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Controllable Synthesis of Polyvinyl Acetate Block Copolymer

A technology of polyvinyl acetate and block copolymer, which is applied in the field of preparation of block copolymer, can solve the problems of restricting large-scale preparation and application, complicated operation steps and high cost, and achieves efficient preparation, low cost and versatility strong effect

Active Publication Date: 2019-11-26
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned preparation method has cumbersome operation steps and high cost (organic ligands and RAFT reagents in ATRP are expensive), which limits its large-scale preparation and application

Method used

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  • Controllable Synthesis of Polyvinyl Acetate Block Copolymer
  • Controllable Synthesis of Polyvinyl Acetate Block Copolymer
  • Controllable Synthesis of Polyvinyl Acetate Block Copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0039] (1) Preparation of MANDC

[0040] In a three-neck round bottom flask, add 9.03 g, 0.030 mol of tetraethylthiuram disulfide (TETD), 7.5 g, 0.045 mol of azobisisobutyronitrile (AIBN), and 100 mL of toluene, and blow with nitrogen gas Oxygen was removed by bubbles for 30 min, and then reacted at 55 °C for 65 h in a nitrogen atmosphere. The white precipitate was removed by filtration, and the toluene was removed by rotary evaporation to obtain the crude product of MANDC. The crude product of MANDC was distilled under reduced pressure at 107~115°C and 1 mmHg to obtain a light yellow refined product of MANDC, which was analyzed by nuclear magnetic spectrum ( 1 H NMR) and infrared spectroscopy (IR) characterization.

[0041] (2) Preparation of block copolymer PMMA-b-PVAc

[0042] 5.0 mL, 47.2 mmol of monomeric MMA, 0.118 mmol of MANDC and 0.059 mmol of Cu(OAc) 2 Add it into a 20 mL colorless and transparent reactor, seal the tube directly without deoxygenation, move the tr...

Embodiment approach 2

[0047] (1) Preparation of 1-cyano-1-methylethyl N, N-diethyldithiocarbamate: It is exactly the same as Embodiment 1, and will not be repeated here.

[0048] (2) Synthesis of block copolymer PEGMA-b-PVAc:

[0049] Add 5.0 mL, 11 mmol of monomeric mPEGMA 500 , 0.118 mmol of MANDC and 0.059 mmol of Cu(OAc) 2 Add it into a 20 mL colorless and transparent reaction bottle, seal the tube directly without removing oxygen, move the transparent reactor to a high-pressure mercury lamp, the power of the light source is 10 kW, and the polymerization temperature is 30 °C. After the polymerization is carried out under magnetic stirring for 10 h , directly added 4.0 mL, 43.2 mmol of monomer VAc into the reactor, sealed the reaction bottle, and continued to polymerize for 12 h under a high-pressure mercury lamp to obtain the block copolymer PEGMA-b-PVAc. After the polymerization, the reaction flask was unsealed, and an appropriate amount of tetrahydrofuran was added thereto to allow the PEGM...

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Abstract

The invention relates to the technical field of preparation of block copolymers and discloses a controllable synthesis method for a polyvinyl acetate block copolymer. The method comprises the following steps: S1, adding a first monomer, an iniferter reagent and a copper catalyst into a sealed reaction container under an ultraviolet lamp, and performing lighting polymerization while magnetic stirring; and S2, removing seal of the reaction container after polymerization is ended, adding a second monomer into the container, resealing the reaction container, and performing lighting polymerizationagain, thereby obtaining the block copolymer. According to the method disclosed by the invention, a copper salt being low in price, non-toxic and easily washable and removable serves as the catalyst,and the iniferter reagent is introduced as an initiator, the PVAc-containing block copolymer with a controllable molecular weight and narrow molecular weight distribution is prepared by virtue of sequential dosing under high-efficiency ultraviolet induction. The method is low in cost, high in universality, easy and convenient to operate and easy to enlarge, and the bottleneck that the PVAc-containing block copolymer is high in preparation cost and low in yield is broken.

Description

technical field [0001] The invention relates to a preparation method of a block copolymer containing vinyl acetate structural units, in particular to a controllable synthesis method of a polyvinyl acetate block copolymer. Background technique [0002] Structure-controllable block polymers comprising polyvinyl acetate (PVAc) and its hydrolysis product polyvinyl alcohol (PVOH) are widely used in coatings, pharmaceuticals, agriculture, and biological applications. Controlled radical polymerization (CRP) has the advantages of a wide range of free radical polymerization monomers, mild polymerization conditions and controllable polymer structure, and is an important method for preparing block copolymers. At the same time, due to the unique properties of its monomer vinyl acetate (VAc), its polymer is obtained by free radical polymerization, making CRP the only method for preparing block copolymers containing polyvinyl acetate. However, due to the low activity of VAc monomer, the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F220/14C08F218/08C08F2/48
CPCC08F2/48C08F218/08C08F220/14C08F293/00
Inventor 姜孝武韩杰曹路南蔡鹏倪伶俐陈静
Owner HUAIYIN INSTITUTE OF TECHNOLOGY