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A kind of preparation method and application of nitroxide free radical polymer brush inhibitor

A nitroxide free radical, polymer brush technology, applied in fatty acid esterification, organic chemistry, chemical recycling and other directions, can solve problems such as difficult recycling and reuse, prevent self-polymerization reaction, light color, and avoid gel phenomenon Effect

Active Publication Date: 2016-06-29
廊坊市安次区调河头振达生物技术推广中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the technical problem that the existing small molecule polymerization inhibitors are difficult to recycle and reuse when used in the synthesis of epoxy soybean oil acrylate, and provides: (1) A method of loading TEMPO on a polymer brush to prepare nitrogen and oxygen free (2) a method of applying the nitroxide free radical polymer brush inhibitor prepared above to the synthesis of epoxy soybean oil acrylate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Disperse 5 g of PS-OH (containing 1.5 mmol of hydroxyl groups on the surface) in 35 ml of N,N-dimethylformamide (DMF), perform ultrasonic vibration to make the two evenly dispersed, and place a thermometer, magnetic stirring rotor, constant Add the above mixture and 1.65mmol triethylamine into the 50ml three-necked flask with a separating funnel, and continuously feed N 2 protection, then 8ml of DMF and 1.65mmol of 2-bromoisobutyryl bromide were mixed and slowly added through a constant pressure dropping funnel. Under ice-water bath, react for 2h, and continue to react for 24h at room temperature. Pour it into 150ml of absolute ethanol for centrifugation, and dry at 60°C to obtain PS-Br. The loading amount of the initiator is 0.25mmol / g microspheres.

[0033] (2) After mixing copper bromide and 30ml solvent anisole, perform ultrasonic vibration to disperse the two evenly, then add it to a 50ml three-necked flask for stirring, and continuously feed N 2For protectio...

Embodiment 2

[0036] (1) Disperse 5g of PS-OH (containing 1.5mmol of hydroxyl groups on the surface) in 35ml of DMF, perform ultrasonic vibration to disperse the two evenly, and add the above mixture to a 50ml three-neck flask equipped with a thermometer, magnetic stirring rotor, and constant pressure separatory funnel and 3mmol triethylamine, continuous feeding of N 2 protection, and then 8ml of DMF and 3mmol of 2-bromoisobutyryl bromide were mixed and slowly added through a constant pressure dropping funnel. Under ice-water bath, react for 1 h, and continue to react for 12 h at room temperature to end. Pour it into 150ml of absolute ethanol for centrifugation, and dry at 60°C to obtain PS-Br. The loading amount of the initiator is 0.29mmol / g microspheres.

[0037] (2) After mixing copper bromide and 30ml solvent anisole, perform ultrasonic vibration to disperse the two evenly, then add it to a 50ml three-necked flask for stirring, and continuously feed N 2 For protection, add the monome...

Embodiment 3

[0043] Add 120g of epoxidized soybean oil and PS-PGMA-TEMPO loaded with 0.15% TEMPO into a 500ml three-necked flask, heat the oil bath to 110°C under mechanical stirring, and then feed 28g of acrylic acid steadily at a feeding rate of 10.67ml / h with a peristaltic pump And a mixture of 1.5% triphenylphosphine, the feeding time is 2.5h. After the feed was completed, the reaction was continued at a constant temperature of 120° C. for 6 h. During the reaction process, the acid value of the system was measured, and the acid value was less than or equal to 5 mgKOH / g when the heating was stopped. The reaction product was naturally cooled to room temperature to obtain light yellow transparent viscous oily epoxy soybean oil acrylate. Filter to recover PS-PGMA-TEMPO. The performance test results of epoxy soybean oil acrylate are shown in Table 1.

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Abstract

The invention relates to a preparation method of a nitroxide free radical polymer brush inhibitor and its application in the synthesis of epoxy soybean oil acrylate. The preparation method is to first adopt electron transfer regeneration catalyst atom transfer radical polymerization technology on the surface of cross-linked polystyrene microspheres, graft polyglycidyl methacrylate polymer brushes; Bonded thereon, a nitroxide radical polymer brush is obtained. Said application is to use nitroxide free radical polymer brush as the main polymerization inhibitor, and the small molecular polymerization inhibitor as auxiliary polymerization inhibitor to form a composite polymerization inhibition system to prepare epoxy soybean oil acrylate. The composite inhibitory system can not only have high-efficiency polymerization inhibitory effect in the preparation of epoxy soybean oil acrylate, but also is easy to recycle the main inhibitory agent nitroxide free radical polymer brush, so that it can be recycled, and a small amount of auxiliary inhibitory agent remains In the system, it can also prevent the self-aggregation of the product during storage.

Description

technical field [0001] The invention belongs to the technical field of nitroxide radical polymerization inhibitors, and in particular relates to a preparation method of a nitroxide radical polymer brush and its application in the synthesis of epoxy soybean oil acrylate. Background technique [0002] Sustainable development is still an important issue in the world today. With the decreasing oil resources, various countries are actively researching and developing new materials and new energy sources. Finding and developing the utilization of renewable resources has become a development trend in future material research, among which the development and utilization of vegetable oil is an important direction. Vegetable oil has many advantages: such as low cost, large output, rich chemical active points in structure, etc. Epoxy soybean oil acrylate is an epoxy acrylate resin synthesized based on epoxy soybean oil and acrylic acid. Acrylated epoxy soybean oil has low viscosity, l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F257/02C08F220/32C08F8/30C07D303/42C11C3/08
CPCY02P20/584
Inventor 刘少杰褚晓萌赵风清胡倩倩刘洪杰张志国李配欣
Owner 廊坊市安次区调河头振达生物技术推广中心
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