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Hollow expandable microsphere with super-large particle size and preparation method thereof

A technology of expanding microspheres and hollowing, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problem that the hollow core-shell structure microspheres have not been further studied, the uniformity of the particle size of the hollow microspheres cannot be achieved, and the expandable microspheres cannot be obtained. Ball and other problems, to achieve uniform particle size, increase adsorption, environmental protection in the process

Pending Publication Date: 2021-12-03
NANOSPHERE SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although the existing technology can prepare large-pore solid microspheres, there is no further research on hollow core-shell microspheres; and the preparation methods of expandable microspheres reported in current patent documents are mostly based on the acidic silica water phase. For the water phase, the pH of the water phase needs to be adjusted between 1-4 with acidic substances such as hydrochloric acid, and 20-30% of saturated electrolyte needs to be added to keep the water phase stable. The particle size of the prepared microspheres is mostly below 30um, even if The large particle size can be achieved by adjusting the polymerization process, but the uniformity of the particle size of the hollow microspheres cannot be achieved, and the multi-core structure phenomenon and the core-shell structure of the core-shell structure microspheres are not obvious when the particle size is large, so it is impossible to obtain more than 50μm ultra-large expandable microspheres

Method used

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  • Hollow expandable microsphere with super-large particle size and preparation method thereof
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  • Hollow expandable microsphere with super-large particle size and preparation method thereof

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preparation example Construction

[0028] The embodiment of the present application provides a method for preparing hollow expandable microspheres with super large particle size, including the following steps:

[0029] Step 1, the parts by weight are 0-100 parts of air-tight monomer, 10-100 parts of acrylate monomer, 0-50 parts of amide monomer, 0-10 parts of initiator, 0-10 parts of cross-linking Agent, 20-60 parts of core materials are mixed, stirred in a 0-15Mpa oil phase tank, and prepared into an oil phase. Mix air-tight monomers, acrylate monomers, functional monomers, initiators, crosslinking agents, and core materials to prepare an oil phase, and then stir in the oil phase tank. The oil phase tank can be adjusted according to the core material Depending on the difference, the pressure is set, and the pressure can be selected from 0-15Mpa, preferably 0-10Mpa, more preferably 5-8Mpa.

[0030] Step 2: Add deionized water, silica sol, N,N-dimethylamide, surfactant, 1M sodium hydroxide solution, and 0.5M di...

Embodiment 1

[0050] Mix 700g of acrylonitrile, 100g of N-acryloylmorpholine, 200g of methacrylonitrile with 10g of azobisisobutyronitrile, 1g of triallyl isocyanurate, and 300g of pentane, and stir in a 5Mpa oil phase tank. Formulated into an oil phase;

[0051] Stir the oil phase and 5000gSW water phase in proportion to fully, and transfer the oil-water phase to the homogenization kettle for homogenization. The homogenization time is 0.5h, and the homogenization speed can be selected as 500rpm. , heated up to 40-80° C., and after 24 hours of reaction, suction-filtered and dried to obtain hollow expandable microsphere powder with an ultra-large particle size above 50 um.

Embodiment 2

[0056] 500g of vinylidene chloride, 300g of acrylonitrile, 60g of N-acryloylmorpholine, 200g of methacrylonitrile and 10g of bis(2-ethylhexyl) peroxydicarbonate, 1g of trimethylolpropane trimethacrylic acid Mix esters and 400g isobutane, stir in a 10Mpa oil phase tank, and prepare an oil phase;

[0057] Stir the oil phase and 5000gSW water phase in proportion to fully, and transfer the oil-water phase to the homogenization tank for homogenization. The homogenization time is 1h, and the homogenization speed can be selected as 5000rpm. After the homogenization is completed, according to the half-life of the initiator, The temperature is raised to 60° C., and after 24 hours of reaction, suction filtration is dried to obtain a hollow expandable microsphere powder with a super large particle size above 50 um.

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Abstract

The invention providesa hollow expandable microsphere with super-large particle size and a preparation method thereof, and belongs to the field of polymer functional materials.The method specifically comprises the steps that airtight monomers, acrylate monomers, 0-50 parts of amide monomers, an initiator, a cross-linking agent and a core material are mixed and stirred in an oil phase kettle, and an oil phase is prepared; deionized water, silica sol, N, N-dimethylformamide, a surfactant, a 1M sodium hydroxide solution and a 0.5 M disodium hydrogen phosphate solution are sequentially added into a water phase kettle to be prepared into a water phase; the oil phase and the water phase are fully stirred in proportion, the oil phase and the water phase are transferred into a homogenization kettle to be homogenized, the homogenization time is 0.5-1 h, the homogenization rotating speed can be 500-10000 rpm, after homogenization is finished, the temperature is increased to 40-80 DEG C, after a reaction is conducted for 24 h, suction filtration and drying are conducted, and hollow expandable microsphere powder with the super-large particle size being 50 micrometers or above is obtained. By means of the treatment scheme, the hollow expandable microsphere powder which is uniform in particle size, free of foaming and large in particle size of 50 micrometers or above is prepared.

Description

technical field [0001] The invention relates to the field of polymer functional materials, in particular to a hollow expandable microsphere with super large particle size and a preparation method thereof. Background technique [0002] Hollow expandable microspheres are polymer plastic microspheres with a core-shell structure composed of airtight thermoplastic polymer shells and hydrocarbons (C4-C12 alkanes) as the core. At room temperature, hydrocarbons are confined by the polymer shell and exist in the core in a two-phase coexistence state. When the microsphere is heated, the hydrocarbon vaporizes and the pressure inside the microsphere increases. At the same time, when the polymer shell reaches its glass At the transition temperature (Tg), the shell becomes soft and malleable. After the microspheres are foamed, the thermoplastic shell changes from thick to thin, the volume increases by more than 80 times, the density decreases significantly, most of the hydrocarbons escap...

Claims

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Application Information

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IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 成晓军刘利利
Owner NANOSPHERE SHANGHAI