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Preparation method of XDI molecular imprinting solid phase extraction column filling material

A solid-phase extraction column and molecular imprinting technology are applied in the field of preparation of m-xylylene isocyanate molecularly imprinted solid-phase extraction filling materials, which can solve the problem that plastic products cannot enter the EU market, and achieve good results.

Inactive Publication Date: 2017-08-18
邵秋荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is understood that the European Union has continuously upgraded the technical trade regulations on food contact materials in recent years, which will have a long-term impact on our export enterprises. Plastic products that do not meet the requirements of the new regulations will not be able to enter the EU market.

Method used

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  • Preparation method of XDI molecular imprinting solid phase extraction column filling material

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Experimental program
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Effect test

Embodiment 1

[0019] The preparation of m-xylylene dimethyl isocyanate molecularly imprinted solid-phase extraction column packing material, the specific raw material dosage is shown in Table 1.

[0020] Table 1 Reaction raw materials and dosage

[0021] Reaction material Molecular weight (g / mol) Reaction dosage m-xylylene isocyanate 166.17 43.1mg Methacrylate 86.09 104.3mg Ethylene glycol dimethacrylate 198.22 1.89 mL Dibenzoyl peroxide 242.23 73mg Porogen (ethyl acetate) 88.11 18mL

[0022] 1. the reaction raw material template molecule m-xylylene isocyanate, functional monomer methacrylic acid, cross-linking agent ethylene glycol dimethacrylate and porogen ethyl acetate are added successively according to the consumption of table 1 Put it into a two-neck bottle with a grinding mouth, ultrasonic 35min, mix evenly, then add 73mg of dibenzoyl peroxide, ultrasonic degassing for 15min, nitrogen gas for 35min, seal it, react in 40℃ oil b...

Embodiment 2

[0025] The preparation of m-xylylene dimethyl isocyanate molecularly imprinted solid-phase extraction column packing material, the specific raw material consumption is shown in Table 2.

[0026] Table 2 Reaction raw materials and dosage

[0027] Reaction material Molecular weight (g / mol) Reaction dosage m-xylylene isocyanate 166.17 43.1mg Methacrylate 86.09 125mg Ethylene glycol dimethacrylate 198.22 2.83 mL Dibenzoyl peroxide 242.23 73mg Porogen (ethyl acetate) 88.11 40mL

[0028] 1. Add reaction raw material template molecule m-xylylene dimethyl isocyanate, functional monomer methacrylic acid, crosslinking agent ethylene glycol dimethacrylate and porogen acetonitrile and water to the grinding port in turn according to the consumption in Table 2 In a two-neck bottle, ultrasonic 35min, after mixing evenly, then add 73mg of dibenzoyl peroxide, ultrasonic degassing 15min, nitrogen gas 35min, seal, react in 80 ℃ oil bath fo...

Embodiment 3

[0031] The preparation of m-xylylene dimethyl isocyanate molecularly imprinted solid-phase extraction column packing material, the specific raw material dosage is shown in Table 3.

[0032] Table 3 Reaction raw materials and dosage

[0033] Reaction material Molecular weight (g / mol) Reaction dosage m-xylylene isocyanate 166.17 43.1mg Methacrylate 86.09 125mg Ethylene glycol dimethacrylate 198.22 2.83 mL Dibenzoyl peroxide 242.23 61mg Porogen (ethyl acetate) 88.11 40mL

[0034] 1. Add the reaction raw material template molecule m-xylylene dimethyl isocyanate, functional monomer methacrylic acid, crosslinking agent ethylene glycol dimethacrylate and porogen ethyl acetate to the grinding port in sequence according to the dosage in Table 3 In a two-neck bottle, ultrasonic 30min, after mixing evenly, then add 61mg of dibenzoyl peroxide, ultrasonic degassing 15min, nitrogen gas 35min, seal, react in 60 ℃ oil bath for 24h, to o...

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Abstract

The invention relates to the field of food contact material detection safety, in particular to a preparation method of an m-Xylylene diisocyanate (XDI for short) molecular imprinting solid phase extraction column filling material. The method comprises the steps of adding reactive raw material template molecules XDI, methacrylic acid and a cross-linking agent EGDMA into a pore-foaming agent ethyl acetate, mixing evenly, and then adding an initiator dibenzoyl peroxide; maintaining the molar ratio of the template molecules to functional monomers to the cross-linking agent to be 1 to (4-6) to (40-60), degassing, charging nitrogen, and then sealing, reacting for 20-48hr at the temperature of 40-80 DEG C, and obtaining a crude molecular imprinting polymer; grinding the polymer until the particle sizes are 35-80mu m, performing Soxhlet extraction by using a mixed solvent of methyl alcohol, acetic acid and water, and then removing the methyl alcohol and the acetic acid by using acetonitrile to rinse repeatedly until reaching neutrality; and finally, settling repeatedly by using acetone to remove fine particles, and thus obtaining the XDI molecular imprinting solid phase extraction column filling material. By the molecular imprinting solid phase extraction column detection, the XDI can be separated and concentrated simply, conveniently, efficiently and specifically.

Description

technical field [0001] The present invention relates to a method in the technical field of food safety, specifically, it relates to the highly selective separation, purification, A method for preparing enriched m-xylylene dimethyl isocyanate molecularly imprinted solid-phase extraction filling material. Background technique [0002] m-xylylene isocyanate, the structural formula is as follows: [0003] [0004] Recently, the European Commission officially released the latest regulation (EU) 2015 / 174 on plastic products in contact with food. take effect. It is understood that the European Union has continuously upgraded the technical trade regulations on food contact materials in recent years, which will have a long-term impact on our export companies. Plastic products that do not meet the requirements of the new regulations will not be able to enter the EU market. Export enterprises should pay close attention to building a quality assurance system centered on "purchase ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30B01D15/20C08F220/06C08F222/14G01N30/02G01N30/06
CPCB01D15/206B01J20/268C08F220/06G01N30/02G01N30/06G01N2030/062C08F222/102
Inventor 邵秋荣方邢有孟昭建李天宝
Owner 邵秋荣
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