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A method for photo-induced organocatalytic preparation of polymers at the microscale

A catalytic preparation and organic catalyst technology, applied in chemical instruments and methods, chemical/physical processes, chemical/physical/physical chemical processes, etc., can solve the problems of many side reactions, slow reaction speed, low initiator efficiency, etc., to achieve The effect of fast reaction speed, less side reactions, and uniform distribution of reaction temperature

Active Publication Date: 2019-09-20
NANJING TECH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

To solve the defects of low initiator efficiency, slow reaction speed and many side reactions in the existing technology

Method used

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  • A method for photo-induced organocatalytic preparation of polymers at the microscale
  • A method for photo-induced organocatalytic preparation of polymers at the microscale
  • A method for photo-induced organocatalytic preparation of polymers at the microscale

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Experimental program
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preparation example Construction

[0030] The preparation method of the organic catalyst refers to the following documents, 10-phenylphenothiazine reference [1], 10-(4-methoxyphenyl) phenothiazine reference [2], 10-(1-naphthalene base) phenothiazine reference [3], 3,7-bis(4-(1,1'-biphenyl))-(10-(1-naphthyl))-10-phenoxazine reference [4 ], 5,10-diphenyl-5,10-dihydrophenazine[5], 5,10-bis(4-methoxyphenyl)-5,10-dihydrophenazine[6], 5 ,10-bis(4-(trifluoromethyl)phenyl)-5,10-dihydrophenazine, 5,10-bis(4-(nitrile)phenyl)-5,10-dihydrophenazine or 5,10-bis(1-naphthyl)-5,10-dihydrophenazine reference [7], 5,10-bis(2-naphthyl)-5,10-dihydrophenazine reference [ 8]. The structures of the compounds prepared in the present invention are consistent with those reported in the literature. In addition, perylene can be purchased directly (CAS: 198-55-0, purity: 98%, manufacturer: Beijing Bailingwei Technology Co., Ltd.)

[0031] [1] Eric B, Kochi K. Journal of the chemical society-perkin transactions, 1995, 8:1057-1064.

[0...

Embodiment 1

[0040] At 20°C, the organic catalyst 10-phenylphenothiazine (31mg, 0.1128mmol) was dissolved in the solvent DMSO (30ml) under nitrogen protection to obtain a homogeneous solution for later use; the initiator α-bromophenylacetic acid methyl ester (345 μl, 2.256mmol) and monomeric MMA (12ml, 112.8mmol) are mixed uniformly and then pumped into the micro-mixer in the micro-reaction device simultaneously with the above-mentioned homogeneous solution respectively, control DMSO flow rate to be (0.059ml / min), MMA flow rate Be (0.024ml / min), pass in the microchannel reactor that has ultraviolet light (380nm) to irradiate after fully mixing, the residence time of mixed system in the microchannel reactor is 60min, and flow velocity is (0.083ml / min), fully Reaction, the product was collected and precipitated with a mixture of methanol and water (1:1). The product was washed 3 times with ethanol to remove residual monomer and solvent in the product. After the product was vacuum-dried at 3...

Embodiment 2

[0042] At 20°C, the organic catalyst 10-phenylphenothiazine (31mg, 0.1128mmol) was dissolved in the solvent DMSO (30ml) under the protection of nitrogen to obtain a homogeneous solution for later use; the initiator 2-bromopropionate methyl (250 μl, 2.256mmol) and monomeric MMA (12ml, 112.8mmol) are mixed uniformly and then pumped into the micro-mixer in the micro-reaction device simultaneously with the above-mentioned homogeneous solution respectively, control DMSO flow rate to be (0.119ml / min), MMA flow rate Be (0.048ml / min), pass in the microchannel reactor that has ultraviolet light (380nm) to irradiate after fully mixing, the residence time of mixed system in the microchannel reactor is 30min, and flow velocity is (0.167ml / min), fully Reaction, the product was collected and precipitated with a mixture of methanol and water (1:1). The product was washed 3 times with ethanol to remove residual monomer and solvent in the product. After the product was vacuum-dried at 30° C. ...

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Abstract

The invention discloses a method for preparing a polymer by micro-scale photo-induced organic catalysis. The method comprises the following steps: using alkyl halide as an initiator in a microreactor; and using an organic small molecule as a catalyst to catalyze atom-transfer radical-polymerization, so as to prepare the polymer. Compared with the prior art, the method provided by the invention has advantages of high reaction speed, controllable molecular weight and molecular weight distribution of a polymerization product, no residue, and wide application in fields of optoelectronic materials and biomedical materials.

Description

technical field [0001] The invention belongs to the field of fine chemistry and polymer material synthesis, and in particular relates to a method for organically catalyzing and preparing poly(meth)acrylate, a polymer without metal residues. Background technique [0002] Poly(meth)acrylate has excellent properties such as low density, strong mechanical strength, low melting point, and high light transmittance, which make it an important polymer. There are also many studies on its polymerization method, among which living radical polymerization (LRP) is a good polymerization method for producing poly(meth)acrylate. Living radical polymerization (LRP) is an important way to carry out molecular design, synthesize polymers with precise primary structure, and realize controllable molecular weight and molecular weight distribution of polymers. It has been widely used in the synthesis of functional polymer materials and polymer brushes. Atom transfer radical polymerization (ATRP) i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/14C08F2/01C08F2/48C08F120/44C08F4/00B01J19/00
Inventor 郭凯掌亚军胡欣朱宁方正崔国朋
Owner NANJING TECH UNIV
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