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Process for synthesizing pipetting block copolymer gel

A block copolymer and liquid-absorbing technology, which is applied in the field of synthesizing liquid-absorbing block copolymer gels, can solve the problems of atom transfer radical synthesis that have not been reported in the literature, and achieve uniform molecular weight distribution of chain segments, Convenient design and controllable crosslink density

Inactive Publication Date: 2008-10-15
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, in the field of design of liquid-absorbing multifunctional block polymer gels, the application of atom transfer radical synthesis has not been reported in the literature so far.

Method used

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  • Process for synthesizing pipetting block copolymer gel
  • Process for synthesizing pipetting block copolymer gel
  • Process for synthesizing pipetting block copolymer gel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Synthesis of polystyrene (PS) bifunctional macromolecular initiator

[0035] According to the ratio n(styrene):n(α,α'-dichloro-p-xylene (DCX)):n(CuBr):n(2,2'-bipyridine (bpy))=200~1000:1: 1:3, sequentially add CuBr, bpy, DCX and styrene to a 10mL ampoule, vacuum-fill with N 2 - Vacuum, repeat 5 times, seal the tube under vacuum, and place it in an oil bath at a constant temperature of 130° C. for a predetermined time (45 h) to react.

[0036] After the reaction, take out the sealed tube, cool it with cold water immediately, open the sealed tube, dissolve the polymer PS with THF, methanol is used as a precipitant, collect the polymer, dry it in a vacuum oven at 50°C to constant weight, and calculate the conversion rate. The relational curve of its theoretical molecular weight and measured molecular weight is as follows figure 1 As shown, it exhibits very good characteristics of living / controlled polymerization.

[0037] (2) Synthesis of PBA-b-PS-b-PBA triblock cop...

Embodiment 2

[0044] (1) Synthesis of polybutyl acrylate difunctional macroinitiator

[0045] According to the ratio n(butyl acrylate):n(α,α'-dichloro-p-xylene (DCX)):n(CuBr):n(2,2'-bipyridine (bpy))=200~1000:1 : 1: 3, sequentially add CuBr, bpy, DCX and butyl acrylate in a 10ml ampoule, vacuum-fill with N 2 - Vacuum, repeat 5 times, seal the tube under vacuum, and place it in an oil bath at a constant temperature of 130° C. to react for a predetermined time (137 h).

[0046] After the reaction, take out the sealed tube, cool it with cold water immediately, open the sealed tube, dissolve the polymer PS with THF, methanol is used as a precipitant, collect the polymer, dry it in a vacuum oven at 50°C to constant weight, and calculate the conversion rate.

[0047] (2) Synthesis of PS-b-PBA-b-PS triblock copolymer

[0048] Add PBA bifunctional macromolecular initiator (M n，GPC =10210g / mol, PDI=1.38; 0.57g, 0.057mmol), 2.0ml of toluene was shaken and mixed until the PBA was completely dissolv...

Embodiment 3

[0065] Example 3: Post-crosslinked amphiphilic three-arm diblock copolymer gel

[0066] (1) Synthesis of trifunctional polymethyl methacrylate (PMMA) macroinitiator

[0067] According to the ratio n(MMA):n(BTBiB):n(CuCl):n(bpy)=100~500:1:1:3, add CuCl, bpy, DMF, BBTiB and MMA in 5mL ampoule in turn, Vacuum-N filled 2 -Vacuum, repeat 5 times, seal the tube under vacuum, and place it in an oil bath at a constant temperature (90° C.) for a predetermined time (18 h) to react.

[0068] After the reaction is over, take out the sealed tube, cool it with cold water immediately, open the sealed tube, dissolve the polymer (PMMA) with THF, use methanol as a precipitant, collect the polymer, and dry it in a vacuum oven at 50°C to constant weight to obtain the product PMMA .

[0069] (2) Synthesis of star amphiphilic PMMA-b-PDMAEMA three-arm macroinitiator

[0070] According to the proportioning n(DMAEMA):n(PMMA):n(CuCl):n(bpy)=300~800:1:1:3, add CuCl, bpy, DMF, PMMA and DMAEMA in the ...

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Abstract

The invention discloses a method for synthesizing an imbibing block polymer gel. The method comprises the following steps that: (1) the ATRP reaction is performed on a monomer A to synthesize a polyfunctional group macromolecule evocating agent; (2) the polymer polyfunctional group macromolecule is taken as the evocating agent, the ATRP reaction is performed on a monomer B to synthesize the block polymer evocating agent; (3) a cross-linking agent is added to perform the ATRP reaction in order to synthesize the block polymer gel; wherein, the monomer A and the monomer B are selected from different one of the cinnamene and (methyl) acrylic ester. The network size of the polymer obtained by the method can be conveniently controlled by the molecular weight of a linear polymer or the dosage of the cross-linking agent; in addition, the structure of the polymer can be conveniently controlled by the selection and the combination of the monomer kinds, thereby controlling the imbibing performance of the polymer gel.

Description

technical field [0001] The invention relates to a method for designing a multifunctional block polymer, in particular to a method for synthesizing a liquid-absorbing block copolymer gel. Background technique [0002] Gels are composed of liquid and polymer networks. Due to the affinity between the liquid and the polymer network, the liquid is enclosed by the polymer network and loses its fluidity, so the gel can display a certain shape like a solid. During the swelling process of the gel, on the one hand, the solvent tries to penetrate into the polymer to expand its volume; on the other hand, due to the volume expansion of the cross-linked polymer, the molecular chains of the network expand to three-dimensional space, causing the molecular network to undergo elastic contraction under stress. And can shrink the molecular network. Swelling equilibrium is reached when these two opposing tendencies counteract each other. The swelling behavior of polymer gel is closely related...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F4/00C08F212/08C08F220/10
Inventor 朱秀林程振平张丽芬朱健周年琛张正彪张伟
Owner SUZHOU UNIV
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