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Azos thermal initiator, synthetic method and application thereof

A technology of thermal initiator and synthesis method, applied in organic chemistry and other directions, can solve problems such as expensive and difficult to realize industrialized production, and achieve the effects of controllable initiation rate, high initiation efficiency and high grafting rate

Inactive Publication Date: 2009-03-11
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, expensive and complicated ultraviolet light reactors are difficult to realize industrial production

Method used

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  • Azos thermal initiator, synthetic method and application thereof
  • Azos thermal initiator, synthetic method and application thereof
  • Azos thermal initiator, synthetic method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Synthesis of intermediates of azo derivatives with hydroxyl groups at the end

[0037] Put 150ml of benzene, 150ml of ethylene glycol, and 22g of azobisisobutyronitrile into a 500ml flask. Under the condition of mechanical stirring, dry hydrogen chloride gas was introduced slowly and continuously, and reacted at 5°C for 10 hours. At the end of the reaction, the reactant turned into a white viscous liquid. Add 15g of ice cubes to the white viscous liquid and stir vigorously for 2 hours to fully hydrolyze it.

[0038] Use a separatory funnel to separate the viscous material in the lower layer, collect the upper benzene layer; then wash with 1200ml saturated sodium chloride solution for 3 times, then wash with 900ml saturated sodium bicarbonate solution for 3 times, add anhydrous magnesium sulfate to dry; The solvent benzene was evaporated under pressure, and then 20ml of methanol was added to precipitate a small amount of white oligomer. After the methanol was ...

Embodiment 2

[0039] Embodiment 2 prepares thermal initiator by intermediate

[0040] 4.0 ml of methacryloyl chloride, 6.0 g of the intermediate and 50 ml of benzene were added to a vessel equipped with a magnetic stirrer. Then, 3.6ml of pyridine was slowly added dropwise, and the dropping process was cooled with an ice-water bath. After the dropwise addition, the container was sealed and reacted at room temperature for three days.

[0041] The pyridinium salt was removed by filtration, washed three times with 900 ml of saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The crude product was separated and purified by silica gel column chromatography, and the eluent was a mixed solvent of benzene:acetone=2:1 (volume ratio). Finally, 0.9 g of product was obtained with a purity of 96%.

Embodiment 3

[0042] Example 3 Preparation of Thermal Initiator by Intermediate

[0043] In a container equipped with magnetic stirring, 4.8ml of pyridine was slowly dropped into 5.6ml of methacryloyl chloride, and the dropping process was cooled with an ice-water bath. Then add 43ml of acetone and accelerate the stirring to disperse the generated pyridinium salt evenly. Then slowly add 8.7g of the intermediate dropwise, and cool with an ice-water bath during the dropwise addition. After the dropwise addition, the container was sealed and reacted at room temperature for three days.

[0044] The pyridinium salt was removed by filtration, the acetone was evaporated under reduced pressure, and 50 ml of benzene was added as a solvent. Wash with 900 ml of saturated sodium chloride solution three times, and dry over anhydrous magnesium sulfate. The crude product was separated and purified by silica gel column chromatography, and the eluent was a mixed solvent of benzene:acetone=2:1 (volume rat...

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Abstract

The invention relates to an azo thermal initiator for use in preparation of a nano-sized spherical polyelectrolyte brush, a synthesis method and an application thereof. Firstly, azodiiso-alkylnitrile and diol are taken as raw materials to synthesize an intermediate azodiisoacid diol ester; and then the intermediate reacts with alkyl acrylyl chloride to obtain the novel azo thermal initiator with a C=C double bond as a terminal group. A novel azo thermal initiator both ends of which contain C=C double bonds can be obtained through the separation by a certain method. The thermal initiator can initiate the in-situ polymerization of monomers such as acrylic acid, 4-ethenyl-benzenesulfonic acid sodium salt and so on, on the surfaces of polystyrene milk globules to prepare the nano-sized spherical polyelectrolyte brush with controllable polyelectrolyte length and grafting density.

Description

technical field [0001] The present invention relates to a thermal initiator and its synthesis method and application, more specifically, relates to an azo thermal initiator. Background technique [0002] Polymer brushes are composed of many polymer chains fixed at one end on a solid surface and densely arranged. Because such brush-like structures can greatly modify surface properties, such as adhesion, lubricity, wettability, friction, biocompatibility, etc., they have broad application prospects in many fields. The charged polymer brushes formed on the surface of nanoscale emulsion particles are called nanospherical polyelectrolyte brushes. The nano-spherical polyelectrolyte brush not only has good stability and redispersibility, but also its size can be controlled by external conditions (such as temperature, pH value, ion concentration, etc.), while the internal counter ion concentration and pH value do not change with the external environment. And obviously changed. Th...

Claims

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Application Information

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IPC IPC(8): C08F4/04C07C245/02C08F285/00C08F257/02C08F222/22
Inventor 郭旭虹许军李莉房鼎业
Owner EAST CHINA UNIV OF SCI & TECH
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