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Preparation method of Janus-structure composite emulsion particle

A composite latex and particle technology, which is applied in the synthesis of asymmetric non-spherical composite colloidal particles, can solve the problems of poor fluidity of highly cross-linked Janus particles, inability to distinguish newborn polymer protrusions from the matrix, and complex synthesis processes.

Active Publication Date: 2012-09-05
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a crystalline polymer in view of the complex synthesis process existing in the current technology, the inability to distinguish the nascent polymer protrusions from the matrix, and the poor fluidity of highly cross-linked Janus particles in processing and application. Composite with its incompatible polymer to form the preparation method of Janus latex particles

Method used

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  • Preparation method of Janus-structure composite emulsion particle
  • Preparation method of Janus-structure composite emulsion particle
  • Preparation method of Janus-structure composite emulsion particle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0030] Example 1 Preparation of PVDF / PS Composite Particles with Janus Structure

[0031] Component Mass

[0032] PVDF emulsion 10.5g

[0033] Deionized water 60.0g

[0034] Styrene 6.0g

[0035] Initiator 0.042g

[0036] In a 250ml beaker, 10.5g of PVDF seed emulsion (industrial product) with a solid content of 10.4% and an average particle diameter of 180nm was added, followed by 60.0g of deionized water, and ultrasonically dispersed for 1 hour. The ultrasonically dispersed emulsion was poured into a four-necked reaction flask equipped with a condenser tube, magnetic stirring, and nitrogen gas introduction tube, the stirring was started and nitrogen gas was introduced, and the stirring rate was set at 400 rpm. After 15 minutes, start to heat up the reaction system, add 6.0g styrene to the reaction bottle simultaneously, and open the cooling water of the reflux condenser. When the temperature of the system was raised to 75°C, 5 ml of an aqueous solution containing 0.042 ...

Embodiment example 2-4

[0040] The polymerization reaction time of implementation case 2-4 is respectively 1 hour, 3 hours, 4 hours, and all the other implementation processes are the same as implementation case 1, and the morphological TEM photos of the composite particles prepared by implementation case 2-4 are shown in the attached document respectively. Figure 2-4 . figure 2 The TEM pictures shown are taken by electron energy filtering technology, according to the characteristics of fluorine compounds showing the maximum loss peak at a certain electron energy. From figure 2 In the photo, we can clearly distinguish the two phases of PVDF and PS, as well as the morphology and growth of composite particles. The black part is the PVDF seed, and the white part is the newly grown PS polymer protrusion. Then, compared to the photos taken without electronic energy filtering technology figure 1 From the photos, it is not easy for us to distinguish the two phases of PVDF and PS.

[0041] Depend on ...

Embodiment example 5

[0043] In Example 5, the polymerization temperature was 65° C., the amount of styrene monomer added was 8.0 g, the amount of initiator potassium persulfate was 0.08 g, and the rest of the operating steps were the same as in Example 1. The TEM photo of the composite particle form prepared by embodiment case 5 is shown in the appendix Figure 5 .

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Abstract

The invention relates to a preparation method of a Janus-structure composite emulsion particle. The method comprises the following steps: adding deionized water into a PVDF seed emulsion, performing ultrasonic dispersion for 1 hour, pouring the dispersed emulsion into a reactor equipped with a reflux condensing tube, a stirring device, and a nitrogen introducing port, starting stirring and continuously introducing nitrogen, after 15 min, heating the reaction system, adding monomers, introducing cooling water into the reflux condensing tube; when the system is heated to a reaction temperature, adding an initiator, performing a polymerization reaction at a reaction temperature of 20-80 DEG C for 1-8 hours; drying the emulsion at a reduced pressure and a low temperature to obtain a constant weight so as to obtain the Janus-structure composite particle. Through the selection of PVDF seeds with different particle sizes, the seed monomer mass ratio and the polymerization time, the invention can effectively control the form and the size of the composite particle. The invention is widely applicable to various fields in polymer blending modification, such as compatilizers, self-cleaned coatings, and the like.

Description

Technical field: [0001] The present invention belongs to the synthesis of anisotropic asymmetric non-spherical composite colloidal particles, specifically a method for preparing composite latex particles with a Janus structure. The method takes polyvinylidene fluoride (PVDF) emulsion as a seed and is incompatible with it The polymer monomer is subjected to seed emulsion polymerization to obtain the preparation method of composite latex particles with Janus structure. technical background: [0002] The term "Janus" is used to describe objects or objects of varying chemical composition and / or properties. Janus composite particles can be composed of inorganic-inorganic, inorganic-organic and organic-organic components, and the preparation methods are also various. The preparation methods of Janus structure particles commonly reported in the literature include: template method, microfluidic method, embedding method, etc. Segment copolymer derivation method, dispersion polymeriz...

Claims

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Application Information

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IPC IPC(8): C08F259/08C08F212/08C08F212/14C08F220/18C08F220/32C08F220/44
Inventor 潘明旺祝磊官冰杨连云
Owner HEBEI UNIV OF TECH
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