Nylon/silica composite microsphere, preparation method and application thereof

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

Active Publication Date: 2017-10-17
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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  • Nylon/silica composite microsphere, preparation method and application thereof
  • Nylon/silica composite microsphere, preparation method and application thereof
  • Nylon/silica composite microsphere, preparation method and application thereof

Examples

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preparation example Construction

[0044] The preparation method of porous nylon 6 microspheres is:

[0045] Preparation of porous nylon 6 microspheres by the dissolution-precipitation method: add 40g nylon 6 pellets and 240ml formic acid to the reactor and heat up to 80°C, stir for 2h to fully dissolve the material, and then add 400ml of 10% g / ml polyethylene The ethanol solution of pyrrolidone (PVP-K30) was stirred vigorously and then stood still to precipitate a powder. Suction filtration, ethanol washing, and vacuum drying to obtain polyamide porous microspheres; the SEM picture of the obtained pore-containing nylon 6 microspheres is as follows figure 1 Shown; the obtained nylon 6 microspheres have an average particle size of 60μm and a specific surface area of ​​23m 2 / g, the porosity is 77%, the pore size is 0.1-2μm, and the bulk density is 0.2g / mL.

[0046] The preparation method of porous nylon 12 microspheres is:

[0047] Preparation of porous nylon 12 microspheres by the dissolution-precipitation method: ad...

Embodiment 1

[0050] Take 0.5 g of porous nylon 6 microspheres, 3 mL of 25% ammonia water, and 10 mL of deionized water into a 150 mL three-necked flask, and ultrasonicate for 0.5 h to obtain a dispersion of porous nylon microspheres; add 3 mL of ethyl orthosilicate Dissolved in 30mL ethanol and added to the above dispersion at a dropping rate of 5mL / h, and reacted with rapid stirring at 30°C for 10h; the solution obtained after the reaction was filtered, washed, and dried to obtain nylon / silica composite microspheres with good dispersibility.

[0051] The scanning electron microscope picture of the obtained composite microspheres is as follows image 3 As shown; the particle size of the composite microspheres is 40-60μm, and only a small part of the micropores exist on the surface. The particle size of the nano-silica in the composite microspheres is 200-300nm, and it is uniformly dispersed in the porous nylon 6 microspheres . The specific surface area of ​​the composite microspheres is 11m 2...

Embodiment 2

[0053] Take 0.5 g of porous nylon 12 microspheres, 1 mL of 25% ammonia water, and 5 mL of ethanol into a 150 mL three-necked flask, and ultrasound for 0.5 h to obtain a dispersion of porous nylon microspheres; dissolve 1 mL of ethyl orthosilicate 10 mL of ethanol was added to the above dispersion at a dropping rate of 5 mL / h, and reacted with rapid stirring at 30°C for 10 hours; the solution obtained after the reaction was filtered, washed, and dried to obtain nylon 12 / silica composite microspheres with good dispersibility.

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

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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 / silica composite microsphere and its preparation method and application. Background technique [0002] Nylon is a crystalline polymer made from amino acids or corresponding lactams. As one of the five major engineering plastics, it is widely used in automobiles and machinery due to its high melting temperature and glass transition temperature, good mechanical properties, wear resistance, impact toughness, and excellent self-lubricity and easy formability. , Aerospace, military, medical, electronics and other fields. However, many nylon products are easily brittle at low temperature, high water absorption, poor dimensional stability and other shortcomings, which greatly limit their application. The industry often uses inorganic powder to modify nylon materials to improve the above-mentioned unfavorable factors. The preparation and performance resea...

Claims

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Application Information

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Patent Type & Authority Applications(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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