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A kind of method for preparing melamine molecularly imprinted polymer by distillation precipitation polymerization

A technology of distillation precipitation polymerization and melamine, which is applied in the direction of chemical instruments and methods, and other chemical processes, can solve the problems of complex polymer components, etc., and achieve the effect of simple operation and easy control of preparation conditions

Inactive Publication Date: 2017-07-14
SHIHEZI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are disadvantages such as difficult removal of stabilizers such as surfactants and complex components of the prepared polymers.
Moreover, the maximum binding capacity of melamine molecularly imprinted polymers and melamine obtained by the above methods is less than 20 mg / g

Method used

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  • A kind of method for preparing melamine molecularly imprinted polymer by distillation precipitation polymerization
  • A kind of method for preparing melamine molecularly imprinted polymer by distillation precipitation polymerization
  • A kind of method for preparing melamine molecularly imprinted polymer by distillation precipitation polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Synthesis I of embodiment 1 MEL imprinted polymer

[0029] Dissolve 0.22 g of melamine (MEL), 0.60 mL of methacrylic acid, and 5.0 mL of divinylbenzene in 80 mL of acetonitrile, sonicate for 2 min to mix them evenly, and place them in a three-necked flask after standing in the dark for 12 h, then add Azobisisobutyronitrile 0.13 g, deoxygenated by argon for 5 minutes, stirred at a speed of 120 r / min and heated in a water bath at room temperature, heated to the boiling point of acetonitrile within about 30 minutes, and distillate was collected at this time. By controlling the temperature, the reaction was terminated when 40 mL of acetonitrile was evaporated within 1.5 to 2 h. The emulsion obtained by polymerization was ultrasonically and suction-filtered, and the filter residue was washed with methanol three times, then extracted in a Soxhlet extractor with methanol-acetic acid (9:1, v / v) for 24 h, and then rinsed with methanol Several times, drying in an oven at 50 ℃ to...

Embodiment 2

[0032] Example 2 Synthesis II of MEL imprinted polymer

[0033] The amount of methacrylic acid is 0.43 mL, the amount of divinylbenzene is 3.57 mL, other conditions are the same as in Example 1, and the obtained polymer is as follows image 3 Shown (B1 is MIPs, B2 is NIPs).

Embodiment 3

[0034] Example 3 Synthesis of MEL imprinted polymer III

[0035] Dissolve 0.22 g of melamine (MEL), 0.80 mL of methyl methacrylate, and 5.0 mL of divinylbenzene in 80 mL of acetonitrile, sonicate for 2 min to mix them evenly, and place them in a three-necked flask after standing in the dark for 12 h. Then add 0.19 g of benzoyl peroxide, pass through argon gas for deoxygenation for 5 minutes, stir at a speed of 120 r / min, start heating in a water bath at room temperature, and heat to the boiling point of acetonitrile within about 30 minutes. At this time, start to collect distillate. By controlling the temperature, the reaction was terminated when 40 mL of acetonitrile was evaporated within 1.5 to 2 h. Other conditions are with embodiment 1. The maximum binding capacity of the MEL imprinted polymer is 32.75 mg / g (the test method is the same as in Example 4).

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Abstract

The invention discloses a method for preparing a melamine molecularly imprinted polymer by virtue of distillation, precipitation and polymerization. The method comprises the following steps: (1) dissolving melamine, a polymerization reaction monomer and divinylbenzene in acetonitrile, and standing; (2) adding an initiating agent into the solution of the step (1), removing oxygen, and heating to distill acetonitrile; and (3) after the distillation in the step (2), filtering the reaction solution, performing refluxing extraction on filter residues by using a methanol-acetic acid mixed solution, and drying to obtain the melamine molecularly imprinted polymer. By adopting the method disclosed by the invention, the problems that the molecularly imprinted polymer obtained by the conventional method is non-uniform in particle size, difficult in size control and low in binding capacity; the method disclosed by the invention is simple to operate and does not need a complex after-treatment process, and the obtained molecularly imprinted polymer microspheres have good monodispersity and binding capacity of 32-44mg / g, and can be used for separating and detecting melamine in a sample.

Description

technical field [0001] The invention belongs to the field of molecularly imprinted polymers, in particular to a method for preparing melamine molecularly imprinted polymers through distillation precipitation polymerization. Background technique [0002] Melamine (MEL), commonly known as "protein essence", is an important nitrogen heterocyclic organic chemical raw material, with a nitrogen content of about 66%, which is much higher than the average nitrogen content of protein. Due to the defects of the protein content determination method, melamine is often mixed into food or feed by unscrupulous businessmen to improve the protein content index in food or feed testing. Animal experiments have shown that long-term intake of melamine can cause urinary stones and even bladder cancer. In 2008, the well-known infant milk powder poisoning incident was caused by the contamination of milk powder with melamine. The Ministry of Health and relevant departments jointly issued an announ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/06C08F220/14C08F212/36C08J9/26B01J20/26B01J20/30
Inventor 李迎春刘江陈文李乐刘媛宋含
Owner SHIHEZI UNIVERSITY
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