Hollow microsphere and preparation method thereof

A microsphere and hollow technology, applied in the field of hollow microspheres and their preparation, can solve the problems of difficult to control stability, strict requirements for olefinic monomers, complex synthesis methods, etc.

Pending Publication Date: 2021-05-18
NANOSPHERE SHANGHAI +1
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Problems solved by technology

The traditional core-shell template method to prepare hollow microspheres generally uses the combination of vinyl monomers with rapid polymerization characteristics and spray drying technology to quickly form a layer of polymer shell on the surface of the droplet. It grows on the inner surface to prepare hollow spheres with a composite structure. However, the synthesis method is complicated, the stability is difficult to control, and the ethylenic monomers used are demanding. In addition, it needs to be combined with spray drying technology. The cost is high and the product application is limited.
[0003] Although it is possible to adjust the ratio of alcohol to olefin and different reaction conditions, react under certain conditions to form the target product, and then wash away the core substance with an organic solvent to obtain hollow microspheres with different microstructures, but the reaction conditions are not easy to control. , the polymerization of the water phase cannot achieve the stability of the polymerization process, and the particle size of the obtained microspheres ranges from 0.1 to 1000um, and its uniform dispersion is not good

Method used

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preparation example Construction

[0025] The embodiment of the present application provides a method for preparing hollow microspheres, comprising the following steps:

[0026] In parts by mass, 0-100 parts of air-tight monomers, 10-100 parts of acrylate monomers, 0-50 parts of amide monomers, 10-100 parts of olefin monomers and 0-10 parts of initiators, Mix 0-10 parts of cross-linking agent and 20-60 parts of core material, stir in an oil phase tank of 0-15Mpa to prepare the oil phase;

[0027] In parts by mass, 100 parts of deionized water, 0.5-10 parts of inorganic dispersant, 0.5-50 parts of inorganic salt, 0.01-5 parts of surfactant, 0.01-5 parts of thickener, and 0.01-5 parts of molecular weight regulator The ratio is added to the water phase tank in sequence, and the water phase is prepared by stirring evenly under normal pressure. The inorganic dispersant is a sol-like solution obtained by adding the cationic salt of the inorganic particles to the anionic salt of the inorganic particles;

[0028] Afte...

Embodiment 1

[0047] Preparation of the water phase: Take 1500 parts of the prepared silver chloride water phase, then add 0.1 part of sodium dodecylsulfonate, stir vigorously to prepare the water phase, and the pH value of the water phase is 7.

[0048] Preparation of oil phase: Take 170 parts of acrylonitrile, 20 parts of methacrylonitrile, 10 parts of methyl methacrylate, 25 parts of pentane, 1 part of azobisisobutyronitrile, and 0.1 part of divinylbenzene to prepare an oil phase. The oil phase can be mixed evenly under the pressure of 0.6Mpa.

[0049] Then mix the oil phase with the water phase, homogenize for 30 minutes under stirring at 10,000 rpm, put the emulsion in a homogenizing tank, and polymerize at a stirring speed of 300 rpm, the polymerization temperature is 60°C, and the polymerization time is 24 hours.

[0050] After the reaction is over, add a defoamer to the kettle, and slowly release the pressure to allow the pentane to escape. Suction filtration, filter cake drying, s...

Embodiment 2

[0052] Preparation of the water phase: Take 1500 parts of the prepared magnesium hydroxide water phase, then add 0.1 part of sodium dodecylsulfonate into it, stir vigorously to prepare the water phase, and the pH value of the water phase is 7.

[0053] Preparation of oil phase: Take 170 parts of acrylonitrile, 20 parts of methacrylonitrile, 10 parts of methyl methacrylate, 25 parts of pentane, 1 part of azobisisobutyronitrile and 0.1 part of divinylbenzene to prepare an oil phase. The oil phase can be mixed evenly under the pressure of 10Mpa.

[0054] Mix the oil phase and the water phase in a homogenization tank, homogenize for 30 minutes under stirring at 10,000 rpm, transfer the homogenized emulsion to the reactor, and polymerize at a stirring speed of 300 rpm / min at a polymerization temperature of 50°C and a polymerization time of 24 hours.

[0055] After the reaction was finished, suction filtration and drying of the filter cake resulted in core-containing microspheres wi...

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Abstract

The invention provides a hollow microsphere and a preparation method thereof, and belongs to the field of polymer functional materials. The method comprises the steps of: mixing 0-100 parts by mass of an airtight monomer, 10-100 parts by mass of an acrylate monomer, 0-50 parts by mass of an amide monomer, 10-100 parts by mass of an olefin monomer, 0-10 parts by mass of an initiator, 0-10 parts by mass of a cross-linking agent and 20-60 parts by mass of a core material, and stirring the mixture in an oil phase kettle of 0-15Mpa to prepare an oil phase; sequentially adding 100 parts by mass of deionized water, 0.5-10 parts by mass of an inorganic dispersant, 0.5-50 parts by mass of an inorganic salt, 0.01-5 parts by mass of a surfactant, 0.01-5 parts by mass of a thickening agent and 0.01-5 parts by mass of a molecular weight regulator into a water phase kettle according to the proportion, and uniformly stirring the substances at normal pressure to prepare a water phase; fully stirring the oil phase and the water phase respectively, transferring the oil phase and the water phase into a homogenizing kettle according to a proportion of 1:1-10 to be homogenized for 0.5-1h, and selecting a homogenizing rotating speed of 500-10000rpm / min; and after the homogenization is finished, performing heating to 50-60DEG C, carrying out reaction for 24h, carrying out suction filtration on the homogenized reaction liquid, and drying a filter cake to obtain the hollow microsphere.

Description

technical field [0001] The invention relates to the field of polymer functional materials, in particular to a hollow microsphere and a preparation method thereof. Background technique [0002] In recent years, polymer hollow microspheres, represented by expandable microspheres, have become a hot product. It consists of a low-boiling core material as the core, and a thermoplastic polymer as the shell. When heated and expanded, the product density can be reduced to the original 1000. It is widely used in the research of lightweight technology. The traditional core-shell template method to prepare hollow microspheres generally uses the combination of vinyl monomers with rapid polymerization characteristics and spray drying technology to quickly form a layer of polymer shell on the surface of the droplet, and use solvent volatilization to induce the shell-forming substance Its inner surface grows to prepare hollow spheres with a composite structure. However, its synthesis metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14
CPCB01J13/14
Inventor 成晓军刘利利
Owner NANOSPHERE SHANGHAI
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