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Near-infrared light regulated methacrylate monomer polymerization method

A technology of butyl methacrylate and methacrylic acid, which is applied in the field of methacrylate monomer polymerization regulated by near-infrared light, can solve the problems of "living" free radical polymerization system and few reports, and achieve a fast polymerization rate , high conversion rate and small molecular weight distribution index

Inactive Publication Date: 2019-08-16
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the established "living" radical polymerization system regulated by infrared light is rarely reported.

Method used

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  • Near-infrared light regulated methacrylate monomer polymerization method
  • Near-infrared light regulated methacrylate monomer polymerization method
  • Near-infrared light regulated methacrylate monomer polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: the influence of different solvents on polymerization reaction

[0030] MMA (1.0 mL, 9.4 mmol) and CP-I (9.2 mg, 0.047 mmol) were added to a 5.0 mL ampoule preloaded with a stirring bar. Add organic solvent, freeze with liquid nitrogen, evacuate, and inflate three times to remove oxygen in the bottle, and then seal the tube with flame. The ampoule was then placed under near-red light at 25°C to stir the reaction. The light wavelength is 660nm, and the light intensity is 181.8mW / cm 2 , Take out after reacting for 24h, measure the molecular weight and molecular weight distribution of the polymethyl methacrylate (PMMA) that obtains with GPC.

[0031] In order to serve as a control, different experiments were carried out, different volumes of organic solvents were selected, reacted for the same time under the same light conditions, and the molecular weight and molecular weight distribution were measured by GPC. The results are shown in Table 1.

[0032] Th...

Embodiment 2

[0036] Example 2: 181.8mW / cm 2 Polymerization kinetics of MMA under light conditions

[0037] Use [MMA] 0 :[CP-I] 0 =200:1, the amount of MMA is 9.4mmol, 1.0mL DMI is used as a solvent, and the light wavelength is 660nm, at 181.8mW / cm 2 The polymerization reaction of MMA is carried out under the light of sunlight, and the reaction time is 3-21h. When table 2 is different polymerization time, the polymerization situation test result of gained PMMA.

[0038] Table 2 Polymerization kinetics data of MMA

[0039]

[0040] figure 1 is the number average molecular weight (M) of the catalyst-free solution LRP reaction of MMA n，GPC ) and molecular weight distribution (M w / M n ) and monomer conversion. figure 2 is the ln([M] of the above reaction 0 / [M]) versus time.

[0041] The above results show that under the condition of 660nm red light, when the reaction reaches more than 15h, the conversion rate of the monomer reaches about 75%. The molecular weight distribution ...

Embodiment 3

[0043] Example 3: 98.4mW / cm 2 Polymerization kinetics of MMA under light conditions

[0044] Use [MMA] 0 :[CP-I] 0 =200:1, the amount of MMA is 9.4mmol, 1.0mL DMI is used as a solvent, and the light wavelength is 660nm, at 98.4mW / cm 2 The polymerization reaction of MMA is carried out under the light of sunlight, and the reaction time is 5-25h. When table 3 is different polymerization time, the polymerization situation test result of gained PMMA.

[0045] Table 3 Polymerization kinetics data of MMA

[0046]

[0047] Figure 4 is the number average molecular weight (M) of the catalyst-free solution LRP reaction of MMA n，GPC ) and molecular weight distribution (M w / M n ) and monomer conversion. Figure 5 is the ln([M] of the above reaction 0 / [M]) versus time.

[0048] The above results show that at 98.4mW / cm 2 Under light, the conversion rate and molecular weight of MMA increase linearly with time, ln([M] 0 / [M]) shows a good linear relationship with time, and t...

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Abstract

The invention relates to a near-infrared light regulated methacrylate monomer polymerization method. The method comprises the following steps: dissolving a methacrylate monomer and an initiator in anorganic solvent, reacting the obtained solution at 20-30 DEG C under lights with a wavelength of 660-730 nm, and obtaining a polymethacrylate polymer after the completion of the reaction, wherein theinitiator is an iodo compound. The method of the invention has the advantages of simple polymerization component, mild reaction conditions, wide application range of the monomer, high designability ofthe molecular weight, and realization of the active free radical polymerization of the methacrylate monomer without a catalyst.

Description

technical field [0001] The invention relates to the field of iodine transfer active radical polymerization, in particular to a near-infrared light-controlled polymerization method for methacrylate monomers. Background technique [0002] Free radical polymerization is a kind of polymerization mechanism that relies on free radicals to grow and eventually aggregate into macromolecules. It occupies an extremely important position in the development of polymer chemistry. However, due to the existence of chain transfer, traditional free radical polymerization cannot well control the molecular weight and molecular structure of the polymer, which affects the stability and performance of the polymer. In 1956, American chemist Szwarc first proposed the concept of "living polymerization", which triggered a revolution in polymer science. In free radical polymerization, a large number of free radicals are undergoing double-radical termination and chain transfer while growing. People lac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F120/18C08F2/46
CPCC08F2/46C08F120/14C08F120/18
Inventor 程振平田春王鹏张丽芬朱秀林
Owner SUZHOU UNIV
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