Method of preparing polymer by emulsion polymerization by controllable free radical Pickering emulsion

A Pickering emulsion and free radical technology, which is used in the preparation of Pickering emulsion and the controllable polymerization of Pickering emulsion stabilized by cellulose nanocrystals, can solve the problem of unclean washing and polymer separation after polymer post-treatment. It has many problems such as complex and residual impurities in the polymer, and achieves the effects of good biocompatibility, excellent stability and rich sources.

Inactive Publication Date: 2017-09-08
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of living radical emulsion polymerization is that the separation process of the polymer is complicated, and demulsifiers need to be added, and there are many types of additives and a large amount of additives, so there are many residual impurities in the polymer, and the post-treatment of the polymer is not clean.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1: Preparation of RAFT active controllable free radical Pickering emulsion: 0.0120 g of cellulose nanocrystals and 0.0032 g of potassium persulfate were added to an ampoule filled with 3.0 ml of distilled water, stirred and sonicated evenly to form a water phase; add 0.5 milliliters of methyl methacrylate and 0.0026 grams of 4-cyanovaleric acid dithiobenzoic acid into a dry ampoule, dissolve completely to form an oil phase; pour the oil phase into the water phase, stir, Ultrasonic pre-emulsification, nitrogen gas deoxygenation for 8 minutes, direct sealing, and reaction at 65 degrees Celsius for 3 hours, the product was cooled, ultrasonic, centrifuged, dialysis, and freeze-dried to obtain a polymer with controllable molecular weight.

Embodiment 2

[0014] Example 2: Preparation of Active Controllable Free Radical Pickering Emulsion by ATRP Method: Add 0.0120 grams of cellulose nanocrystals and 0.0031 grams of ascorbic acid into an ampoule filled with 3.0 milliliters of deionized water, stir and sonicate evenly to form water phase; add 0.01 ml butyl 2-bromoisobutyrate, 0.0019 g copper bromide, 0.0041 g 2,2-bipyridyl and 0.5 ml butyl methacrylate to a dry ampoule to form the oil phase; Pour the oil phase into the water phase, stir, ultrasonically pre-emulsify, fill with nitrogen and deoxygenate for 8 minutes and seal it directly, and place it at 65 degrees Celsius for 3 hours. polymer.

Embodiment 3

[0015] Example 3: Preparation of active controllable free radical Pickering emulsion by NMP method: 0.0120 grams of cellulose nanocrystals, 0.0017 grams of 2,2,6,6-tetramethyl-1-oxypiperidine were added to the In an ampoule bottle of 3.0 ml of deionized water, stir and sonicate evenly to form an aqueous phase; add 0.0004 g of 2-mercaptobenzothiazole and 0.5 ml of styrene into a dry ampoule, dissolve completely, and form an oil phase; The oil phase is poured into the water phase, stirred, ultrasonically pre-emulsified, filled with nitrogen and deoxygenated for 8 minutes and sealed directly, placed at 120 degrees Celsius for 3 hours, and the product is cooled, ultrasonicated, centrifuged, dialyzed, and freeze-dried to obtain a polymer with controllable molecular weight thing.

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PUM

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Abstract

The invention discloses a method of preparing a polymer by emulsion polymerization by a controllable free radical Pickering emulsion. The method is mainly applied to polymerization systems such as an RAFT method, an ATRP method and a NMP method. The method is characterized by comprising the following steps: forming an aqueous phase by cellulose nanocrystals, deionized water and a water soluble component; then forming an oil phase from an oil soluble monomer and an oil soluble component; stirring and emulsifying the mixture to obtain a Pickering emulsion which is excellent in stability; and storing the Pickering emulsion for more than 30 days at room temperature. Cooling, ultrasonic treatment, centrifugalization, dialysis and freezing and drying are performed on the product to obtain a molecular weight controlled polymer. The invention provides the preparation method of the controllable polymerized Pickering emulsion, wherein the preparation method is simple in process, green and environment-friendly and low in cost.

Description

technical field [0001] The invention relates to a preparation method of Pickering emulsion, in particular to a controllable polymerization method of Pickering emulsion stabilized by cellulose nanocrystals, and belongs to the field of polymer material synthesis. Background technique [0002] With the development of science and technology, material science and biological science, bioengineering, chemistry, physics, information science and environmental science continue to intersect and infiltrate, which promotes the invention and utilization of new materials, but it still cannot meet people's growing demand for material functions. Therefore, there is an urgent need for new technologies and new methods to inject new vitality into the research and development of new materials. [0003] In recent years, cellulose nanocrystals (CNC) have been widely concerned in the field of nanomaterial applications due to their abundant sources, renewable, biodegradable, recyclable, low density,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F120/18C08F112/08C08F2/22
CPCC08F2/22C08F112/08C08F120/14C08F120/18
Inventor 陈厚刘蓓芳柏良久王文香梁英
Owner LUDONG UNIVERSITY
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