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Method for preparing branched polystyrene by emulsion polymerization

A technology of branched polystyrene and emulsion polymerization, which is applied in the field of emulsion polymerization synthesis of branched polystyrene, and can solve the problems of restricting the development of large-scale application of branched polystyrene, consuming large organic solvents, and long polymerization time, etc. problems, to achieve the effects of small environmental impact, short response time, and simple operation

Active Publication Date: 2013-02-13
宁夏永润新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two types of polymerization methods also have two common shortcomings in the process of preparing branched polystyrene. The polymerization time required for high monomer conversion is long, and a large amount of organic solvents will be consumed in the reaction process, which will cause environmental pollution. certain hazard
These deficiencies limit the development of large-scale application of branched polystyrene to a certain extent.

Method used

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  • Method for preparing branched polystyrene by emulsion polymerization
  • Method for preparing branched polystyrene by emulsion polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A mixed solution of styrene (41.6071g, 0.4mol) and 3-mercaptohexyl methacrylate (0.4083g, 2mmol) was added to a solution of sodium dodecylbenzenesulfonate (2.9128g, 7 wt % styrene) , sodium bicarbonate (1.2421g, 3 wt % styrene), potassium persulfate (2.1614g, 8mmol) and water (82.9802g) in a reaction flask, after vacuuming and exhausting oxygen, stir the reaction at 80°C for 2 hours, The conversion of styrene was measured to be 95.3%. Demulsify with sodium chloride, wash with water three times, and dry to obtain a polymer. 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 = 335400, molecular weight distribution PDI = 3.30, Mark-Houwink index α = 0.659, branching factor g '=0.76, confirming that the obtained polymer has a branched structure. figure 1 The branching factor of embodiment 1 gained branched polystyrene g 'Relationship with the change of mo...

Embodiment 2

[0025] A mixed solution of styrene (41.6101g, 0.4mol) and 3-mercaptohexyl methacrylate (0.4045g, 2mmol) was added to a solution of sodium dodecylbenzenesulfonate (2.8913g, 7 wt % styrene) , sodium bicarbonate (1.2490g, 3 wt % styrene), potassium persulfate (0.2172g, 0.8mmol) and water (83.3322g) in a reaction flask, after vacuuming and exhausting oxygen, stir and react at 70°C for 5 hours , The conversion rate of styrene was measured to be 96.6%. Demulsify with sodium chloride, wash with water three times, and dry to obtain a polymer. 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 = 1635000, molecular weight distribution PDI = 5.83, Mark-Houwink index α = 0.671, branching factor g ' = 0.81, confirming that the obtained polymer has a branched structure.

[0026]

Embodiment 3

[0028] A mixed solution of styrene (41.6311g, 0.4mol) and 3-mercaptohexyl methacrylate (1.6132g, 8mmol) was added to a solution of sodium dodecylbenzenesulfonate (2.9151g, 7 wt % styrene) , sodium bicarbonate (1.2490g, 3 wt % styrene), potassium persulfate (3.2434g, 12mmol) and water (83.1032g) in a reaction flask, after vacuuming and exhausting oxygen, stir and react at 70°C for 5 hours, The conversion of styrene was measured to be 96.7%. Demulsify with sodium chloride, wash with water three times, and dry to obtain a polymer. 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 = 907500, molecular weight distribution PDI = 5.43, Mark-Houwink index α = 0.656, branching factor g '=0.67, confirming that the obtained polymer has a branched structure.

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Abstract

The invention discloses a method for preparing branched polystyrene by emulsion polymerization, and belongs to the field of functional polymer preparation. A functional monomer containing polymerized double bond and chain transfer mercapto serving as a branched monomer, water serving as a medium, an anionic surfactant serving as an emulsifying agent, persulfate serving as an initiator, sodium hydrogen carbonate serving as a pH regulator and a polystyrene monomer are polymerized for 2 to 8 hours at the temperature of between 70 and 80 DEG C, the conversion rate of the monomer reaches over 95 percent, and the branched polystyrene is successfully obtained. The functional monomer containing the polymerized double bond and the chain transfer mercapto is used as the branched monomer, and the branched polystyrene is prepared by using emulsion polymerization, so the polymerization system is stable; the method is easy to operate, feasible, low in influence on environment, short in reaction time and high in conversion rate; the obtained branched polystyrene is high in molecular weight and narrow in molecular weight distribution; and the branching degree, the molecular weight and the molecular weight distribution of the branched polystyrene can be adjusted in a wide range.

Description

technical field [0001] The invention relates to an emulsion polymerization synthesis technology for preparing branched polystyrene, in particular to a preparation method with fast polymerization rate in the reaction system, high monomer conversion rate, branched structure, high molecular weight and narrow molecular weight distribution. , belongs to the field 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. [0003] The current synthesis technology of branched polystyrene mainly adopts the solution polymerization of living / controllable free radicals in the presence of self-initiating monomers (inimer) or dienes, and the conventiona...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F220/38C08F2/26
Inventor 黄文艳杨宏军蒋其民薛小强蒋必彪
Owner 宁夏永润新材料科技有限公司