Method for preparing branched polyhydroxyethyl methacrylate by inverse emulsion polymerization at room temperature

A technology of branched poly(hydroxyethyl methacrylate) and inverse emulsion polymerization, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid amides, etc. Long time and other problems, to achieve the effect of simple and stable reaction system, high monomer conversion rate and short reaction time

Active Publication Date: 2020-07-03
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the thiol chain transfer hyperbranched polymerization method needs to introduce monomers with mercapto groups, most of which have an unpleasant smell; while ATRP polymerization requires the introduction of transition metal compounds, which seriously affects the application range of the product, and the cost is high and the conditions are harsh.
There are also two common disadvantages in the preparation of polyhydroxyethyl methacrylate by these two polymerization methods: the polymerization time required for high monomer conversion is long, and the molecular weight of the product is low

Method used

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  • Method for preparing branched polyhydroxyethyl methacrylate by inverse emulsion polymerization at room temperature
  • Method for preparing branched polyhydroxyethyl methacrylate by inverse emulsion polymerization at room temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Hydroxyethyl methacrylate (10.4112g, 0.0800mol) was added into water (31.2336g, 300wt% hydroxyethyl methacrylate) to dissolve, and an aqueous solution of hydroxyethyl methacrylate (25wt%) was configured. The aqueous solution of hydroxyethyl methacrylate was added to a mixture of toluene (41.6448g, 400wt% hydroxyethyl methacrylate), Span85 (2.0822g, 5wt% toluene), Tween80 (2.0822g, 5wt% toluene), reducing agent single MPAEMA (0.2320g, 0.0010mol) in a reaction flask, stirred evenly and evacuated oxygen, then added the oxidant BPO (0.2422g, 0.0010mol), placed in a water bath at 25°C for 8 hours, measured methacrylic acid The conversion rate of hydroxyethyl ester was 94.3%. Demulsify with tetrahydrofuran, wash with water three times and then dry, then purify three times and then dry to obtain polymer. The polymer is analyzed by dynamic and static light scattering and Ubbelohde viscometer, the results are as follows: absolute weight average molecular weight M w.MALLS =2442...

Embodiment 2

[0030] Hydroxyethyl methacrylate (13.0140g, 0.1000mol) was added into water (39.0420g, 300wt% hydroxyethyl methacrylate) to dissolve, and an aqueous solution of hydroxyethyl methacrylate (25wt%) was configured. The aqueous solution of hydroxyethyl methacrylate was added to a mixture of toluene (52.0560g, 400wt% hydroxyethyl methacrylate), Span85 (2.6028g, 5wt% toluene), Tween80 (2.6028g, 5wt% toluene), reducing agent single MPAEMA (0.2320g, 0.0010mol) in a reaction flask, stirred evenly and evacuated oxygen, then added the oxidant BPO (0.2422g, 0.0010mol), placed in a water bath at 25°C for 8 hours, measured methacrylic acid The conversion rate of hydroxyethyl ester was 93.7%. Demulsify with tetrahydrofuran, wash with water three times and then dry, then purify three times and then dry to obtain polymer. The polymer is analyzed by dynamic and static light scattering and Ubbelohde viscometer, the results are as follows: absolute weight average molecular weight M w.MALLS =2083...

Embodiment 3

[0033]Hydroxyethyl methacrylate (15.6168g, 0.1200mol) was added into water (46.8504g, 300wt% hydroxyethyl methacrylate) to dissolve, and an aqueous solution of hydroxyethyl methacrylate (25wt%) was configured. The aqueous solution of hydroxyethyl methacrylate was added to a mixture of toluene (62.4672g, 400wt% hydroxyethyl methacrylate), Span85 (3.1234g, 5wt% toluene), Tween80 (3.1234g, 5wt% toluene), reducing agent single MPAEMA (0.2320g, 0.0010mol) in a reaction flask, stirred evenly and evacuated oxygen, then added the oxidant BPO (0.2422g, 0.0010mol), placed in a water bath at 25°C for 8 hours, measured methacrylic acid The conversion rate of hydroxyethyl ester was 94.5%. Demulsify with tetrahydrofuran, wash with water three times and then dry, then purify three times and then dry to obtain polymer. The polymer is analyzed by dynamic and static light scattering and Ubbelohde viscometer, the results are as follows: absolute weight average molecular weight M w.MALLS =16710...

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Abstract

The invention belongs to the field of polymer synthesis, and discloses a method for preparing branched polyhydroxyethyl methacrylate at the room temperature through inverse emulsion polymerization. Dibenzoyl peroxide is used as an oxidizing agent, and 2-methyl-N-[3-(methyl-phenyl-amino)-propyl]-acrylamide is used as a reducing agent monomer to form a redox initiation system; water and methylbenzene are taken as a medium, a nonionic surfactant is used as an emulsifier, hydroxyethyl methacrylate is taken as a monomer, and polymerization is performed at the room temperature under a normal pressure to obtain branched hydroxyethyl methacrylate. The polymerization system is simple and stable, the synthesis and purification of the reducing agent monomer are simple, and the polymerization cost isgreatly reduced. The reaction does not need temperature control and pressurization, the energy consumption is low, the operation is easy, and the influence on the environment is small. The molecular weight of obtained branched polyhydroxyethyl methacrylate is high, and the molecular weight and branching degree can be regulated and controlled in a wide range. The method has important significance for theoretical research and large-scale application of branched polyhydroxyethyl methacrylate.

Description

technical field [0001] The invention belongs to the field of preparation of functional polymers in polymer synthesis, and in particular relates to a method for preparing branched polyhydroxyethyl methacrylate at room temperature by inverse emulsion polymerization. Background technique [0002] Poly(hydroxyethyl methacrylate) is a hydrophilic polymer. Linear poly(hydroxyethyl methacrylate) is often used as a hydrophilic modified material, as well as hydrophilic film, fiber film forming, spinning, and as a water-soluble polymer material, it can also be used as a flocculant with oil repellant. Cross-linked poly(hydroxyethyl methacrylate), as a hydrogel material with better light transmission, can be used to make contact lenses and artificial corneas. Compared with linear polyhydroxyethylmethacrylate, branched polyhydroxyethylmethacrylate has lower viscosity at the same molecular weight. When forming a film and spinning, the polymer solution is required to have a certain visc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/20C08F220/60C08F2/30C08F4/40C07C231/02C07C233/38
CPCC08F220/20C08F2/30C08F4/40C07C231/02C07C233/38C08F220/60C08F120/20C08F226/06
Inventor 黄文艳朱迪赵毅卓蒋必彪薛小强杨宏军江力蒋其民
Owner CHANGZHOU UNIV
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