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Light polymerization process for preparing block or graft polymer

A technology of graft polymer and photopolymerization, which is applied in the field of free radical polymerization of thioxanthone and its derivatives by visible light irradiation, can solve the problems of damage to biological substrates, and achieve the effect of easy acquisition and low cost

Active Publication Date: 2010-06-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its high energy, ultraviolet light has certain damage to biological substrates (such as biological tissues, cells, proteins), and its application is limited to a certain extent.

Method used

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  • Light polymerization process for preparing block or graft polymer
  • Light polymerization process for preparing block or graft polymer
  • Light polymerization process for preparing block or graft polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 5ml of methyl methacrylate, 0.0254g of isopropyl thioxanthone, 0.0193g of p-(dimethylamino) ethyl benzoate and 5 milliliters of ethyl acetate into a reaction flask with a quartz cap and mix them. Nitrogen, evacuated to remove oxygen, and placed under a xenon lamp for 6 hours. Precipitate with methanol to obtain polymethyl methacrylate, and dissolve it with ethyl acetate for four times to remove residual isopropylthioxanthone.

[0040] Dissolve 0.05 g of the polymer obtained in step 1 in 2.5 ml of glycidyl methacrylate and 7.5 ml of ethyl acetate, add to the reaction bottle, pass through nitrogen, vacuumize and remove oxygen, and place under a xenon lamp (power 500W, add a filter , by light with a wavelength of 380nm to 760nm), the reaction mixture is sampled within a certain period of time, methanol is precipitated, dried, and the molecular weight and molecular weight distribution are measured. Detailed results are shown in Table 1.

[0041] Table 1 Polymethyl met...

Embodiment 2

[0045] Add 5ml of methyl methacrylate, 0.3g of isopropyl thioxanthone, 0.23g of p-(dimethylamino) ethyl benzoate and 5 ml of ethyl acetate into a reaction flask with a quartz cap and mix them. Nitrogen, evacuated to remove oxygen, and placed under a xenon lamp for 4.5 hours. Precipitate with methanol to obtain polymethyl methacrylate, and dissolve it with ethyl acetate for four times to remove residual isopropylthioxanthone.

[0046] Dissolve 0.05 g of the polymer obtained in step 1 in 5 ml of glycidyl methacrylate, add it to the reaction bottle, pass nitrogen, vacuumize and deoxygenate, and place it under a xenon lamp (power 500W, add a filter, and the passing wavelength is 380nm to 760nm) Illumination, the reaction mixture is sampled within a certain period of time, precipitated with methanol, dried, and the molecular weight and molecular weight distribution are measured. Detailed results are shown in Table 2.

[0047] Table 2 Polymethyl methacrylate-b-polyglycidyl methacr...

Embodiment 3

[0051] Add 5ml of methyl methacrylate, 2.032g of isopropyl thioxanthone, 1.544g of p-(dimethylamino) ethyl benzoate and 5 milliliters of ethyl acetate into a reaction flask with a quartz cap and mix them. Nitrogen, evacuated to remove oxygen, and placed under a xenon lamp for 3 hours. Precipitate with methanol to obtain polymethyl methacrylate, and dissolve it with ethyl acetate for four times to remove residual isopropylthioxanthone.

[0052] Dissolve 0.05 g of the polymer obtained in step 1 in 7.5 ml of glycidyl methacrylate and 2.5 ml of ethyl acetate, add to the reaction bottle, pass through nitrogen, vacuumize and remove oxygen, and place under a xenon lamp (power 500W, add a filter , by light with a wavelength of 380nm to 760nm), the reaction mixture is sampled within a certain period of time, methanol is precipitated, dried, and the molecular weight and molecular weight distribution are measured. Detailed results are shown in Table 3.

[0053] Table 3 polymethyl metha...

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Abstract

The invention relates to a photopolymerization method for preparing a block polymer or a graft polymer, belonging to the polymerization field. The method comprises the following steps that: a commercialized photo-initiator with low cost is adopted; a dormant radical is led to a polymer chain, and is added with a comonomer or a graft monomer; under the condition of visible light (ultraviolet light) radiation, the dormant radical is broken for carrying out free radical polymerization. The method uses the visible light (ultraviolet light) as a radiation light source and can be carried out underthe room temperature without a high-temperature violent reaction condition; and the method has mild reaction condition and can be used in certain situations which have severe requirement on the reaction condition.

Description

technical field [0001] The invention relates to a visible light (ultraviolet light) radiation free radical polymerization method of thio(oxy)xanthone and its derivatives, which can be implemented in homogeneous phase, heterogeneous phase polymerization system and surface graft polymerization system. Background technique [0002] Free radical polymerization is an important method for industrial production of polymers, which can polymerize most vinyl monomers under simple process conditions. However, the nature of free radical polymerization determines the uncontrollable behavior of the polymerization reaction, which seriously affects the performance of the polymer. The development of new polymerization methods to predictably and controllably synthesize polymers with special structures has attracted more and more attention. One of the ways to achieve this goal is through the living polymerization process. Compared with traditional polymerization methods, this method can well ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F291/18C08F293/00C08F2/50C08J7/18
Inventor 杨万泰白华栋马育红刘莲英邓建平何辰凤
Owner BEIJING UNIV OF CHEM TECH