Method for preparing branched poly(hydroxyethyl 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: 2022-02-11
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 poly(hydroxyethyl methacrylate) by inverse emulsion polymerization at room temperature
  • Method for preparing branched poly(hydroxyethyl methacrylate) by inverse emulsion polymerization at room temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Hydroxyethyl methacrylate (10.4112 g, 0.0800 mol) was dissolved in water (31.2336 g, 300 wt% methacrylate) hydroxyethyl methacrylate, configured to form a hydroxyethyl methacrylate (25 wt%). The hydroxyethyl methacrylate aqueous hydroxyethyl methacrylate was added to the presence of toluene (41.6448 g, 400 wt% methyl methacrylate), SPAN85 (2.0822 g, 5 wt% toluene), Tween 8 (2.0822 g, 5 wt% toluene), reducing agent In the reaction bottle of MPaema (0.2320 g, 0.0010 mol), stirred and vacumed, the oxidant BPO (0.2422 g, 0.0010 mol) was added, and the reaction was reacted in a 25 ° C water bath for 8 hours, and methacrylic acid was measured. The hydroxyethyl ester conversion is 94.3%. The milk was broken with tetrahydrofuran, dried after three water washing, and then dried after three purification, the polymer was obtained. The analysis is analyzed with the Wushu viscometer with the ubus viscosity. The result is as follows: absolute weight average molecular weight M w.MALLS = 2...

Embodiment 2

[0030] Methyl methacrylate (13.0140 g, 0.1000 mol) was dissolved in water (39.0420 g, 300 wt% methacrylate) hydroxyethyl methacrylate, configured to form a hydroxyethyl methacrylate (25 wt%). The hydroxyethyl methacrylate aqueous hydroxyethyl methacrylate was added to the plycetol (52.0560 g, 400 wt% methacrylate), SPAN85 (2.6028 g, 5 wt% toluene), Tween 8 (2.6028 g, 5 wt% toluene), reducing agent In the reaction bottle of MPaema (0.2320 g, 0.0010 mol), stirred and vacumed, the oxidant BPO (0.2422 g, 0.0010 mol) was added, and the reaction was reacted in a 25 ° C water bath for 8 hours, and methacrylic acid was measured. The hydroxyethyl ester conversion is 93.7%. The milk was broken with tetrahydrofuran, dried after three water washing, and then dried after three purification, the polymer was obtained. The analysis is analyzed with the Wushu viscometer with the ubus viscosity. The result is as follows: absolute weight average molecular weight M w.MALLS = 2083000g / mol, mean squa...

Embodiment 3

[0033]Methyl methacrylate (15.6168 g, 0.1200 mol) was dissolved in water (46.8504 g, 300 wt% methacrylate) hydroxyethyl methacrylate, configured to form a hydroxyethyl methacrylate (25 wt%). The hydroxyethyl methacrylate aqueous hydroxyethyl methacrylate (62.4672 g, 400 wt% methyl methacrylate), SPAN85 (3.1234 g, 5 wt% toluene), Tween 8 (3.1234 g, 5 wt% toluene), reducing agent In the reaction bottle of MPaema (0.2320 g, 0.0010 mol), stirred and vacumed, the oxidant BPO (0.2422 g, 0.0010 mol) was added, and the reaction was reacted in a 25 ° C water bath for 8 hours, and methacrylic acid was measured. The hydroxyethyl transformation rate was 94.5%. The milk was broken with tetrahydrofuran, dried after three water washing, and then dried after three purification, the polymer was obtained. The analysis is analyzed with the Wushu viscometer with the ubus viscosity. The result is as follows: absolute weight average molecular weight M w.MALLS = 1671000g / mol, mean square rotary radius...

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Abstract

The invention belongs to the field of polymer synthesis and discloses a method for preparing branched polyhydroxyethyl methacrylate at room temperature by inverse emulsion polymerization. Use dibenzoyl peroxide as an oxidizing agent, 2-methyl-N-[3-(methyl-phenyl-amino)-propyl]-acrylamide as a reducing agent monomer to form a redox initiation system, water and toluene as the medium, the non-ionic surfactant as the emulsifier, and the hydroxyethyl methacrylate as the monomer. Polymerize at room temperature and pressure to obtain branched polyhydroxyethyl methacrylate. The polymerization system of the invention is simple and stable, the synthesis and purification of the reducing agent monomer are simple, and the polymerization cost is greatly reduced. The reaction does not require temperature control and pressurization, low energy consumption, easy operation, and less impact on the environment. The molecular weight of the obtained branched polyhydroxyethyl methacrylate is high, and the molecular weight and branching degree can be regulated in a wide range. This method is of great significance to the theoretical research and large-scale application of branched poly(hydroxyethyl methacrylate).

Description

Technical field [0001] The present invention belongs to the functional polymer preparation in polymer synthesis, and in particular, to a method of phytically preparing hydroxyethyl methacrylate in an inverted emulsion polymerization chamber. Background technique [0002] Polymethyl methacrylate is a hydrophilic polymer. Linear polymethacrylic hydroxyethyl ester is often used as a hydrophilic modified material and a hydrophilic film, a film formation, spinning, and spinning as a water soluble polymer material, can also be used as a flocculant With the oil oil. Crosslinked polymethyl methacrylate is used as a well-transmitted hydrogel material, which can be used as the production of contact lenses and artificial cornea. Compared to hydroxyethyl methacrylate, branched polymethyl methacrylate has a lower viscosity at the same molecular weight. When film formation, spinning, the solution requiring the polymer has a certain viscosity, while the branched polymethyl methacrylate can have...

Claims

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Application Information

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Patent Type & Authority Patents(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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