Preparation method for amphiphilic segmented copolymer with pH value and temperature sensitivities

A multi-block copolymer and amphiphilic technology, which is applied in the field of preparation of amphiphilic multi-block copolymer P-b-P, can solve the problems of ATRP polymerization development limitation, inapplicability of direct polymerization, low reaction rate, etc. The effects of wide range of monomers, high yield, and high polymerization rate

Inactive Publication Date: 2017-05-10
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] GTP is currently widely used in the synthesis of polymethacrylate responsive polymers, but GTP is not based on a free radical mechanism, and its synthesis is limited to methyl methacrylate monomers, while the reaction rate of NMP polymerization in CLRP Low, the range of applicable monomers is narrow; the disadvantage of ATRP polymerization is that it cannot be applied to the direct polymerization of acidic, basic, amide or halogen-containing

Method used

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  • Preparation method for amphiphilic segmented copolymer with pH value and temperature sensitivities
  • Preparation method for amphiphilic segmented copolymer with pH value and temperature sensitivities
  • Preparation method for amphiphilic segmented copolymer with pH value and temperature sensitivities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1: Weigh 2.75 g tert-butyl acrylate (tBA) into a 50 mL single-necked round bottom flask, take 20 mg 4-cyano-4-(thiobenzoyl)valeric acid and 3.52 mg azobis Dissolve isobutyronitrile in a 50 mL beaker by adding 10 mL of dioxane. Then the two were mixed, and the one-necked flask was evacuated at 0 °C through the "T-shaped" tee, and nitrogen gas was introduced. Under the protection of nitrogen, put it in an oil bath at 70°C for 12 h, and stir evenly with magnetic force. After the reaction was completed, the flask was cooled in an ice-water bath and ventilated to the atmosphere, and the cooled solution was added dropwise to 200 mL of methanol / water (v: v = 2: 1) mixed solution, allowed to stand for 4 h, and the upper layer liquid was removed to obtain Pale pink precipitate at the bottom. The above precipitation step was repeated once, and finally the sample was vacuum-dried at 40 °C for 48 h to obtain a pale pink sample, namely poly(tert-butyl acrylate) (P(tBA)).

[...

Embodiment 2

[0028] Compared with Example 1, the amount of tert-butyl acrylate (P(tBA)) in the first step is changed to 2.29 g, and other conditions remain unchanged, then the monomer tert-butyl acrylate, chain transfer agent 4-cyano The molar ratio of base-4-(thiobenzoyl)valeric acid and initiator azobisisobutyronitrile becomes 250: 1: 0.3.

Embodiment 3

[0030] Compared with Example 1, the amount of tert-butyl acrylate (P(tBA)) in the first step is changed to 1.84 g, and other conditions remain unchanged, then the monomer tert-butyl acrylate and chain transfer agent 4-cyanide in the system The molar ratio of base-4-(thiobenzoyl)valeric acid and initiator azobisisobutyronitrile becomes 200: 1: 0.3.

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Abstract

The invention relates to a preparation method for an amphiphilic segmented copolymer with pH value and temperature sensitivities. The preparation method comprises the following steps: by adopting a reversible addition-fragmentation chain transfer polymerization process, synthesizing a macromolecular chain transfer agent namely tert-butyl polyacrylate, and subjecting the tert-butyl polyacrylate with dimethylaminoethyl methacrylate and ethylene glycol monomethyl ether methacrylate to the reversible addition-fragmentation chain transfer (RAFT) polymerization process again so as to synthesize the amphiphilic segmented copolymer P(tBA)-b-P(DMAEMA-co-PEGMA. The segmented copolymer provided by the invention can self-assemble to form micelles in an aqueous solution, and has pH value and temperature sensitivities, wherein the micelles have a critical pH value of 7 and a critical temperature of 37.5 DEG C. The preparation method provided by the invention has the advantages of high yield, relatively wide applicable monomer range, low requirements on reaction conditions, simple and convenient operation, greenness and environmental friendliness; and the amphiphilic segmented copolymer prepared by using the method provided by the invention has double pH value and temperature sensitivities and broad application prospects, and can be applied to the chemical production fields like dye adsorption, the environment protection fields like heavy metal pollution treatment, and the biomedical fields like controllable release of insoluble drugs.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering and new materials, in particular to a pH- and temperature-sensitive amphiphilic multi-block copolymer P(tBA)- b -P(DMAEMA- co - PEGMA) preparation method. Background technique [0002] Environmentally responsive polymer materials refer to polymer materials that undergo some obvious physical or chemical property mutations in the case of minor external environment changes. Such materials usually undergo conformational adjustments in specific environments to respond to Responsive responses to environmental changes lead to phase structure transitions. Utilizing this characteristic of environmentally responsive polymer materials, smart materials with special responsiveness can be designed according to requirements. Amphiphilic multi-block copolymers can self-assemble in some selective solvents to form specific structures such as micelles and vesicles. Combining the advantages of the abo...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F120/18C08J3/09
CPCC08F120/18C08F293/005C08J3/09C08J2353/00
Inventor 杨正龙傅康裕
Owner TONGJI UNIV
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