Method for preparing amphiphilic gradient copolymer

A gradient copolymer and amphiphilic technology, applied in the fields of polymer chemistry and emulsion polymerization, to overcome the instability of latex, the preparation method is simple and easy to control

Inactive Publication Date: 2012-11-07
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This approach has not been attempted in the preparation of amphiphilic gradient copolymers

Method used

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  • Method for preparing amphiphilic gradient copolymer
  • Method for preparing amphiphilic gradient copolymer
  • Method for preparing amphiphilic gradient copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] First disperse 2.5g of dodecylmercaptan and 0.27g of tetrapropylammonium bromide in a mixed solvent composed of 5ml of water and 40ml of acetone, then add 0.5g of sodium hydroxide and stir to dissolve it, and wait for the mixture to drop to Then add 0.95g of carbon disulfide at room temperature, stir for 30 minutes, add 1.91g of dibromopropionic acid, stir and react at room temperature for more than 12 hours, then let it naturally volatilize to 1 / 4 of its original volume, then add hydrochloric acid (2mol / L, 50mL) was slowly acidified, diluted with 150mL of water, filtered and washed to obtain the product, and finally recrystallized with petroleum ether and n-hexane to obtain the basic RAFT reagent S-1-dodecyl-S'-(α-methyl-α'-acetic acid ) Trithiocarbonate. In the three-necked flask, add 1.75 g of S-1-dodecyl-S'-(α-methyl-α'-acetic acid) trithiocarbonate, 4.4 g of dioxane, and 2.16 g of acrylic acid after passing nitrogen gas for 15 minutes. , V-501 initiator 0.14g, ful...

Embodiment 2

[0042] Add 31.16g of water, 1.64g of acetone and 0.2346g of S-1-dodecyl-S'-[(1,3,5,7,9,11,13-heptacarboxy) -Tetradecyl] trithiocarbonate (obtained by the method of Example 1), after stirring and dissolving fully, add 2.88g of acrylic acid, start heating after fully mixing. When the temperature reaches 60°C, add 0.042g of initiator 4,4'-azobis(4-cyanovaleric acid) to dissolve, and start to add dropwise at a rate of 2.1ml / h using a micro-sampling pump after the water bath is heated to 70°C 5.04g of trifluoroethyl methacrylate, heat preservation reaction for 6h. The copolymer emulsion is demulsified with a calcium chloride solution, and then filtered, washed and vacuum-dried to obtain a copolymer product. Depend on image 3 can be seen by 1 H NMR analysis of the relationship between the molar weight of acrylic acid and trifluoroethyl methacrylate monomer units in the copolymer and the conversion rate. The obtained gradient copolymer was dissolved in a mixed solvent of dioxane...

Embodiment 3

[0044] In the three-necked flask, 31.16g of water, 1.64g of tetrahydrofuran and 0.2346g of S-1-dodecyl-S'-[(1,3,5,7,9,11,13-heptacarboxy) were added after passing nitrogen gas for 15 minutes -Tetradecyl] trithiocarbonate (obtained by the method of Example 1), after stirring and dissolving fully, add 2.88g of acrylic acid, start heating after fully mixing. When the temperature reaches 60°C, add 0.042g of initiator 4,4'-azobis(4-cyanovaleric acid) to dissolve, and start to add dropwise at a rate of 2.1ml / h using a micro-sampling pump after the water bath is heated to 70°C 5.04g of trifluoroethyl methacrylate, heat preservation reaction for 6h. The copolymer emulsion is demulsified with a calcium chloride solution, and then filtered, washed and vacuum-dried to obtain a copolymer product. The obtained gradient copolymer was dissolved in a mixed solvent of dioxane and water (volume ratio 94:6), and stirred for more than 12 h to completely dissolve into monomolecular dispersion. T...

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Abstract

The invention relates to a method for preparing an amphiphilic gradient copolymer by using special chain transfer function and self-emulsifying function of an amphiphilic RAFT (Reversible Addition Fragmentation chain Transfer) and adopting a thermal decomposition initiator for initiating without adding an emulsifying agent in a mixed dispersing medium with water as a main body through emulsifier-free emulsion polymerization. When the reactivity ratios of comonomers have large difference, a one-time feeding method is adopted to ensure that a monomer unit spontaneously forms a gradient copolymer; and when the reactivity ratios of comonomers have little difference, a feeding process of replenishing a hydrophobic monomer by adopting a micro sample introduction pump is utilized for forcedly forming the gradient copolymer. The amphiphilic gradient copolymer prepared in the method has a molecular chain with a gradient structure, and can be used in the fields of a macromolecule emulsifying agent, a cosmetic additive or coating dispersing agent; and a nano micelle prepared by the self-assembly of the amphiphilic gradient copolymer is applied to a biomedical vector. The method has the advantages of simple process, low cost and no pollution on environment, and is easy to control a molecular chain structure and a polymerization process.

Description

technical field [0001] The invention relates to the fields of polymer chemistry and emulsion polymerization, in particular to a method for preparing amphiphilic gradient copolymers by using RAFT (reversible addition-fragmentation chain transfer) soap-free emulsion polymerization method and its self-assembly and application. Background technique [0002] Gradient copolymer is a new type of copolymer composed of two monomer units, A and B, whose monomer composition gradually changes along the main chain from A monomer unit to B monomer unit as the molecular weight increases. status. The precise gradient chain structure makes the interaction between the molecular chains of the gradient copolymer gradually and smoothly disperse along the main chain of the polymer molecule, effectively increasing their phase interface affinity, so the gradient copolymer, as a new material with unique structure, can concentrate The best advantages of various component units obtain some special pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00C08F2/38C08F2/22C08F220/22C08F220/06C08L53/00C08J3/00B01F17/52A61K8/90C09D7/12A61K47/32C09K23/52
Inventor 陈艳军罗文孙冲张超灿周辉刘欢
Owner WUHAN UNIV OF TECH
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