Polymer-based micro/nano functional composite spherical powder and preparation method thereof

Abstract

The invention belongs to the field of macromolecules, and particularly relates to polymer-based micron / nano functional composite spherical powder and a preparing method thereof. According to the method, polymer-based micron / nano functional composite ultrafine powder compact in combination and uniform in scattering is obtained through solid-phase shearing grinding, and the powder grain size rangesfrom 30 microns to 200 microns; the above functional composite powder is evenly scattered in a scattering agent to be heated to the temperature above the heating deformation temperature of the functional composite powder for spheroidization treatment; and then heated suspension liquid is cooled, filtered, washed, dried and screened, and the functional composite spherical powder is obtained. The method is simple in operation, economical and environment-friendly, and large-scale preparing of the polymer-based micron / nano functional composite spherical powder can be achieved. The beneficial effects that the degree of sphericity is high, size distribution is narrow, the inner structure is uniform, and mobility and stacking density are high are achieved. The functional composite powder preparedthrough the method can meet the selective laser sintering requirement and can also be applied to the fields of the biomedical engineering, super capacitors, coatings, cosmetics and the like.

Description

technical field

[0001] The invention belongs to the field of macromolecules, and in particular relates to a polymer-based micro / nano functional composite spherical powder and a preparation method thereof. Background technique

[0002] 3D printing is an advanced manufacturing technology based on materials, machinery, control, computer software, etc., which embodies the characteristics of green manufacturing, intelligent manufacturing and social manufacturing. At present, products prepared by 3D printing are widely used in high-tech fields such as major national defense equipment, aerospace, biomedicine, industrial design, communication electronics, and automobiles. Developed countries in Europe and the United States attach great importance to this, believing that this technology "will promote the realization of the third industrial revolution", and was listed as "the ten fastest-growing industries in the United States" by the American "Time Magazine". In view of this, countr...

Examples

preparation example Construction

[0042] The preparation method of polymer-based micro / nano functional composite spherical powder comprises the following steps:

[0043] A. The first milling: Use a disc-type mechanochemical reactor to mix and mill the polymer pellets and inorganic functional particles to refine and mix the raw materials uniformly to obtain primary composite powders;

[0044] B. Melt extrusion: The primary composite powder is melt-extruded and pelletized to obtain composite particles; this step makes the polymer and inorganic functional particles bond together; but the particle size of the composite particles obtained in this step is millimeter-level, which cannot meet the requirements Use requirements, so it needs to be further pulverized and then spheroidized;

[0045] C. Second milling: Grinding the composite particles with a disc-type mechanochemical reactor to obtain a secondary composite powder with a suitable particle size, so as to finally obtain a micron or nanometer product with a sui...

Embodiment 1

[0058] Example 1: PA11 / BaTiO 3 Preparation of Piezoelectric Nanocomposite Spherical Powder

[0059] 800 g of nylon 11 (PA11) with a particle size of 2 to 5 mm and BaTiO with an average particle size of 500 nm 3 Piezoelectric nanopowder particles 200g and antioxidant 1,3,5-trimethyl-2,4,6(3,5-di-tert-butyl-4-hydroxybenzyl)benzene 9g and 2,2- Add 1 g of ethyl bis(4,6-di-tert-butylphenyl) fluorophosphite into the opened disc-type mechanochemical reactor through the feed port for mixing and grinding, and control the cooling cycle water temperature during the grinding process to 25°C, milling pressure 25MPa, milling speed 500rpm, after 10 times of milling, the first PA11 / BaTiO mixed evenly was obtained 3 Piezoelectric nanocomposite powder;

[0060] The PA11 / BaTiO obtained by grinding 3 The piezoelectric nanocomposite powder is melt-extruded in a twin-screw extruder, the extrusion temperature is controlled at 190-210°C and the extrusion speed is 80rpm, and then pelletized to obt...

