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Polymethacrylate polymer with ultra-narrow molecular weight distribution and preparation method thereof

A technology of polymethacrylic acid and methacrylic acid, which is applied in the field of ultra-narrow molecular weight distribution polymethacrylate polymers and its preparation, can solve the problems of low energy, difficult removal, and difficult synthesis of catalysts, and achieve near-infrared light energy Low, penetrating effect

Active Publication Date: 2021-06-01
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low energy of near-infrared light, it is a great challenge to achieve polymerization under near-infrared light, which often requires the participation of external photocatalysts, and these catalysts are usually difficult to synthesize and difficult to remove from the product.

Method used

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  • Polymethacrylate polymer with ultra-narrow molecular weight distribution and preparation method thereof
  • Polymethacrylate polymer with ultra-narrow molecular weight distribution and preparation method thereof
  • Polymethacrylate polymer with ultra-narrow molecular weight distribution and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The research of the effect of embodiment 1 sodium iodide consumption on polymerization

[0043] The effect of sodium iodide dosage on monomer conversion and polymer molecular weight distribution was investigated by using ethyl α-bromophenylacetate as initiator, sodium iodide as nucleophilic substitution reagent and catalyst, and tetramethylurea as solvent.

[0044] Specifically, molar ratio [MMA] 0 :[EBPA] 0 :[NaI] 0 =150:1:1~6, respectively add MMA (0.7mL, 6.6mmol), EBPA (7.7μL, 0.0439mmol), different amounts of sodium iodide and tetramethylurea (0.35mL) into a clean ampoule Add a clean magnetic stir bar. The mixed solution is light yellow, put the ampoule bottle in liquid nitrogen to freeze the solution, then pump it for 30-60 seconds, then let it thaw and dissolve at room temperature while passing in argon protective gas, then freeze, pump, Thaw and inflate, and perform three cycles in sequence to remove the oxygen in the ampoule. After deoxygenation, quickly mo...

Embodiment 2

[0048] Polymerization research of embodiment 2 benzyl methacrylate (BnMA) and water-soluble monomer hydroxypropyl methacrylate (HPMA)

[0049] In addition to simple monomers like methyl methacrylate, other functional monomers such as benzyl methacrylate (BnMA) and the water-soluble monomer hydroxypropyl methacrylate (HPMA) are also used in this polymerization system has been studied.

[0050] Specifically, for BnMA, fix [BnMA]:[EBPA]:[NaI]=150:1:5, add BnMA (0.7mL), EBPA (4.82μL), NaI (20.6mg), TMU (0.35mL) In a 2 ml clean ampoule bottle, a stirring bar was added, and the subsequent deoxygenation, tube sealing and polymerization process were the same as in Example 1. For HPMA, also fix [HPMA]:[EBPA]:[NaI]=150:1:5, add HPMA (0.7mL), EBPA (6.0μL), NaI (25.9mg), TMU (0.35mL) to 2 Add a stirrer to a clean ampoule bottle in milliliters, and the subsequent oxygen removal, tube sealing and polymerization process are the same as above. After 18 hours of reaction, transfer to a dark ...

Embodiment 3

[0053] Polymerization kinetics research of embodiment 3MMA monomer

[0054] In order to study the aggregation process in detail, [MMA] 0 :[EBPA] 0 :[NaI] 0 =150:1:5 has studied the in-situ bromine-iodine conversion polymerization kinetics process of MMA monomer under near-infrared light as a charge ratio, and the steps are as follows:

[0055] Prepare 8 clean 2ml ampoules, add MMA (0.7mL, 6.6mmol), EBPA (7.7μL, 0.0439mmol), NaI (33mg) and TMU (0.35mL) to each ampoule, and add one Clean magnetic stir bar. The mixed solution is light yellow. Put all the ampoules in liquid nitrogen to freeze the solution, then pump for 30-60 seconds, and then let it thaw and dissolve at room temperature while passing in argon protective gas, and then freeze and pump again. Thaw and inflate, and perform three cycles in sequence to remove the oxygen in the ampoule. After deoxygenation, quickly move all ampoules to the mouth of the spray gun for flame sealing. Transfer all sealed ampoules to a...

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Abstract

The invention relates to a method for synthesizing a polymethacrylate polymer with ultra-narrow molecular weight distribution through near-infrared light control. The molecular weight distribution range D of the polymethacrylate polymer prepared by the method disclosed by the invention is 1.03-1.10. The preparation method comprises the following steps of: uniformly mixing a methacrylate monomer, an alkyl bromide initiator, iodide and a solvent, and carrying out light-operated in-situ bromine-iodine conversion polymerization reaction on the obtained mixed solution under the irradiation of near-infrared light. According to the invention, the polymethacrylate polymer with ultra-narrow molecular weight distribution is prepared by using near-infrared light-controlled in-situ bromine-iodine conversion RDRP technology at room temperature, the components are simple, the synthesis method is green, simple and convenient, the polymerization process accords with the characteristics of 'active' free radical polymerization, and the prepared polymer not only has controllable component size, but also has ultra-narrow molecular weight distribution (D<=1.10).

Description

technical field [0001] The invention relates to the field of polymer preparation with controllable molecular weight and molecular weight distribution, in particular to an ultra-narrow molecular weight distribution polymethacrylate polymer and a preparation method. Background technique [0002] The molecular weight distribution of a polymer is one of the important parameters of the polymer structure, which determines the final properties and applications of the polymer. For example, the thermal properties, mechanical properties, flow modification properties and crystallization properties of some polymers will be improved with the decrease of dispersibility. Further, ultra-narrow molecular weight distribution Polymers are widely used as calibration standards for gel permeation chromatography (GPC). However, the precise preparation of this class of polymers faces enormous challenges. The preparation strategies of ultra-narrow molecular weight distribution polymers are mainl...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08F120/18C08F120/20C08F2/46
CPCC08F120/14C08F120/18C08F120/20C08F2/46
Inventor 张丽芬赵海涛程振平李海辉朱秀林
Owner SUZHOU UNIV
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