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Method for synthesising polymers by controlled-radical inverse emulsion polymerisation

An inverse emulsion polymerization, polymer technology, applied in the field of free radical polymerization, can solve the problem of inability to obtain high molecular weight polymers

Pending Publication Date: 2021-06-15
爱森集团
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Despite the use of water-soluble precursors, high molecular weight polymers cannot be obtained with this technique

Method used

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  • Method for synthesising polymers by controlled-radical inverse emulsion polymerisation
  • Method for synthesising polymers by controlled-radical inverse emulsion polymerisation
  • Method for synthesising polymers by controlled-radical inverse emulsion polymerisation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] Example 1: Synthesis of Water Soluble Precursors

[0097] In a 50 kg reactor, at room temperature (20° C.), 2 kg of O-ethyl-S-(1-methoxycarbonyl) ethyl dithiocarbonate, 10 kg of acrylamide, 12 Kg of water, 20 kg of acetic acid and 140 g of azo initiator (V044). The mixture was degassed by bubbling nitrogen, then heated to 60°C with stirring. Polymerization was carried out with stirring for 3 hours.

[0098] The water-soluble precursor thus obtained corresponds to formula (I), wherein:

[0099] Z=O,

[0100] R 1 =CH 2 -CH 3 ,

[0101] A=(CH(C(=O)NH 2 )-CH 2 ) n

[0102] n=7,

[0103] R 2 =CH(CH 3 )-C(=O)-O-CH 3 .

[0104] In particular, the precursor passes through the D 2 in O 1 H NMR spectrum (300.13MHz) to characterize ( figure 2 ).

Embodiment 2

[0105] Example 2: Synthesis of polymer P1 in an inverse emulsion according to the invention

[0106] Preparation of the aqueous phase: 400 g of acrylamide (50% by weight in water), 90 g of acrylic acid, 150 g of water and 0.0015% by weight of the water-soluble precursor of example 1 relative to the emulsion were mixed. The aqueous phase was neutralized with 90 g of sodium hydroxide (50% by weight in water).

[0107] Preparation of the organic phase: All water-in-oil surfactants (2.5% by weight of alkanolamides relative to the emulsion and 3% by weight of stearyl methacrylate relative to the emulsion) were mixed in 200 g of oil of the ISOPAR type (Isopar N and L).

[0108] The aqueous and organic phases are mixed and emulsified. The emulsion was then degassed for 60 minutes before polymerization was initiated by adding the reducing agent sodium metabisulfite (MBS).

[0109] At the end of the polymerization, the polymer obtained is recovered by precipitation in acetone.

Embodiment 3

[0110] Example 3: Synthesis of Polymer P2 in Inverse Emulsion

[0111] Polymer P2 was synthesized as described in Example 2, substituting sodium hypophosphite for the water-soluble precursor.

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Abstract

The present invention concerns a method for preparing a polymer by inverse emulsion polymerisation, the method comprising the following steps: a) preparing an aqueous phase comprising at least one water-soluble monomer and at least one water-soluble precursor of formula (I): formula (I) b) preparing an organic phase comprising a lipophilic solvent and at least one water-in-oil surfactant, c) mixing the aqueous phase and the organic phase by stirring in order to form an inverse emulsion, d) once the inverse emulsion is formed, adding a radical polymerisation initiator to the inverse emulsion, and obtaining a polymer by polymerisation of the at least one water-soluble monomer.

Description

technical field [0001] The present invention relates to a new method for free radical polymerization in reverse emulsion. Background technique [0002] The simplicity of conventional free radical polymerization makes it a method of choice for the synthesis of high molecular weight polymers at an industrial scale. In fact, it works with a wide range of monomers, is tolerant to functional groups carried by a wide range of monomers or to impurities present in a wide range of reaction media, is reproducible, compatible with homogeneous or heterogeneous media, and can Performed in protic solvents, including water. [0003] However, this technique cannot obtain precise chain lengths. In addition, chains of different sizes imply a rather high dispersion. Compositional drift also occurs during conventional free-radical copolymerization of two types of monomers if one type of monomer is consumed much faster than the other. It is then difficult to obtain polymers with macromolecul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/32C08F2/38C08L33/26
CPCC08F2/32C08F2/38C08L33/26C08F220/56C08F220/06C08F293/005C08F2400/02
Inventor O·博朗E·里德T·勒布朗克
Owner 爱森集团