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A kind of nylon/silicon dioxide composite microsphere, preparation method and application

A technology of silica and composite microspheres, used in chemical instruments and methods, pharmaceutical formulations, other chemical processes, etc., to achieve the effect of low porosity, increased bulk density, and good fluidity

Active Publication Date: 2019-11-22
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The second object of the present invention is to provide a preparation method of nylon / silicon dioxide composite microspheres, which uses a sol-gel method to polymerize silica in situ in a porous nylon skeleton. The preparation method is simple and easy to control , which not only solves the problem of uniform dispersion of a large amount of silica in the porous nylon microsphere matrix, but also solves the problem of nylon material water absorption through the introduction of hydrophobic silica and the improvement of the crystallinity of the nylon skeleton structure; at the same time, it can effectively improve the nylon composite Bulk density, thermal stability, crystallization properties and mechanical strength of powder

Method used

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  • A kind of nylon/silicon dioxide composite microsphere, preparation method and application
  • A kind of nylon/silicon dioxide composite microsphere, preparation method and application
  • A kind of nylon/silicon dioxide composite microsphere, preparation method and application

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preparation example Construction

[0044] The preparation method of hole-containing nylon 6 microspheres is:

[0045] Preparation of pore-containing nylon 6 microspheres by dissolution-precipitation method: add 40g of nylon 6 pellets and 240ml of formic acid into the reaction kettle and heat up to 80°C, stir for 2 hours to fully dissolve the material, and then add 400ml of polyethylene with a concentration of 10% g / ml Pyrrolidone (PVP-K30) ethanol solution, stirred vigorously and left to stand, precipitated powder. Suction filtration, ethanol washing, and vacuum drying obtain polyamide porous microspheres; the scanning electron microscope pictures of the nylon 6 microspheres containing pores are as follows: figure 1 Shown; The average particle size of the resulting nylon 6 microspheres is 60 μm, and the specific surface area is 23m 2 / g, the porosity is 77%, the pore diameter is 0.1-2μm, and the bulk density is 0.2g / mL.

[0046] The preparation method of pore-containing nylon 12 microspheres is:

[0047] Pre...

Embodiment 1

[0050] Take 0.5g of pore-containing nylon 6 microspheres, 3mL of 25% ammonia water, and 10mL of deionized water and add them together into a 150mL three-necked flask, and ultrasonically 0.5h to obtain a pore-containing nylon microsphere dispersion; Dissolve in 30mL of ethanol and add to the above dispersion liquid at a dropping rate of 5mL / h, stir rapidly at 30°C for 10h; filter, wash and dry the solution obtained after the reaction to obtain nylon / silica composite microspheres with good dispersibility.

[0051] The scanning electron microscope pictures of the resulting composite microspheres are as follows: image 3 As shown; the particle size of the composite microspheres is 40-60 μm, and only a small number of micropores exist on the surface. The particle size of nano-silica in the composite microspheres is 200-300 nm, and they are uniformly dispersed in the porous nylon 6 microspheres. . The specific surface area of ​​the composite microsphere is 11m 2 / g, porosity 30%. ...

Embodiment 2

[0053] Take 0.5g of pore-containing nylon 12 microspheres, 1mL of 25% ammonia water, and 5mL of ethanol and add them together into a 150mL three-neck flask, and ultrasonicate for 0.5h to obtain a pore-containing nylon microsphere dispersion; dissolve 1mL of ethyl orthosilicate in 10mL of ethanol was added to the above dispersion at a rate of 5mL / h, and stirred rapidly at 30°C for 10h; the solution obtained after the reaction was filtered, washed, and dried to obtain nylon 12 / silicon dioxide composite microspheres with good dispersibility.

[0054] The scanning electron microscope pictures of the resulting composite microspheres are as follows: Figure 4 As shown; the particle size of the composite microsphere is 60 μm, and there are only a few micropores on the surface. The particle size of nano-silica in the composite microsphere is 200-300 nm, and it is uniformly dispersed in the porous nylon 12 microsphere. Composite microsphere specific surface area is 5m 2 / g, porosity 2...

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Abstract

The invention discloses a nylon / silica composite microsphere, a preparation method and an application thereof. The composite microsphere is spherical and / or near spherical particles with the particle size of 0.5-300 [mu]m, and is formed by an aperture-containing nylon microsphere matrix and silica uniformly dispersed in the aperture-containing nylon microsphere aperture and / or surface. The content of the aperture-containing nylon microsphere is 10-99.9 wt%, and the content of the silica is 0.1-90 wt%. The composite microsphere is obtained by performing silica in-situ hydrolysation in aperture-containing nylon microsphere dispersion liquid. Addition of silica can effectively reduce the water absorption of the aperture-containing nylon microsphere, and increases the heat stability, crystallization property and mechanical intensity; the composite microsphere can be taken as consumable in a SLS selective laser sintering technology, and widens the application of the SLS technology in the fields of aviation, automobile, medical apparatus, electronic apparatus, machinery die and artwork.

Description

technical field [0001] The invention relates to the technical field of polymer materials. More specifically, it relates to a nylon / silicon dioxide composite microsphere and its preparation method and application. Background technique [0002] Nylon is a crystalline polymer made from amino acids or the corresponding lactams. As one of the five major engineering plastics, it is widely used in automobiles and machinery because of its high melting temperature and glass transition temperature, good mechanical properties, wear resistance, impact toughness, and excellent self-lubrication and easy formability. , aerospace, military, medical, electronics and other fields. However, many nylon products are easily brittle at low temperature, have high water absorption, and poor dimensional stability, which greatly limits their application. In the industry, inorganic powders are often used to modify nylon materials to improve the above unfavorable factors. The preparation and propert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L77/02C08L77/06C08K3/36C08J3/14B33Y70/00C09D5/46C09D5/03B01J20/286A61K47/69A61K9/16A61K47/04A61K47/34
CPCA61K9/1611A61K9/1641B01J20/286B33Y70/00C08J3/14C08K3/36C08K2201/003C08K2201/011C08L2201/08C09D5/03C08L77/02
Inventor 王格侠刘平季君晖孙潇潇甄志超王萍丽
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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