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Initiation system for photo-polymerization of active free radicals of methacrylate monomers

A technology of methacrylic acid and initiating system, applied in the field of initiating system, can solve problems such as few advantages and complex structure, and achieve the effect of simple and easy preparation method and strong practicability

Active Publication Date: 2017-05-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these organic photoredox catalysts have complex structures, and the cost has little advantage compared with noble metal catalysts.

Method used

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  • Initiation system for photo-polymerization of active free radicals of methacrylate monomers
  • Initiation system for photo-polymerization of active free radicals of methacrylate monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment one, the photopolymerization of MMA monomer under p-methoxybenzaldehyde / 1-iodoperfluorohexane initiation system

[0022] The mass fraction of monomer MMA in N,N-dimethylformamide (DMF) solvent (6.0g) was 24wt%. According to the molar ratio [MMA] / [1-iodoperfluorohexane] / [p-methoxybenzaldehyde] / [DMA]=100 / 2 / 5 / 5, respectively add the above-mentioned raw materials into 25mL single branch round bottom in the flask. seal. Refrigerated and evacuated three times, and finally introduced argon, so that the polymerization reaction was carried out under the irradiation conditions of two 23W compact energy-saving lamps in an inert atmosphere. Distance response devices such as figure 1 shown. At different time intervals, a small amount of samples were taken from the reaction system with a syringe, and the samples were precipitated three times with a mixture of methanol and water with a volume ratio of 7:3, and dried in vacuum to constant weight to obtain a white powder....

Embodiment 2

[0027] Example two, the photopolymerization of PEGMA monomer under p-methoxybenzaldehyde / 1-iodoperfluorohexane initiation system

[0028] Referring to Example 1, the photopolymerization of PEGMA monomer under the p-methoxybenzaldehyde / 1-iodoperfluorohexane initiation system was carried out. The molar ratio [PEGMA] / [1-iodoperfluorohexane] / [p-methoxybenzaldehyde] / [DMA] was 42 / 2 / 5 / 5. Samples taken at different time periods were precipitated with ether three times, dried in vacuum to constant weight, and a viscous substance was obtained. At 20.5h, the monomer conversion rate was 88%, and the polymer product M was recorded by GPC. n= 14200, PDI = 1.39. In addition, during the polymerization process, the molecular weight of the polymer increases linearly with the increase of the conversion rate, and the molecular weight distribution of the polymer is narrow (less than 1.49), which conforms to the law of living polymerization.

Embodiment 3

[0029] Embodiment three, the photopolymerization of MMA monomer under p-methoxybenzaldehyde / other initiator initiation system

[0030] Referring to Example 1, carry out the photopolymerization of the MMA monomer under p-methoxybenzaldehyde / other initiator initiation system. The difference is that the selected initiators are ethyl 2-bromoisobutyrate, ethyl α-bromophenylacetate, 1-iodoperfluorobutane and 1-iodoperfluorooctane, etc.

[0031] Specifically, the monomer concentration is 33 wt%, and the molar ratio [MMA] / [ethyl 2-bromoisobutyrate] / [p-methoxybenzaldehyde] / [DMA]=100 / 1 / 10 / 50 The substance was added into the DMF solvent, reacted for 36h, and the monomer conversion rate was 85%, and the polymer product M was recorded by GPC. n = 26100, PDI = 1.72. Under the same conditions, when the molar ratio [MMA] / [α-ethyl bromophenylacetate] / [p-methoxybenzaldehyde] / [DMA]=100 / 1 / 10 / 50, the reaction was 35h, and the monomer The conversion rate was 90%, and the polymer product M was re...

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Abstract

The invention discloses an initiation system for photo-polymerization of active free radicals of methacrylate monomers. The initiation system comprises organic halide initiators, aromatic tertiary amine reducing agents and benzaldehyde photocatalysts with substituents. Visible light (such as a household 23W energy-saving lamp) can be used as a light source for the initiation system, and polymerization of the active free radicals of the methacrylate monomers can be initiated at the room temperature. The free radicals of methyl methacrylate (MMA), polyethylene glycol methacrylate (PEGMA) and methacrylic acid benzyl ester (BnMA) monomers and the like can be polymerized under preferred matching conditions. Polymers prepared by the aid of the initiation system are macromolecular initiators, chain extension reaction is successfully carried out, and accordingly block polymers can be obtained. The initiation system has the advantages that catalysts are low in toxicity, and polymerization reaction conditions are mild; the cost of polymerization reaction is lowered to a great extent owing to the usage of organic catalysts as compared with polymerization reaction catalyzed by transition metal complexes, and after-treatment working procedures can be reduced to a great extent.

Description

technical field [0001] The invention relates to an initiation system for visible light active radical polymerization, in particular to an initiation system composed of a substituent-containing benzaldehyde organic catalyst, an organic halide initiator and an aromatic tertiary amine reducing agent at room temperature . Visible light active radical polymerization of methacrylate monomers can be realized by using the initiation system. Background technique [0002] In 1956, American chemist Szwarc first observed an anionic polymerization reaction of styrene without chain transfer and chain termination, and proposed the concept of "living polymerization". Based on the development of living polymerization, Otsu et al. first proposed the idea of ​​using stable free radicals to realize controllable free radical polymerization in 1980. After nearly forty years of development, important living free radical polymerization methods mainly include Iniferter polymerization method, nitro...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08F120/18C08F299/02C08F283/06C08F220/14C08F2/48
CPCC08F2/48C08F120/14C08F120/18C08F283/065C08F299/028
Inventor 马育红马文超杨万泰
Owner BEIJING UNIV OF CHEM TECH
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