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CO2 stimuli-responsive solid emulsion

A stimuli-responsive, CO2 technology, applied in the field of emulsion polymerization, can solve problems such as difficult and impossible re-dispersion of emulsions, inactivation of chemical substances, etc.

Active Publication Date: 2017-08-15
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

What's more, conventional emulsions are difficult or impossible to redisperse into the emulsion after coagulation, because the surface active ingredients can deactivate the added chemicals, which is more serious after drying the emulsion into a powder

Method used

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  • CO2 stimuli-responsive solid emulsion
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  • CO2 stimuli-responsive solid emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Example 1. With CO 2 Stimulus response polystyrene emulsion and dry powder preparation

[0062] (1) Synthesis of diblock copolymer surfactant

[0063] The two-block copolymer surfactant polydimethylaminoethyl methacrylate-b-polystyrene is obtained by two-step RAFT polymerization, such as figure 1 Shown.

[0064] In the first step, the RAFT chain transfer agent (2-(dodecyltrithiocarbonate)-2-methylpropionic acid) (0.218g, 0.6mmol), dimethylaminoethyl methacrylate (abbreviated DMAEMA, 0.943g, 6mmol), initiator azobisisobutyronitrile (abbreviated as AIBN, 9.85mg, 0.06mmol) and 1,4-dioxane (1.5mL) were added to the Schlenk tube, and N 2 Remove oxygen for 30min, and then react for 8h at 70°C with stirring. After the reaction, the Schlenk tube was quenched in liquid nitrogen, diluted with 1,4-dioxane (2 mL), and precipitated twice in cold n-hexane. The purified product was vacuum dried overnight at room temperature to obtain a yellow solid, that is, the intermediate product RAFT ...

Embodiment 2

[0077] Example 2. With CO 2 Preparation of stimulus-responsive polymethylmethacrylate-polystyrene emulsion and dry powder

[0078] (1) Synthesis of diblock copolymer surfactant

[0079] The preparation method is the same as in Example 1 of the present invention.

[0080] (2) Emulsion polymerization

[0081] Put PDMAEMA10-b-PS10 (0.077g, 0.025mmol) through CO in an ice water bath 2 Dissolve in deionized water (15g) under the condition of 15min; at the same time, the initiator azobisimidazolinylpropane (21.4mg, 0.085 mmol) is passed CO in an ice water bath 2 Dissolve in another portion of deionized water (5g) under the condition of 15min, and then mix azobisimidazolinylpropane, St (1.111g, 10.67mmol) and methyl methacrylate (abbreviated as MMA, 1.111g, 11.1mmol) ) Add PDMAEMA10-b-PS10 aqueous solution successively, and then pass CO in an ice water bath 2 15min, then react for 6h at 55°C with stirring.

[0082] The number average molecular weight of the polymer latex particles in the o...

Embodiment 3

[0088] Example 3. With CO 2 Preparation of stimulus-responsive polyethylmethacrylate-polystyrene emulsion and dry powder

[0089] (1) Synthesis of diblock copolymer surfactant

[0090] The preparation method is the same as in Example 1 of the present invention.

[0091] (2) Emulsion polymerization

[0092] Put PDMAEMA10-b-PS10 (0.077g, 0.025mmol) through CO in an ice water bath 2 Dissolve in deionized water (15g) under the condition of 15min; at the same time, the initiator azobisimidazolinylpropane (21.4mg, 0.085 mmol) is passed CO in an ice water bath 2 Dissolve in another portion of deionized water (5g) under the condition of 15min, then mix azobisimidazolinylpropane, St (1.111g, 10.67mmol) and ethyl methacrylate (referred to as EMA, 1.111g, 9.73mmol) ) Add PDMAEMA10-b-PS10 aqueous solution successively, and then pass CO in an ice water bath 2 15min, then react for 6h at 55°C with stirring.

[0093] The number average molecular weight of the polymer latex particles in the obtaine...

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Abstract

The invention discloses CO2 stimuli-responsive 'solid emulsion'. A preparation method of the CO2 stimuli-responsive 'solid emulsion' comprises the following steps: (1) performing reversible addition-fragmentation chain transfer polymerization reaction on dimethylaminoethyl methacrylate and styrene, thus obtaining a two-block copolymer surfactant; (2) mixing the two-block copolymer surfactant with a solvent, thus obtaining a mixed solution, feeding CO2 into the mixed solution, then mixing the CO2-added mixed solution with a CO2-added initiator and a CO2-added emulsion polymerization monomer, and performing polymerization reaction, thus obtaining CO2 stimuli-responsive emulsion; (3) agglomerating and drying the CO2 stimuli-responsive emulsion, thus obtaining CO2 stimuli-responsive dry powder. According to the preparation method, the CO2 stimuli-responsive emulsion is prepared, and then the emulsion is dried into emulsion particle dry powder; the dry powder can be recovered into emulsion at any time and put into operation; and the preparation method is easy and convenient to prepare, clean and environmentally friendly, and the CO2 stimuli-responsive dry powder is easy to store and transport; the CO2 stimuli-responsive emulsion can be applied to various common emulsion polymerization monomers.

Description

Technical field [0001] The present invention relates to a CO 2 Stimulus response "solid emulsion", specifically related to a kind of 2 Stimulus response emulsions and dry powders and preparation methods and applications thereof belong to the technical field of emulsion polymerization. Background technique [0002] Generally, the water content of emulsion products exceeds 50-60wt.%, which occupies a large part of energy consumption, transportation and other processing costs, prompting people to study the method of converting emulsion into dry powder and restoring original performance before use. The surface active agent in the emulsion or sludge and the functional groups contained in the polymer chain (such as imidazole) may undergo hydrolysis or other side reactions to reduce the effective content. However, there is no moisture in the dry powder, and the product stored in the dry powder state can have more Long shelf life. Usually the agglomeration of latex particles depends on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/08C08F220/14C08F212/08C08F220/18C08F2/24C08F293/00C08F6/22C08F6/14
CPCC08F2/24C08F6/14C08F6/22C08F112/08C08F212/08C08F220/14C08F220/18C08F293/005C08F220/1804C08L25/14C08L25/06C08L33/08C08F220/1802
Inventor 袁金颖方立城万正一霍猛
Owner TSINGHUA UNIV
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