Sulfhydryl chain transfer hyperbranched polymerization process

A polymerization method and chain transfer technology, applied in the field of novel thiol chain transfer hyperbranched polymerization method, can solve the problems of complex and difficult structure of AB branched monomers, restricting the development of hyperbranched polymers, low monomer universality, etc. The branched monomers are simple and easy to obtain, have strong applicability, and control the degree of branching.

Inactive Publication Date: 2009-09-30
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the various existing SCVP methods have more or less disadvantages, such as the complex structure of AB branched monomers, difficult preparation, harsh polymerization conditions, and low universality of monomers, which limit the further development of hyperbranched polymers.

Method used

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  • Sulfhydryl chain transfer hyperbranched polymerization process
  • Sulfhydryl chain transfer hyperbranched polymerization process
  • Sulfhydryl chain transfer hyperbranched polymerization process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0023] 0.0253 g (0.1 mmol) (4-vinyl)-benzyl sodium thiosulfate, 0.0328 g (0.2 mmol) AIBN, and 2.0830 g (20 mmol) styrene were successively added to a 25 mL round bottom flask. Add 2 mL of DMSO as the reaction solvent. Close the polymerization system, and remove oxygen and other polymerization inhibitors in the system by freezing and pumping air with liquid nitrogen. Put it into a constant temperature oil bath at 70°C, react for 9 hours, and precipitate twice with a mixture of methanol and water (volume ratio 3:1), collect the solid and dry it in a vacuum oven at 40°C. The weight-average molecular weight of the product measured by GPC-MALLS is 5.10×10 4 , the molecular weight distribution is 1.569. The intrinsic viscosity is 26.5wmL / g. The alpha value was 0.540 ± 0.006. The glass transition temperature of the product was determined by differential scanning calorimetry to be 99.34°C.

Embodiment 3

[0025] 0.0506g (0.2mmol) (4-vinyl)-benzyl sodium thiosulfate, 0.0328g (0.2mmol) AIBN, and 2.0830g (20mmol) styrene were successively added to a 25mL round bottom flask. Then 2 mL of DMF was added as the reaction solvent. Close the polymerization system, and remove oxygen and other polymerization inhibitors in the system by freezing and pumping air with liquid nitrogen. Put it into a constant temperature oil bath at 70°C, react for 9 hours, and precipitate twice with a mixture of methanol and water (volume ratio 3:1), collect the solid and dry it in a vacuum oven at 40°C. The weight-average molecular weight of the product measured by GPC-MALLS is 6.57×10 4 , the molecular weight distribution is 1.781. The intrinsic viscosity is 27.5wmL / g. The alpha value was 0.580 ± 0.005. The glass transition temperature of the product was measured with a differential scanning calorimeter to be 99.17°C.

Embodiment 4

[0027] 0.0759g (0.3mmol) (4-vinyl)-benzyl sodium thiosulfate, 0.0328g (0.2mmol) AIBN, and 2.0830g (20mmol) styrene were successively added to a 25mL round bottom flask. Then 2 mL of DMF was added as the reaction solvent. Close the polymerization system, and remove oxygen and other polymerization inhibitors in the system by freezing and pumping air with liquid nitrogen. Put it into a constant temperature oil bath at 70°C, react for 9 hours, and precipitate twice with a mixture of methanol and water (volume ratio 3:1), collect the solid and dry it in a vacuum oven at 40°C. The weight-average molecular weight of the product measured by GPC-MALLS is 6.89×10 4 , the molecular weight distribution is 2.024. The intrinsic viscosity was 25.9wmL / g. The alpha value was 0.574 ± 0.006. The glass transition temperature of the product measured by differential scanning calorimetry was 94.88°C. hyperbranched polymer 13 C-NMR spectrum see figure 1.

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Abstract

The invention relates to a sulfhydryl chain transfer hyperbranched polymerization process belonging to the technical field of polymer synthesis and functional polymer preparation. In the invention, styrene monomer containing alkyl sodium (potassium) thiosulfate taken as a branched monomer, other ethenyl monomers taken as main polymeric monomers, dimethyl sulfoxide (DMSO) or N-N'-dimethyl formamide (DMF) taken as polymeric solvent and radical initiator as polymeric initiator undergo polymeric reaction under the thermal initiation condition; active sulfhydryl released by the alkyl sodium (potassium) thiosulfate under the action of DMSO, the DMF or any other strong polar reagent is used for chain transfer branched reaction so as to achieve the purpose of preparing hyperbranched polymer; and the branched structure of the hyperbranched polymer is adjusted through adjusting the molar ratio, the polymeric reaction time and the polymeric reaction temperature of the branched monomer, the main polymeric monomers, the radical initiator. The sulfhydryl chain transfer hyperbranched polymerization process has the advantages of simple and available branched monomer, mild polymeric condition, controllable branching coefficient, strong applicability to various monomers, and the like.

Description

technical field [0001] The invention relates to a novel thiol chain transfer hyperbranched polymerization method, which belongs to the technical field of polymer synthesis research and functional polymer preparation. Background technique [0002] Dendritic and hyperbranched polymers are a class of highly branched polymers with a dendritic structure. Compared with traditional linear polymers, these polymers have a unique three-dimensional branched molecular structure and a large number of intramolecular cavities. There is no entanglement between them, and it contains a large number of reactive active end groups, so it exhibits special properties that many linear polymers do not have, such as high solubility, low viscosity, and high chemical reactivity. Moreover, compared with dendritic polymers, the synthesis method of hyperbranched polymers is relatively simple, the product cost is low, and it is more conducive to large-scale production, making hyperbranched macromolecules w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/38
Inventor 江金强宗奕吾代鹏刘晓亚林凤英张胜文陈明清倪忠斌
Owner JIANGNAN UNIV
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