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Iodine-regulated reversible-inactivated free radical polymerization catalytic polymerization system

A technology of polymerization catalysis and free radicals, applied in the field of controllable synthesis of polymers, can solve the problems of non-conformity with green chemistry, difficult synthesis, and limitation of practical application, and achieve the effect of controllable molecular weight distribution and great application value

Active Publication Date: 2022-08-09
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of metal catalysts in the above technologies does not conform to the characteristics of green chemistry, and photosensitizers with special NIR absorption are usually expensive or difficult to synthesize
For iodine-regulated polymerization, although the fragile carbon-iodine bond (C-I) can be directly activated by near-infrared light to construct an "active" controllable polymerization system, the efficiency is still very low, and the polymerization process generally takes 15-20 hours, which greatly limits its practical application

Method used

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  • Iodine-regulated reversible-inactivated free radical polymerization catalytic polymerization system
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  • Iodine-regulated reversible-inactivated free radical polymerization catalytic polymerization system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Example 1 Synthesis of catalyst precursor NTCDI-1

[0072] According to the attached image 3 The shown reaction scheme prepares the appendix figure 1 The NTCDI-1 electron-deficient precursor shown in . Specifically, 1.6 g of 1,4,5,8-naphthalenetetracarboxylic dianhydride (NTCDA) and 100 mL of DMF were added to a 250 mL three-necked flask and placed in an oil bath. Subsequently, argon gas was passed through the reaction solution and heated to 80°C to dissolve completely, then 1.75 g of n-butylamine was slowly added using a constant pressure funnel, the orange solution became cloudy, and then the reaction was refluxed at 120°C for 18 hours to complete the reaction. When the reaction solution was cooled to room temperature, a precipitate formed at the bottom, which was filtered and repeatedly washed with ice water. Finally, the obtained solid was dried in a freeze dryer to obtain a pink product NTCDI-1, which was 1 HNMR spectrum as attached Image 6 shown.

Embodiment 2

[0073] Example 2 Synthesis of catalyst precursor BTI-B

[0074] According to the attached Figure 4 The shown reaction scheme prepares the appendix figure 1 The BTI-B electron-deficient precursor shown in . Specifically, 14.2 g of dimethyl butynedioate was added to a three-necked flask and 120 mL of ethanol was added to dissolve. Subsequently, 42.83 g of benzylamine was slowly added through a constant pressure dropping funnel under ice-water bath conditions, then the constant pressure funnel was rinsed with 20 mL of ethanol and added to the reaction flask, stirred at room temperature for 96 hours, resulting in a large amount of yellow solids, filtered and added with a large amount of ethanol Washed to obtain pure maleimide derivative X-1, 1 H NMR spectrum as attached Figure 7 shown. Subsequently, 3 g of maleimide derivative X-1 was added to a clean three-necked flask, and 30 mL of a mixture of acetic acid and water (V 乙酸 / V 水= 4 / 1). The reaction solution was then heat...

Embodiment 3

[0075] Example 3 Synthesis of catalyst precursor TPT-1

[0076] According to the attached Figure 5 The shown reaction scheme prepares the appendix figure 1 The TPT-1 electron-deficient precursor shown in . Specifically, 1 g of 2,4,6-tris(4-pyridyl)-1,3,5-triazine (TPT) and 25 mL of DMF were added to a clean three-necked flask and placed in an oil bath under argon. Heating under conditions, then adding 6.55mL 1-iodobutane to carry out reflux reaction at 120 ° C, the color of the solution changed from a white suspension to brownish purple, and finally changed to dark red black, the reaction was terminated after 24 hours of reaction and cooled to room temperature. Then, the reaction solution was precipitated into a large amount of n-hexane, washed repeatedly with stirring, and the upper layer of n-hexane containing a large amount of DMF was poured off. After repeating this operation for many times, the DMF solvent and the residual unreacted butyl chain on the TPT were removed...

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Abstract

The invention relates to the field of controllable synthesis of macromolecules, in particular to an iodine-regulated reversible-inactivated free radical polymerization catalytic polymerization system, which is characterized in that an inherent electron-deficient compound is used as a catalyst precursor and is reduced into a stable free radical anion catalyst in situ under the action of a common reducing agent; and the construction of a rapid RDRP system under visible light and near-infrared light is easily realized, and almost complete conversion of polymeric monomers is realized within 3-5 hours at room temperature. The catalyst developed by the invention is free of transition metal participation and single wavelength selectivity, and has strong universality for an iodine-regulated RDRP system.

Description

technical field [0001] The invention relates to the field of controllable synthesis of polymers, in particular to an iodine-regulated reversible-deactivated radical polymerization catalytic polymerization system. Background technique [0002] Reversible-Deactivating Radical Polymerization (RDRP), also known as Controlled Radical Polymerization (CRP), as a preparation with narrow dispersion and excellent strategies for functional macromolecules with well-defined structures have attracted widespread attention. Especially with the development of green chemistry and LED technology, light-controlled RDRP is making rapid progress. As a green energy, light is an ideal tool for triggering reactions, and its outstanding ability to control space and time is its most prominent advantage. In addition, reactions activated with different energy demands can also be selectively carried out by changing the wavelength of diffracted light, which also creates the opportunity for "one-pot" re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/00C08F2/38C08F2/46C08F2/48C08F120/14C08F120/20C08F120/18C08F120/32C08F120/28C08F120/44C08F293/00
CPCC08F4/00C08F2/38C08F2/46C08F2/48C08F120/14C08F120/20C08F120/18C08F120/32C08F120/28C08F120/44C08F293/005C08F2438/02
Inventor 程振平赵海涛张丽芬徐想陈帅杰
Owner SUZHOU UNIV
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