Temperature response monomer-based soap-free emulsion polymerization method

A temperature-responsive, soap-free emulsion technology, applied in the field of soap-free emulsion polymerization, to achieve the effects of preparing polymers with high molecular weight, mild polymerization conditions and wide selection.

Active Publication Date: 2017-06-13
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of temperature-responsive monomers to form aggregates above the LCST to further initiate polymerization to achieve soap-free emulsion polymerization has never been reported.

Method used

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  • Temperature response monomer-based soap-free emulsion polymerization method
  • Temperature response monomer-based soap-free emulsion polymerization method
  • Temperature response monomer-based soap-free emulsion polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: The specific steps are as follows: put 0.5g of temperature-responsive monomer MeG1 into a reaction tube, and add 2.5mg of 4,4'-azo(4-cyanovaleric acid) (AVCA) as a water-soluble free radical initiator , and then add 5 mL of distilled water. Add magnets to stir at room temperature to make the mixture even, then seal the reaction tube, replace nitrogen, and then place the reaction tube in an oil bath at 65°C, the system changes from clear to milky white, and reacts for 6 hours. Yield 82%. The polymer molecular weight (Mn) was 1,300,000. The product became a viscous oil.

Embodiment 2

[0023] Embodiment two: concrete steps are as follows:

[0024] Take 0.2 g of temperature-responsive monomer EtG1 into the reaction tube, add 1 mg of 4,4'-azo(4-cyanovaleric acid) (AVCA) as a water-soluble free radical initiator, and then add 2 mL of distilled water. Add magnets at room temperature to stir to make the mixture even, then seal the reaction tube, replace nitrogen, and then place the reaction tube in an oil bath at 65°C, the system changes from clear to milky white, and reacts for 4 hours. Yield 75%. The polymer molecular weight (Mn) was 2,200,000. The product became a viscous oil.

Embodiment 3

[0025] Embodiment three: concrete steps are as follows:

[0026] Take 0.5g of temperature-responsive monomer EtG1 and 0.5g of non-temperature-responsive styrene, add 2.5mg of 4,4'-azo(4-cyanovaleric acid) (AVCA) as a water-soluble free radical initiator, and then add Distilled water 10mL. Add magnets at room temperature to stir to make the mixture even, then seal the reaction tube, replace nitrogen, and then place the reaction tube in an oil bath at 65°C, the system changes from clear to milky white, and reacts for 4 hours. The product is in the form of a viscous emulsion.

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Abstract

The invention provides a temperature response monomer-based soap-free emulsion polymerization method. According to the method, a temperature response monomer water solution is utilized; when the temperature of a system ascends to above a minimum critical solution temperature, the monomer is subjected to dehydration and phase change to generate an aggregate in water, the local concentration of the monomer is increased and the aggregate is similar to a micelle; and the monomer is subjected to polymerization reaction under existence of a water-soluble initiator. The emulsion is formed only through temperature increase under the condition of not adding an emulsifier, so that soap-free emulsion polymerization is achieved, and elusion polymerization can be achieved by the emulsion and a non-temperature response monomer. The temperature response monomer-based monomer soap-free emulsion polymerization method has the advantages that the influence of the emulsifier on the performance of a product can be avoided, and meanwhile, the complicated technology of the emulsifier is omitted.

Description

technical field [0001] The invention relates to a soap-free emulsion polymerization method based on a temperature-responsive monomer. Background technique [0002] Due to the introduction of emulsifiers, the products obtained by emulsion polymerization have the defects caused by residual emulsifiers. If drying needs to break the emulsifier, the process is difficult to control. Soap-free emulsion polymerization refers to emulsion polymerization in which no emulsifier is added or only a small amount of emulsifier is added. Soap-free emulsion polymerization can avoid the influence of emulsifier on product performance, and avoid the complicated process of removing emulsifier. [0003] Temperature-induced phase transition behavior is widely used in the field of controlled release of drugs. Such substances usually have a lower critical solution temperature (LCST). Below the LCST, they are in a well-dissolved state in water. When the temperature is above, its hydrophobicity is gr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/30C08F2/22C08F220/30C08F212/08C08F220/14C08F4/04
CPCC08F2/22C08F4/04C08F120/30C08F212/08C08F220/14C08F220/30C08F220/305
Inventor 张阿方张夏聪李文刘洁董庆豪
Owner SHANGHAI UNIV
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