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

Method for preparing methyl methacrylate-acrylic acid block polymer with the existence of 1, 1-diphenylethylene

A technology of methyl methacrylate and diphenylethylene, applied in the field of polymer chemistry, can solve problems such as the preparation of methyl methacrylate-acrylic acid block polymer, which is beneficial to industrial production and avoids hydrolysis. , the effect of simple operation steps

Inactive Publication Date: 2009-09-30
CHINA PETROLEUM & CHEM CORP +1
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there have been no reports on the preparation of methyl methacrylate-acrylic acid block polymers using the polymerization system in the presence of DPE

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
  • Method for preparing methyl methacrylate-acrylic acid block polymer with the existence of 1, 1-diphenylethylene
  • Method for preparing methyl methacrylate-acrylic acid block polymer with the existence of 1, 1-diphenylethylene
  • Method for preparing methyl methacrylate-acrylic acid block polymer with the existence of 1, 1-diphenylethylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Add 20.0 g of monomer methyl methacrylate (0.2 mol), initiator azobisisobutyronitrile 196.8 mg (1.2 mmol) and 1,1-diphenylethylene 324 mg (1.8 mmol) to In a single-branch tube reaction flask containing a magnetic stirring rotor, after reacting at 70°C for 3 hours, the reaction was stopped and the reaction system was poured into methanol for precipitation, filtered and dried, and the PMMA precursor obtained was re-dissolved with chloroform and precipitated with methanol. To remove the unreacted monomer, initiator and 1,1-diphenylethylene, the obtained polymer powder was placed in a vacuum oven for 24 hours; the conversion rate of the monomer measured by the weighing method was 19%, and the molecular weight and molecular weight distribution of the product obtained : Mn=12900, PDI=1.45;

[0019] 2) Add 0.5g PMMA precursor, 2.5g acrylic acid and 20mL 1,4-dioxane into a single-branch tube reaction flask containing a magnetic stirring rotor, mix well and polymerize acrylic mon...

Embodiment 2

[0022] 1) Add 20.0 g of methyl methacrylate (0.2 mol), 131.2 mg (0.8 mmol) of azobisisobutyronitrile catalyst, and 216 mg (1.2 mmol) of 1,1-diphenylethylene to the magnetic stirring In the single-branch tube reaction flask of the rotor, react at 80℃ for 3h, stop the reaction and pour the reaction system into methanol for precipitation, filter and dry, redissolve the PMMA precursor obtained with chloroform, and precipitate with methanol to remove Unreacted monomer, initiator and 1,1-diphenylethylene, and the resulting polymer powder is placed in a vacuum oven for 24 hours. The conversion rate of the monomer measured by the weighing method is 22%, and the product is 1 The H NMR spectrum is shown as figure 1 As shown, no impurities were seen. The molecular weight and molecular weight distribution were determined by gel permeation chromatography, and narrow-distributed polystyrene was used as a standard sample. The results obtained: Mn=13400, PDI=1.40.

[0023] 2) Add 0.5g PMMA precur...

Embodiment 3

[0026] 1) Add 20.0 g of methyl methacrylate (0.2 mol), 196.8 mg (1.2 mmol) of azobisisobutyronitrile catalyst and 324 mg (1.8 mmol) of 1,1-diphenylethylene to the magnetic stirring In the single-branch tube reaction flask of the rotor, react at 80℃ for 3h, stop the reaction and pour the reaction system into methanol for precipitation, filter and dry, redissolve the PMMA precursor obtained with chloroform, and precipitate with methanol to remove Unreacted monomer, initiator and 1,1-diphenylethylene, and the resulting polymer powder is placed in a vacuum oven for 24 hours. The conversion rate of the monomers measured by the weighing method was 21%, and the molecular weight and molecular weight distribution of the obtained product: Mn = 11700, PDI = 1.36;

[0027] 2) Add 0.5g PMMA precursor, 0.5g acrylic acid and 20mL 1,4-dioxane into a single-tube reaction flask containing a magnetic stirring rotor, mix well and polymerize acrylic monomers under nitrogen protection, the reaction tem...

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

No PUM Login to View More

Abstract

The invention relates to a method for preparing methyl methacrylate-acrylic acid block polymer with the existence of 1, 1-diphenylethylene, which belongs to the field of high polymer chemistry. The invention solves the problems of complex polymerization systems, severe reaction conditions, fussy operation steps and inconvenience for industrial production in the prior PMMA-b-PAA preparation method. The method comprises the following steps: free radicals of MMA are polymerized to prepare a PMMA precursor with a special semiquinone structure and controllable molecular weight by taking AIBN as an evocating agent with the existence of little DPE; the polymerization of acrylic acid monomer is directly carried out with the existence of PMMA; and the polymerization systems are separated to obtain a PMMA-b-PAA amphipathic block polymer. The invention has the advantages of simple components of the DPE polymerization system, and same reaction conditions with common free radical polymerization and simple operation steps, directly carries out the polymerization of AA monomers, avoids the hydration to polyacrylic acid tert-butyl ester chain segment and is more beneficial to industrial production.

Description

Technical field [0001] The invention belongs to the field of polymer chemistry, and particularly relates to a C08L polymer compound composition, and more particularly to a method for preparing block polymers in the presence of 1,1-diphenylethylene (DPE). Background technique [0002] Methyl methacrylate-acrylic acid amphiphilic block polymer (PMMA-b-PAA) because its hydrophilic segment polyacrylic acid is a weak polyelectrolyte, the degree of ionization can be controlled by the pH value and the ionic strength of the solution, making it slow in the drug Interpretation and other fields have broad application prospects. The basic preparation method is the living polymerization stepwise feeding method using the group-protected monomer tert-butyl acrylate (tBA): Teyssié et al. used tetrahydrofuran as the solvent, and used the stepwise feeding method to carry out the monomer at -78°C. Living anionic polymerization of methyl methacrylate (MMA) and tBA to obtain the block polymer PMMA-bP...

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): C08F220/14C08F220/06
Inventor 付志峰陈冬石艳
Owner CHINA PETROLEUM & CHEM CORP
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