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Fluorine-containing superbranching-grafting block polymer and its preparation

A block polymer and hyperbranched polymer technology, applied in the field of copolymers, can solve the problems of harsh living anionic polymerization reaction conditions, impure products, difficult to remove, etc., to improve dual response performance, improve hydrophilic performance, reduce surface energy effect

Inactive Publication Date: 2008-10-01
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the living anionic polymerization reaction conditions are harsh, the reaction temperature is very low, and it is difficult to realize industrial control and production; the atom transfer radical polymerization (ATRP) method needs to modify the terminal group of the polymer, and the repeatability is not good enough. The final product Contains a catalyst in it, it is difficult to remove, and the product is not pure; for the reversible addition-fragmentation chain transfer polymerization (RAFT) method, it is necessary to modify the terminal group of the polymer into a dithioester structure for the reaction, and the final dithio The ester structure has a certain influence on the properties of the polymer

Method used

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  • Fluorine-containing superbranching-grafting block polymer and its preparation
  • Fluorine-containing superbranching-grafting block polymer and its preparation
  • Fluorine-containing superbranching-grafting block polymer and its preparation

Examples

Experimental program
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Effect test

Embodiment 1

[0058] Embodiment one: HPE-g-DMAEMA 15 -b-OFPMA 5 and its preparation

[0059] (1) Preparation of KH: Put the stirring rotor into a dry reaction bottle in advance, and plug it tightly with a reversible rubber stopper. Then use a needle, a latex tube, and connect it to a vacuum pump, and fill it with high-purity argon gas while evacuating it, and repeat the operation three times. After moving a certain amount of KH into the reaction bottle, inject 5 mL of dry THF with a dry syringe, stir and wash, and suck out the THF containing mineral oil with a syringe after resting, repeat this three times, and finally dry the residual THF solution with high-purity argon. Accurately weigh the amount of KH (0.05-0.15 g, about 1.25-3.75 mmol) in the reaction vial by subtraction method.

[0060] (2) Preparation of initiator: inject 20 mL of THF into the polymerization bottle. Place the reaction vial in an ice-water bath with magnetic stirring. Prepare the polymerization bottle that agitat...

Embodiment 2

[0062] Embodiment two: HPE-g-DMAEMA 15 -b-OFPMA 10 and its preparation

[0063] (1) Preparation of KH: same as Example 1.

[0064] (2) Preparation of initiator: same as Example 1.

[0065](3) Polymerization: According to the length of the required graft chain (first monomer polymer chain) and block chain (second monomer polymer chain), control the oxygen anion in the first monomer and macroinitiator The molar ratio (measured in the molar concentration corresponding to the initiator) is 15: 1, and the first monomer methacrylate-2-(dimethylamino)ethyl (dimethylamino) ethyl ester ( DMAEMA), reacted for 0.5~1.5h; then control the molar ratio of the second monomer and the initiator oxyanion to be 10:1, inject the second monomer methacrylic acid- (2,2,3,3,4,4,5,5-octafluoro)pentyl ester (OFPMA), react for 0.5-1.5h, and finally terminate the reaction with dry methanol. The reacted polymer is subjected to rotary evaporation at 60-70°C to remove the solvent, followed by precipitat...

Embodiment 3

[0066] Embodiment three: HPE-g-DMAEMA 30 -b-OFPMA 10 and its preparation

[0067] (1) Preparation of KH: same as Example 1.

[0068] (2) Preparation of initiator: same as Example 1.

[0069] (3) Polymerization: According to the length of the required graft chain (first monomer polymer chain) and block chain (second monomer polymer chain), control the oxygen anion in the first monomer and macroinitiator The molar ratio (measured with the molar concentration corresponding to the initiator) is 30: 1, and the first monomer methacrylate-2-(dimethylamino) ethyl ester (dimethylamino) ethyl ester ( DMAEMA), reacted for 0.5~1.5h; then control the molar ratio of the second monomer and the initiator oxyanion to be 10:1, inject the second monomer methacrylic acid- (2,2,3,3,4,4,5,5-octafluoro)pentyl ester (OFPMA), react for 0.5-1.5h, and finally terminate the reaction with dry methanol. The reacted polymer is subjected to rotary evaporation at 60-70°C to remove the solvent, followed b...

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Abstract

The present invention relates to one kind of fluoric super branched-grafted block polymer, and features that the polymer has core-arm structure comprising core of super branched poly(3-ethyl-3-methyol trimethylene oxide) and arm of alkyl substituted amino methacrylate and fluoric methacrylate block polymerized structure. The fluoric super branched-grafted block polymer is prepared through an oxygen ion initiated polymerization process. The fluoric amphiphilic super branched copolymer of the present invention has double temperature and pH responding performance and lowered surface energy, and the preparation process has fast reaction speed, high conversion rate and high product purity.

Description

technical field [0001] The present invention relates to a copolymer grafted with one or more unsaturated aliphatic group compounds and hyperbranched polyether, each unsaturated aliphatic group has only one carbon-carbon double bond, and only one is based on carboxylic acid ester-terminated; it specifically relates to a "hyperbranched-grafted block" copolymer composed of hyperbranched polyether, (alkyl-substituted amino) methacrylate and fluoromethacrylate, with pH / temperature Responsiveness. Background technique [0002] Hyperbranched polymers, although the structure is not highly perfect compared with dendrimer polymers, the degree of branching DB<100%, and have a certain degree of molecular weight distribution, but they have similar properties to dendrimers, the synthesis method It is relatively simple and widely used, so it has become one of the research hotspots in the field of polymer science. [0003] Due to its special properties, stimuli-responsive polymers can ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06
Inventor 倪沛红毛江麦亦勇颜德岳
Owner SUZHOU UNIV
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