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

A nano-functional, spherical powder technology, applied in the polymer field, can solve the problems of inability to prepare high-filling composite powder, unsatisfactory particle size, uneven dispersion of inorganic particles, etc., achieving easy implementation, breaking through technical bottlenecks, The effect of short spheroidization time

Active Publication Date: 2020-05-05
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Chinese patent CN102311637 adopts SLS commercial nylon powder and inorganic particles to prepare nylon composite materials for SLS by simple mechanical blending. Although this method is simple to operate and low in preparation cost, there are inorganic particles dispersed unevenly inside the polymer, and the process of transportation and storage Problems such as "segregation" and low laser absorption efficiency appear; the solvent precipitation method dissolves the polymer in a good solvent under certain special conditions (such as high temperature, high pressure, and strong stirring), and then the solvent becomes Poor solvent, so that the polymer gradually precipitates to the surface of the inorganic particles to obtain a polymer composite powder. The advantages of this method are that the prepared powder particles are close to spherical, the powder particle size distribution is narrow, and the fluidity is good. However, the problems in the preparation process are The solvent is not universal, and different reagents or dissolving processes need to be selected for different polymers to dissolve the polymers. The preparation process may use toxic reagents, the process conditions are relatively complicated, and it is impossible to prepare highly filled composite powders (CN101148541A); Synthetic methods such as emulsion polymerization, dispersion polymerization, suspension polymerization, seed polymerization, membrane emulsification, and emulsion solvent evaporation (Wang Yaning, Wang Han, Liang Jie. Progress in the synthesis and application of polymer microspheres (1) [J]. Ion exchange and Adsorption, 2016,32(4):377-384.), although the prepared particles have higher sphericity and smoother surface, but the raw material loss rate is high, and the particle size cannot meet the requirements of SLS (Chen Liqing, Wu Bozhen, ZHU Zhengdong, et al. Preparation and Thermal Properties of PA6 / 12 Powder with Controllable Particle Size for 3D Printing[J]. New Chemical Materials, 2017,45(5):226-228.)
However, there are few technologies for the spheroidization of polymer powder at present, and there are few reports
Schmidt J et al. (Schmidt J, Sachs M, Blümel C, et al. A novel processroute for the production of spherical LBM polymer powders with small size and good flowability [J]. Powder Technology, 2014, 261:78-86; Schmidt J, Sachs M, Blümel C, et al. A novel process chain for the production of spherical SLS polymer powders with good flowability [J]. Procedia Engineering, 2015, 102: 550-556.) tried to wet-grind PS or PBT powder It is passed into a specially designed high-temperature pipeline fluidized bed for spheroidization, and the sphericity, fluidity and bulk density of the spheroidized PS or PBT powder particles have been greatly improved. However, this method requires Different lengths of pipes need to be designed for polymers with different melting points. In addition, polymers are easily adhered to the pipe wall in the molten state, causing blockage and low spheroidization yield. These problems largely limit the Application of the method

Method used

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

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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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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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B29B9/12C08L77/02C08L71/02C08K3/24C08K3/32C08L27/16C08K7/24C08L75/04C08K7/06C08L23/06C08K3/38C08L25/06
CPCB29B9/12B29B2009/125C08K3/32C08K3/38C08K7/06C08K7/24C08K2003/325C08K2003/385C08K2201/011C08L77/02C08L2207/062C08L71/02C08K3/24C08L27/16C08L75/04C08L23/06C08L25/06B29B9/06B29B9/16B29B2009/166
Inventor 王琪戚方伟陈宁
Owner SICHUAN UNIV
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