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Preparation method of segmented copolymer from vinylidene chloride copolymer and polyethylene glycol

A technology of block copolymer and vinylidene chloride, applied in the field of preparation of block copolymer, can solve the problems of no block copolymer, increasing the molecular composition and difficulty of structure control of vinylidene chloride polymer, etc.

Inactive Publication Date: 2012-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vinylidene chloride has a high phase monomer chain transfer constant (such as C tr，VDC，50℃ =2.2×10 -3 , C tr，VDC，60℃ =3.8×10 -3 , C tr，VDC，70℃ =6.3×10 -3 ), therefore, the molecular weight and structure of the polymer are mainly determined by the chain transfer reaction, and the common living radical polymerization method aimed at controlling the chain termination is not suitable for the polymerization of vinylidene chloride, which increases the control of the molecular composition and structure of the vinylidene chloride polymer difficulty
However, there is no report on the preparation of block copolymers composed of vinylidene chloride polymers and PEG by RAFT polymerization.

Method used

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  • Preparation method of segmented copolymer from vinylidene chloride copolymer and polyethylene glycol
  • Preparation method of segmented copolymer from vinylidene chloride copolymer and polyethylene glycol
  • Preparation method of segmented copolymer from vinylidene chloride copolymer and polyethylene glycol

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preparation example Construction

[0017] The steps of the preparation method of the block copolymer that are made up of vinylidene chloride polymer and polyethylene glycol are as follows:

[0018] (1) Dissolve 1.0mol polyethylene glycol and 2.0-2.5mol reversible addition-fragmentation chain transfer polymerization chain transfer reagent in 130-170mol methylene chloride, mix well, add 2-2.5mol water remover dicyclohexyl carbon Diimine and 0.4-0.5mol catalyst 4-dimethylaminopyridine, esterification reaction at 25°C for 24-72 hours, after repeated precipitation, dissolution, and drying to obtain a macromolecular reversible addition-fragmentation chain transfer polymerization chain transfer reagent ;

[0019] (2) Add 50-100 parts by mass of 1,4-dioxane, 5-20 parts by mass of vinylidene chloride, and 2-7 parts by mass of macromolecular reversible addition-fragmentation chain transfer polymer chain Transfer reagent, 0.016-0.16 parts by mass of azobisisobutyronitrile initiator, or add 50-100 parts by mass of 1,4-dio...

Embodiment 1

[0026](1) 0.007 mol of polyethylene glycol with a molecular weight of 2000 and 0.0156 mol of reversible addition-fragmentation chain transfer polymerization chain transfer reagent S-1-dodecyl-S'-(α, α'-dimethyl- α”-acetic acid) trithiocarbonate dissolved in 1.1mol methylene chloride, mixed evenly, adding 0.0155mol water remover dicyclohexylcarbodiimide and 0.003mol catalyst 4-dimethylaminopyridine, at 25°C After 24 hours of esterification reaction, after repeated precipitation, dissolution, and drying, a macromolecular reversible addition-fragmentation chain transfer polymer chain transfer reagent was obtained;

[0027] (2) Add 100 grams of 1,4-dioxane, 10.8 grams of vinylidene chloride and 1.2 grams of methyl acrylate, 2 grams of macromolecular reversible addition-fragmentation chain transfer polymerization chain transfer reagent, 0.015 grams of azobisisobutyronitrile initiator, stirred at room temperature for 10 minutes to dissolve and mix the reactants, nitrogen and deoxyge...

Embodiment 2

[0029] (1) 0.007 mol of polyethylene glycol with a molecular weight of 10000 and 0.0156 mol of reversible addition-fragmentation chain transfer polymerization chain transfer reagent S-1-dodecyl-S'-(α, α'-dimethyl- α”-acetic acid) trithiocarbonate was dissolved in 0.91mol of dichloromethane, mixed evenly, adding 0.0155mol of dehydrating agent dicyclohexylcarbodiimide and 0.003mol of catalyst 4-dimethylaminopyridine, at 25°C Esterification reaction for 48 hours, after repeated precipitation, dissolution, and drying to obtain a macromolecular reversible addition-fragmentation chain transfer polymer chain transfer reagent;

[0030] (2) Add 80 grams of 1,4-dioxane, 10.8 grams of vinylidene chloride and 1.2 grams of methyl acrylate, 6.4 grams of macromolecular reversible addition-fragmentation chain transfer polymerization chain transfer reagent, 0.015 grams of azobisisobutyronitrile initiator, stirred at room temperature for 30 minutes to dissolve and mix the reactant, nitrogen deo...

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Abstract

The invention discloses a preparation method of a segmented copolymer from a vinylidene chloride copolymer and polyethylene glycol which comprises the steps of: reacting polyethylene glycol (PEG) and a reversible addition fragmentation transfer radical polymerization (RAFT) chain transfer reagent in dichloromethane under the action of a catalyst 4-dimethylamino pyridine to obtain a PEG macromolecular RAFT reagent; and performing RAFT polymerization on vinylidene chloride or vinylidene chloride and a comonomer in the PEG macromolecular RAFT reagent under the action of azo-bis-iso-butyrynitrile initiator and with 1,4-dioxane as a solvent to obtain a segmented copolymer from a vinylidene chloride copolymer and polyglycol with large molecular weight and narrow molecular weight distribution width. The invention provides a novel method for preparing a vinylidene chloride segmented copolymer, and the segmented copolymer composed of a vinylidene chloride copolymer and polyglycol prepared by the invention has a potential application preparation of hydrophilic modified vinylidene chloride films and vinylidene chloride polymer based mesoporous carbon.

Description

technical field [0001] The invention relates to a block copolymer, in particular to a preparation method of a block copolymer composed of vinylidene chloride polymer and polyethylene glycol. Background technique [0002] Free radical polymerization is the main method for industrial production of polymers, and currently nearly 60% of polymers produced are produced by free radical polymerization. Free radical polymerization has the advantages of wide range of applicable monomers, mild reaction conditions, and high molecular weight of polymerization products. However, ordinary free radical polymerization has the characteristics of slow initiation, rapid growth, and rapid termination. Due to the gel effect and inter-molecular / internal chain transfer during the polymerization process, the molecular weight distribution of the polymerization product is relatively wide. Precise control of polymer molecular composition and structure is an important area of ​​current polymer research...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F214/08C08F220/06C08F220/14C08F220/18C08F220/28C08F2/38
Inventor 杨杰包永忠
Owner ZHEJIANG UNIV
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