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A kind of preparation method of branched amphiphilic random copolymer self-assembled micelle emulsifier

A technology of random copolymer and self-assembly, which is applied in the field of preparation of branched amphiphilic random copolymer self-assembled micelles as emulsifier and branched amphiphilic random copolymer self-assembled micelle emulsifier, can solve the problem of The research on the factors of emulsification performance is not comprehensive, etc., to achieve the effect of excellent long-term stability, obvious pH responsiveness, and good universality

Active Publication Date: 2017-01-11
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, there are many reports on self-assembled micelles of linear amphiphilic random and block copolymers as emulsifiers, and the relevant reports on self-assembled micelles of branched amphiphilic copolymers mostly focus on the molecular design of branched amphiphilic copolymers. , branched amphiphilic copolymer assembly morphology control, the application of branched amphiphilic copolymer micelles in the field of drug sustained release and biomimetic biology, however, the use of branched amphiphilic copolymer self-assembled micelles as emulsifiers There are few reports, and the exploration of the factors affecting its emulsifying performance is not comprehensive. Therefore, the self-assembled micelles of branched amphiphilic copolymers have broad prospects as emulsifiers

Method used

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  • A kind of preparation method of branched amphiphilic random copolymer self-assembled micelle emulsifier
  • A kind of preparation method of branched amphiphilic random copolymer self-assembled micelle emulsifier
  • A kind of preparation method of branched amphiphilic random copolymer self-assembled micelle emulsifier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of branched amphiphilic random copolymer poly(styrene-co-acrylic acid) BPSAA

[0034] In a 100 mL dry round bottom flask, add the initiator α-bromopropionate ethyl ester (EPN-Br), the comonomer styrene (St) and tert-butyl acrylate (tBA) (nSt:ntBA=1:1 ), an appropriate amount of branched monomer p-chloromethylstyrene (CMS), catalyst cuprous chloride (CuCl), ligand bipyridine (bpy), solvent 1,4-dioxane, in which EPN-Br , CuCl and bpy in a molar ratio of 1:2:4. Thoroughly stir and dissolve the feed material, continue to pass nitrogen gas for 20 minutes, freeze with liquid nitrogen and vacuumize, and cycle like this for 3 times, then seal the flask and add it to a 90°C oil bath to react for 24 hours. After the reaction, the product was cooled to room temperature, diluted with tetrahydrofuran (THF), and impurities such as excess catalyst were removed through a basic alumina chromatography column. The filtrate was purified by precipitation with a methanol / wat...

Embodiment 2

[0040] (1) Preparation of branched amphiphilic random copolymer poly(styrene-co-acrylic acid) BPSAA, method is the same as step (1) in Example 1

[0041] (2) Preparation of BPSAA copolymer self-assembled micelles

[0042]BPSAA was dissolved in DMF such that the concentration of copolymer was 20 mg / mL. Take an appropriate amount of DMF solution of BPSAA, under magnetic stirring, slowly add ultrapure water to the above solution to induce self-assembly, the dropping speed is about 8-10μL / min, until the solution appears blue opalescence, stop adding water, continue stirring for 3h , the above solution was reversely dripped into a large amount of water to fix the micellar structure, and after stirring for 3 hours, the solution was moved into a dialysis bag, dialyzed with deionized water to remove DMF in the solution, and the water was changed every 8 hours, and dialyzed for one week to obtain BPSAA micellar solution. Use 1mol / L NaOH or HCl aqueous solution to adjust the pH value ...

Embodiment 3

[0045] (1) Preparation of branched amphiphilic random copolymer poly(styrene-co-acrylic acid) BPSAA, method is the same as step (1) in Example 1

[0046] (2) The preparation of BPSAA copolymer self-assembled micelle, method is with step (2) in the embodiment 1

[0047] (3) BPSAA copolymer self-assembled micelles as emulsifier to prepare emulsion

[0048] Use 1mol / L NaCl solution to adjust the salt concentration of the BPSAA micellar solution (0.0001~0.1mol / L), take 3mL of the above-mentioned micellar solution with different salt concentrations and 3mL of white oil in a 15mL emulsification bottle, and use XHF-D high-speed The disperser was homogenized at 8000 rpm for 2 minutes to obtain the desired emulsion. Figure 4 It is a digital photograph of the appearance of white oil / water emulsion stabilized by BPSAA micellar aqueous solutions with different NaCl salt concentrations. It can be seen from the figure that when the NaCl salt concentration in the system reaches 0.1mol / L, B...

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Abstract

The invention discloses a preparation method of a branched parents random copolymer self-assembly micelle emulsifier. The preparation method comprises the following steps: firstly, preparing branched parents random copolymer poly(styrene-co-crylic acid) by atom transfer radical polymerization, and then forming micellar particles from the copolymer in a selective solvent in a self-assembling manner, wherein the micellar particles can be applied to the field of cosmetics or biological medicines as an emulsifier. The micelle emulsifier prepared by the method is combined with dual advantages of a high molecular surfactant and a particle emulsifier, and also has good emulsifying efficiency, and good universality and compatibility at low micellar concentration (1.25-2.00mg / mL).

Description

technical field [0001] The invention relates to a preparation method of a branched amphiphilic random copolymer self-assembled micelle emulsifier, which introduces a branched structure through molecular design, especially involves using the branched amphiphilic random copolymer self-assembled micelle as an emulsifier The new use of the invention belongs to the technical field of polymer materials. Background technique [0002] Amphiphilic random copolymer self-assembled micelles are considered as ideal model particles for emulsifiers due to their excellent structure controllability and functionality. , and a large number of grafted chains are wound around the micelles, so they have the dual advantages of emulsifiers and macromolecular surfactants, and show more excellent emulsifying properties than rigid particles. Therefore, if the copolymer self-assembled micelles containing longer and more branched chains are used as emulsifiers, the synergistic stabilization effect of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/02C08L25/14C08F212/08C08F220/18C08F212/14C08F8/12
Inventor 顾瑶刘晓亚王婷魏玮孙家娣孙建华赵栋华胡琼卢荣杰孟龙
Owner JIANGNAN UNIV
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