Embodiment 2

[0067] Example 2: Preparation of polyvinylidene fluoride / hydroxyapatite nanocomposite spherical powder for biological tissue scaffolds

[0068]600g of polyvinylidene fluoride (PVDF) with a particle size of 2-5mm, 400g of hydroxyapatite nanopowder particles with an average particle size of 60nm, and N,N'-bis(3,5-di-tert-butyl-4 -Hydroxyphenylpropanamide) 8g and tetrakis(2,4-di-tert-butylphenyl) 2g are added into the opened disc type mechanochemical reactor through the feeding port for mixed grinding, and the cooling cycle is controlled during the grinding process The water temperature is 24°C, the grinding pressure is 20MPa, and the grinding speed is 800rpm. After 8 times of grinding, a uniformly mixed polyvinylidene fluoride / hydroxyapatite nanocomposite powder is obtained;

[0069] The polyvinylidene fluoride / hydroxyapatite nanocomposite powder obtained by grinding is melt-extruded in a twin-screw extruder, the extrusion temperature is controlled at 190-200°C and the extrusion...

technical field

[0001] The invention belongs to the field of macromolecules, and in particular relates to a polymer-based micro / nano functional composite spherical powder and a preparation method thereof. Background technique

[0002] 3D printing is an advanced manufacturing technology based on materials, machinery, control, computer software, etc., which embodies the characteristics of green manufacturing, intelligent manufacturing and social manufacturing. At present, products prepared by 3D printing are widely used in high-tech fields such as major national defense equipment, aerospace, biomedicine, industrial design, communication electronics, and automobiles. Developed countries in Europe and the United States attach great importance to this, believing that this technology "will promote the realization of the third industrial revolution", and was listed as "the ten fastest-growing industries in the United States" by the American "Time Magazine". In view of this, countr...

Examples

preparation example Construction

[0042] The preparation method of polymer-based micro / nano functional composite spherical powder comprises the following steps:

[0043] A. The first milling: Use a disc-type mechanochemical reactor to mix and mill the polymer pellets and inorganic functional particles to refine and mix the raw materials uniformly to obtain primary composite powders;

[0044] B. Melt extrusion: The primary composite powder is melt-extruded and pelletized to obtain composite particles; this step makes the polymer and inorganic functional particles bond together; but the particle size of the composite particles obtained in this step is millimeter-level, which cannot meet the requirements Use requirements, so it needs to be further pulverized and then spheroidized;

[0045] C. Second milling: Grinding the composite particles with a disc-type mechanochemical reactor to obtain a secondary composite powder with a suitable particle size, so as to finally obtain a micron or nanometer product with a sui...

Embodiment 1

[0058] Example 1: PA11 / BaTiO 3 Preparation of Piezoelectric Nanocomposite Spherical Powder

[0059] 800 g of nylon 11 (PA11) with a particle size of 2 to 5 mm and BaTiO with an average particle size of 500 nm 3 Piezoelectric nanopowder particles 200g and antioxidant 1,3,5-trimethyl-2,4,6(3,5-di-tert-butyl-4-hydroxybenzyl)benzene 9g and 2,2- Add 1 g of ethyl bis(4,6-di-tert-butylphenyl) fluorophosphite into the opened disc-type mechanochemical reactor through the feed port for mixing and grinding, and control the cooling cycle water temperature during the grinding process to 25°C, milling pressure 25MPa, milling speed 500rpm, after 10 times of milling, the first PA11 / BaTiO mixed evenly was obtained 3 Piezoelectric nanocomposite powder;

[0060] The PA11 / BaTiO obtained by grinding 3 The piezoelectric nanocomposite powder is melt-extruded in a twin-screw extruder, the extrusion temperature is controlled at 190-210°C and the extrusion speed is 80rpm, and then pelletized to obt...

Embodiment 2

[0067] Example 2: Preparation of polyvinylidene fluoride / hydroxyapatite nanocomposite spherical powder for biological tissue scaffolds

[0068]600g of polyvinylidene fluoride (PVDF) with a particle size of 2-5mm, 400g of hydroxyapatite nanopowder particles with an average particle size of 60nm, and N,N'-bis(3,5-di-tert-butyl-4 -Hydroxyphenylpropanamide) 8g and tetrakis(2,4-di-tert-butylphenyl) 2g are added into the opened disc type mechanochemical reactor through the feeding port for mixed grinding, and the cooling cycle is controlled during the grinding process The water temperature is 24°C, the grinding pressure is 20MPa, and the grinding speed is 800rpm. After 8 times of grinding, a uniformly mixed polyvinylidene fluoride / hydroxyapatite nanocomposite powder is obtained;

[0069] The polyvinylidene fluoride / hydroxyapatite nanocomposite powder obtained by grinding is melt-extruded in a twin-screw extruder, the extrusion temperature is controlled at 190-200°C and the extrusion...

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