Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Functionalized azo initiator for free radical polymerization as well as preparation and application methods thereof

An azo initiator and free radical technology, which is applied in the field of functionalized azo initiator for free radical polymerization and its preparation and application, can solve problems such as instability, and achieve an increase in the absorption coefficient and a stable molecular structure Effect

Inactive Publication Date: 2014-06-25
WUHAN UNIV OF TECH
View PDF2 Cites 7 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the ester group in the molecule, the molecule is extremely unstable in alcohol or amine solutions

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Functionalized azo initiator for free radical polymerization as well as preparation and application methods thereof
  • Functionalized azo initiator for free radical polymerization as well as preparation and application methods thereof
  • Functionalized azo initiator for free radical polymerization as well as preparation and application methods thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Initiator synthesis process:

[0040] (1) Synthesis of methylmalonamide

[0041] At room temperature, 172 mL (1 mol) of diethyl methylmalonate was poured into 200 mL of 27% ammonia water, and stirred at 45°C for 15 hours. When the solution became clear, it was cooled to 0°C to crystallize the product. The product was filtered and washed 2 times with methanol. After recrystallization in water, the product was dried under vacuum and the product weighed 33 g of colorless crystals (yield about 28%).

[0042] Product melting point: 208.9-209.2°C (222:209°C); infrared (IR, KBr) characteristic peak positions: 3353-3177, 2994, 2942, 1678cm -1 ; 1 H NMR (DMSO, ppm): 7.2, 7.4 (s, 4H, NH 2 ), 3.2(q, 1H, CH), 1.3(d, 3H, CH 3 ).

[0043] (2) Synthesis of methylmalononitrile

[0044] Take 8g (0.068mol) of methylmalonamide and 36g (0.296mol) of phosphorus pentoxide and mix them in a three-necked flask, and connect the three-necked flask to the distillation device. The system ...

Embodiment 2

[0056] Fabrication of Polymethacrylic Acid (PMAA) "Micropatterns"

[0057] First, the silicon wafer is used as the substrate, and the initiator dimethylchlorosilyl-3-ethylbenzazomethylmalononitrile (CSAM) is fixed on the surface of the substrate. The fixation steps are as follows:

[0058] At room temperature, put the initiator and the silicon substrate into the Schlenk tube at the same time, use toluene as the solvent, and blow nitrogen to remove oxygen. The concentration of the initiator is 0.5mmol / L (the concentration of the initiator in toluene), add a few drops (0.5 ~ 2ml) of triethylamine as a catalyst, keep it overnight, take it out, and use toluene, methanol, acetone to dissolve the unfixed initiator and The by-products are extracted and dried under vacuum.

[0059] After the initiator is fixed, monomers can be added to initiate polymerization. In order to realize the production of "micropatterns", two ways are provided here, as follows:

[0060] The first one: cover...

Embodiment 3

[0065] Synthesis of polystyrene (PS)

[0066] Take 1.079g (3.5mmol) of the synthesized initiator dimethylchlorosilyl-3-ethylbenzazomethylmalononitrile (CSAM), and add it to a mixed solution of 300mL styrene monomer and toluene (benzene The volume ratio of ethylene to toluene is 1:1), after 5 cycles of freezing-vacuum-thawing to remove the air inside, the mixed solution after removing the air is subjected to free radical polymerization under the protection of nitrogen at 60°C, the polymerization reaction The time is 1.5 to 14 hours. After the polymerization is completed, the polymer is washed with methanol to remove residual monomers. The product was then dissolved in benzene and freeze-dried to obtain a solid product.

[0067] Tested by GPC, the molecular weight of the polymerized product is 1×10 4 ~1×10 6 .

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Melting pointaaaaaaaaaa
Melting pointaaaaaaaaaa
Login to View More

Abstract

The invention relates to a functionalized azo initiator, that is, dimethylchlorosilane-3-ethylbenzene azo methyl malononitrile for free radical polymerization as well as preparation and application methods thereof. The preparation steps comprise the following parts: 1, synthesis for methylmalonamide; 2, synthesis for methylmalononitrile; 3, synthesis for 3-amino styrene; 4, synthesis for 3-(azo methyl malononitrile) styrene; 5, synthesis for dimethylchlorosilane-3-ethylbenzene azo methyl malononitrile. The product synthesised by the method disclosed by the invention is dimethylchlorosilane with a single-functional end, the functional group is capable of being reacted with some groups on the surfaces of some substrates, and forming a monomolecular layer fixed by a covalent bond; another functional group of the initiator is an azo bond and capable of initiating monomers containing double bonds to carry out free radical polymerization. In such a way, a macromolecular layer or a macromolecular brush is formed on the surfaces of the substrates respectively, and the functionalized azo initiator is wide in prospect in the aspect of ordered macromolecular synthesis and application.

Description

technical field [0001] The invention relates to a functionalized azo initiator for radical polymerization-dimethylchlorosilyl-3-ethylbenzazomethylmalononitrile and its preparation and application method. Background technique [0002] At present, ordered structure is a major trend in polymer synthesis, but it is very difficult to change the microstructure of the polymer after the polymer polymerization is completed. So researchers began to explore the direct formation of ordered structures in the polymer polymerization process. For example, a porous material is used as a template to carry out a polymerization reaction in the micropores. After the reaction, the template is selectively dissolved with a relevant solvent to obtain an array-type polymer with an ordered structure. This is a way to synthesize polymers with ordered structures. [0003] Later, the emergence of multifunctional initiators provided a new way for the synthesis of polymers with ordered structures. With ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08F4/04C08F292/00C07F7/12C04B41/48
Inventor 张海宁冯军
Owner WUHAN UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com