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Method for preparing hollow ball with temperature response or temperature and pH responses

A temperature-responsive, hollow sphere technology, applied in the preparation of environment-responsive hollow spheres, the field of hollow sphere preparation

Inactive Publication Date: 2010-04-07
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no relevant report on the functionalization of PNIPAM hollow spheres in the current literature.

Method used

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  • Method for preparing hollow ball with temperature response or temperature and pH responses
  • Method for preparing hollow ball with temperature response or temperature and pH responses
  • Method for preparing hollow ball with temperature response or temperature and pH responses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031]Prepare 200ml of 13.6g / L N-isopropylacrylamide aqueous solution. After 15 minutes of passing nitrogen gas in the aqueous N-isopropylacrylamide solution, 2 ml of a N,N-dimethylformamide (DMF) solution of 24 g / L AIBN was added. After sealing the reactor, polymerization was initiated in a 60°C water bath. When the system changed from transparent to light blue, add 4ml of 9.2g / L dimethyl diallyl ammonium chloride with a syringe, and continue to react for 8 hours. Then the system was cooled to room temperature (about 25°C) and stirred for 36 hours. The solution was collected on a centrifuge at a speed of 8000r / min. The obtained PNIPAM hollow sphere has temperature sensitivity, its LCST is about 32° C., the outer diameter is about 800-1000 nm, and the cavity diameter is 600-800 nm. Its electron microscope photo is as figure 1 As shown, the temperature-sensitive curve is as figure 2 shown.

Embodiment 2

[0033] Prepare 200ml of 6.8g / L N-isopropylacrylamide aqueous solution. After passing nitrogen through the above solution for 15 minutes, add 2ml of 35g / L benzoyl peroxide (BPO) in N,N-dimethylformamide (DMF) solution, seal the reactor, and initiate polymerization in a water bath at 60°C . When the system turns from transparent to light blue, add 2ml of 9.2g / L N,N'-methylenebisacrylamide with a syringe, and add 5ml of 8.6g / L acrylamide solution at the same time, and continue the reaction for 12 hours. Then the system was cooled to room temperature (about 25°C) and stirred for 36 hours. The solution was collected in a centrifuge at a speed of 10000r / min. The obtained PNIPAM hollow sphere containing 5 mol% PAM has temperature sensitivity, its LCST is about 36° C., the outer diameter is about 800-1000 nm, and the cavity diameter is 600-800 nm.

Embodiment 3

[0035] Prepare 200ml of 6.8g / L N-isopropylacrylamide aqueous solution. After passing nitrogen gas through the above solution for 15 minutes, add 2 ml of 2 g / L hydrogen peroxide solution and 2 ml of 6 g / L sodium bisulfite solution. After the reactor was sealed, polymerization was initiated in a 50°C water bath. When the system turns from transparent to light blue, add 2ml of 9.2g / L N,N'-methylenebisacrylamide with a syringe, and simultaneously add 5ml of 17.2g / L acrylamide solution. The reaction was continued for 4 hours. Then the system was cooled to room temperature (about 25°C) and stirred for 36 hours. The solution was collected in a centrifuge at a speed of 10000r / min. The obtained PNIPAM hollow sphere containing 10 mol% PAM has temperature sensitivity, its LCST is about 41° C., the outer diameter is about 800-1000 nm, and the cavity diameter is 600-800 nm.

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Abstract

The invention belongs to the functional polymer material field, in particular to a method for making a hollow sphere which takes poly N-isopropyl acrylamide as the main raw material and has the temperature response or the temperature and pH responses. The method is based on the precipitation polymerization reaction of N-isopropyl acrylamide in a water solution and comprises the following steps that: when the temperature is higher than the lowest intersolubility critical temperature, PNIPAM is hydrophobic and the generated PNIPAM low polymer aggregates to a nucleus; in the stage of the nucleusgrowth, a cross-linking agent is added, a layer of cross-linking shell is formed on the periphery of the nucleus, thereby obtaining a nuclear shell structure. At the same time the cross-linking agentisadded in the stage, a water-solubility functional monomer is added, the nucleus is made of PNIPAM, a shell layer consists of a multipolymer taking the PNIPAM as a main body and a water-solubility pol ymer as the auxiliary part. When the temperature is decreased below the lowest intersolubility critical temperature, the PNIPAM or a hollow structure which takes the PNIPAM as the main body and takes other water-solubility compounds as auxiliary parts is formed.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, and relates to the preparation technology of environment-responsive hollow spheres, in particular to a method for preparing hollow spheres with temperature response or temperature response and pH response using poly-N-isopropylacrylamide as the main raw material . Background technique [0002] In recent years, polymer hollow spheres have great potential application value in the field of catalysis, the packaging of slow-release drugs, the simulation of artificial cells, the coating and protection of active biomacromolecules, and pigment carriers. Hollow microspheres with environmental responsiveness are one of the research hotspots in this field because of their huge potential use and practical value. Among them, temperature response is an important type of environmental response. Hollow sphere materials with temperature response capability have important application value in the field...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F20/56C08F2/24C08F4/04C08F4/40C08F4/30C08F8/00
Inventor 吴飞鹏钱健
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI