±2℃ and stir , reflux reaction for 4 h, after the reaction is completed, separate the solid from the liquid, wash with ethanol, and dry to obtain an aminated porous ceramic powder;

[0029](3) Preparation of perfluorooctane sulfonic acid molecularly imprinted adsorbent on porous ceramic surface: In the reactor, add N,N-dimethylformamide: 69mL, succinimide: 15g, perfluor...

Embodiment 3

[0031] (1) Preparation of porous ceramics: In the grinder, add ceramic powder: 38g, attapulgite powder: 42g, carbon powder: 12g, phenolic resin: 8g, turn on the grinder, grind for 30 minutes, take it out and place it at 90°C Dry in an oven for 8 hours, then place in a high-temperature furnace at 900°C for 6 hours, cool to room temperature, and grind to powder to obtain porous ceramic powder with a particle size between 40 and 60 mesh;

[0032] (2) Preparation of aminated porous ceramic powder: In the reactor, add ethanol: 73 mL, γ-aminopropyltriethoxysilane: 24 g, porous ceramic powder: 18 g, keep the temperature at 65±2°C, Stirring and reflux reaction for 4 h, after the reaction is completed, the solid-liquid separation, washing with ethanol, drying, to obtain aminated porous ceramic powder;

[0033] (3) Preparation of perfluorooctane sulfonic acid molecularly imprinted adsorbent on porous ceramic surface: In the reactor, add N,N-dimethylformamide: 61mL, succinimide: 20g, per...

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Abstract

The present invention discloses a preparation method of a porous ceramic surface perfluorooctane sulfonic acid molecularly imprinted adsorbent. According to the preparation method, waste ceramic is used as the supporting body of an adsorbent, and perfluorooctane sulfonic acid is used as a template molecule; 58-65% by mass of N,N-dimethylformamide, 15-20% by mass of succinimide, 1.0-3.0% by mass of perfluorooctane sulfonic acid, 12-18% by mass of aminated porous ceramic powder, and 1.0-4.0% by mass of ammonium persulfate are added to a reactor, a stirring reaction is performed for 6 h at a temperature of 75+ / -2 DEG C in the absence of oxygen, the obtained product is subjected to stirring washing for 12 h with the mixed solution of ethanol and sodium hydroxide, the template molecule is removed, and drying is performed to obtain the porous ceramic surface perfluorooctane sulfonic acid molecularly imprinted adsorbent. According to the present invention, the porous ceramic surface perfluorooctane sulfonic acid molecularly imprinted adsorbent can specifically recognize perfluorooctane sulfonic acid, and has advantages of high selectivity, good mechanical property, good chemical stability, fast adsorption, easy elution, and regenerative capacity.

Description

technical field [0001] The invention relates to a preparation method and application technology of a molecularly imprinted adsorption material, in particular to a preparation method of a perfluorooctane sulfonic acid molecularly imprinted adsorbent on a porous ceramic surface, which belongs to the technical field of separation material application. Background technique [0002] Perfluorooctanesulfonic acid (PFOS) is an eight-carbon perfluorinated compound with a terminal sulfonate group (CF 3 (CF 2 ) 7 SO 3 H), usually an indispensable processing aid for the production of high performance fluoropolymers. These high-performance fluoropolymers can be widely used in aerospace technology, fire extinguishing agents, surfactants and other household products. Since the early 1980s, the application of this non-volatile perfluorinated organic compound in industrial and civil fields has grown rapidly. The extensive use of this type of product has caused it to enter various enviro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C02F101/34C02F101/36
CPCB01J20/103B01J20/12B01J20/20B01J20/22B01J20/268B01J20/28057B01J20/28088C02F1/285C02F2101/34C02F2101/36C02F2101/40
Inventor 李慧芝卢燕韩斌
Owner UNIV OF JINAN
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