Method for preparing branched polyacrylonitrile

A branched polyacrylonitrile and branched monomer technology, which is applied in the directions of chemical characteristics of fibers, single-component synthetic polymer rayon, textiles and papermaking, etc. Easy operation, simple and easy preparation method, high monomer conversion rate

Active Publication Date: 2013-10-30
溧阳常大技术转移中心有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because there is no fundamental breakthrough in the synthesis of vinyl branched polymers, so far no real scale application has been achieved.

Method used

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  • Method for preparing branched polyacrylonitrile
  • Method for preparing branched polyacrylonitrile
  • Method for preparing branched polyacrylonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Acrylonitrile (4.6647g, 0.088mol), vinyl acetate (0.9463g, 0.011mol), branched monomer mercaptopropionyloxyethyl methacrylate (0.0436g, 0.2mmol), initiator AIBN (0.1643g , 1mmol) and the solvent DMF (18.1425g) were added into the reaction flask, and reacted at 60°C for 35 hours. The measured conversion rate of acrylonitrile was 95.5%, and the conversion rate of vinyl acetate was 82.4%. The polymer was analyzed by three-detection gel permeation chromatography, and the results were as follows: light scattering weight average molecular weight M w.MALLS =30400, molecular weight distribution PDI=1.93, Mark-Houwink index α =0.602, average branching factor g '=0.66, confirming that the obtained polymer has a branched structure. The trends of intrinsic viscosity and branching factor with molecular weight are shown in figure 1 with Figure 4 .

Embodiment 2

[0019] Acrylonitrile (4.6611g, 0.088mol), vinyl acetate (0.9471g, 0.011mol), branched monomer mercaptopropionyloxyethyl methacrylate (0.0868g, 0.4mmol), initiator AIBN (0.1641g , 1mmol) and the solvent DMF (18.1405g) were added to the reaction flask, and reacted at 60°C for 35 hours. The measured conversion rate of acrylonitrile was 94.4%, and the conversion rate of vinyl acetate was 78.3%. The polymer was analyzed by three-detection gel permeation chromatography, and the results were as follows: light scattering weight average molecular weight M w.MALLS = 27700, molecular weight distribution PDI = 1.66, Mark-Houwink index α =0.590, average branching factor g ' = 0.62, confirming that the obtained polymer has a branched structure.

Embodiment 3

[0021] Acrylonitrile (4.6655g, 0.088mol), vinyl acetate (0.9451g, 0.011mol), branched monomer mercaptopropionyloxyethyl methacrylate (0.1305g, 0.6mmol), initiator AIBN (0.1647g , 1mmol) and the solvent DMF (18.1385g) were added to the reaction flask, and reacted at 60°C for 40 hours. The measured conversion rate of acrylonitrile was 99.1%, and the conversion rate of vinyl acetate was 86.8%. The polymer was analyzed by three-detection gel permeation chromatography, and the results were as follows: light scattering weight average molecular weight M w.MALLS =48600, molecular weight distribution PDI=1.55, Mark-Houwink index α =0.488, average branching factor g '=0.42, confirming that the obtained polymer has a branched structure.

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Abstract

The invention discloses a method for preparing branched polyacrylonitrile and belongs to the field of macromolecular syntheses and functional polymer preparation. Methacrylic acid sulfhydryl propionyloxy ethyl ester is used as a branching monomer, azodiisobutyronitrile (AIBN) is used as an initiator and N, N'-dimethylformamide (DMF) or sodium thiocyanate aqueous liquid is used as a solvent to implement free radical polymerization with such monomers as acrylonitrile to successfully obtain the branched polyacrylonitrile. The degree of branching of the polymer is adjusted through adjusting molar ratio between the branched monomer and the polymer monomer. The methacrylic acid sulfhydryl propionyloxy ethyl ester with low cost and good storage stability and comprising polymerizable double bonds and chain transfer sulfhydryl is used as the branching monomer to successfully prepare the branched polyacrylonitrile under a conventional free radical polymerization condition. The polymerization is simple and easy; moreover, the monomer conversion rate is high and the degree of branching of the polymer is controllable.

Description

technical field [0001] The invention relates to the preparation of branched polyacrylonitrile by using a compound containing a polymerizable double bond and a chain transfer mercapto group as a branched monomer under conventional free radical polymerization conditions, and belongs to the fields of polymer synthesis and functional polymer preparation. Background technique [0002] Due to its unique three-dimensional spherical structure, branched polymers have lower melt viscosity and solution viscosity than linear polymers, and can be used to prepare solvent-free coatings and high solid content polymer solutions and improve high Molecular material molding and processing properties, etc. Using branched polymers to modify linear polymers, increase the solid content of polymer solutions, reduce melt viscosity, improve the molding and processing efficiency of polymers, and achieve environmental protection and energy-saving production technology of polymer materials is the industr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/44C08F218/08C08F220/14C08F220/38D01F6/38
Inventor 蒋必彪黄文艳薛小强
Owner 溧阳常大技术转移中心有限公司
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