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Preparation method of polyamide microsphere

A polyamide and microsphere technology, which is applied in the preparation of microspheres, microcapsule preparations, processing and manufacturing, etc., can solve the problems of irregular polyamide powder morphology, narrow particle size distribution, and large bulk density, and achieve flow performance. The effect of good powder flowability and high bulk density

Pending Publication Date: 2020-05-19
POLYROCKS TECH&RES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the problems of irregular appearance and low bulk density of polyamide powder produced in the existing solvent precipitation method, so that polyamide powder can better meet the use of SLS technology, the purpose of the present invention is to provide a kind of polyamide powder with a narrow particle size distribution 1. Preparation method of polyamide microspheres with high bulk density

Method used

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  • Preparation method of polyamide microsphere
  • Preparation method of polyamide microsphere

Examples

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Effect test

Embodiment 1

[0045]Put 600g of nylon 1012 pellets, 3750mL of ethanol, 200g of water, and 6g of PVP-K30 into the autoclave, replace it with high-purity nitrogen for 20 minutes, pressurize to 1MPa, then heat up to 145°C while stirring and keep the temperature for 90 minutes to dissolve the material . Then lower the temperature, the cooling rate in the first stage is 0.5°C / min to 123°C; the cooling rate in the second stage is 0.1°C / min to 108°C, and then rapidly to 45°C at a cooling rate of 1°C / min. Nylon powder is obtained after post-processing such as filtration and drying.

[0046] attached figure 1 It is the scanning electron micrograph of the nylon microspheres made in this example. From figure 1 It can be seen that the appearance of the nylon powder prepared in this example is approximately spherical. After testing, the particle size distribution of the nylon powder is: D10: 31.98 μm, D50: 58.69 μm, D90: 81.03 μm. The bulk density of nylon powder is 435g / L, and the angle of repose ...

Embodiment 2

[0048] Put 600g of nylon 1012 pellets, 3750mL of ethanol, 200g of water, and 12g of PVP-K60 into the autoclave, replace it with high-purity nitrogen for 20 minutes, pressurize to 1MPa, then heat up to 145°C while stirring and keep the temperature for 90 minutes to dissolve the material . Then lower the temperature, the cooling rate in the first stage is 0.5°C / min to 123°C; the cooling rate in the second stage is 0.1°C / min to 108°C, and then rapidly to 45°C at a cooling rate of 1°C / min. After post-processing such as filtration and drying, nylon powder is obtained, and the powder shape is approximately spherical.

[0049] After testing, the particle size distribution of the nylon powder is: D10: 36.74 μm, D50: 57.40 μm, D90: 83.32 μm. The bulk density of nylon powder is 460g / L, and the angle of repose is 27°.

Embodiment 3

[0051] Put 600g of nylon 12 pellets, 6000mL of ethanol, 200g of water, and 12g of PVP-K15 into the autoclave, replace it with high-purity nitrogen for 20 minutes, pressurize to 1MPa, then heat up to 145°C while stirring and keep the temperature for 90 minutes to dissolve the material . Then lower the temperature, the cooling rate in the first stage is 0.5°C / min to 125°C; the cooling rate in the second stage is 0.1°C / min to 110°C, and then quickly to 40°C at a cooling rate of 1°C / min. After post-processing such as filtration and drying, nylon powder is obtained, and the powder shape is approximately spherical.

[0052] After testing, the particle size distribution of the nylon powder is: D10: 26.91 μm, D50: 53.74 μm, D90: 81.80 μm. The bulk density of nylon powder is 421g / L, and the angle of repose is 30°.

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Abstract

The invention discloses a preparation method of a polyamide microsphere. The preparation method of the polyamide microsphere comprises the following steps: 1) adding polyamide, polyvinylpyrrolidone and a solvent into a reaction kettle, and carrying out heating for dissolving; 2) carrying out cooling to a first-stage temperature at a cooling rate of 0.4-1 DEG C / min, then carrying out cooling to a second-stage temperature at a cooling rate of 0.05-0.3 DEG C / min, and then conducting cooling to 45 DEG C or below to obtain a precipitate which is the polyamide microsphere, wherein in the step (1), the heating and dissolving temperature is 135-160 DEG C, in the step (2), the first-stage temperature is 5-15 DEG C higher than the second-stage temperature, and the second-stage temperature is a precipitation temperature. The polyamide microsphere prepared by the method has the characteristics of narrow particle size distribution, high apparent density and good flowing property, and is particularly suitable for a selective laser sintering technology.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of polyamide microspheres. Background technique [0002] Selective laser sintering technology, namely SLS (Selective Laser Sintering) technology, is a typical 3D printing technology. This technology uses the idea of ​​layered manufacturing, uses the principle of discrete-stacking, uses laser as the heat source, and is supplemented by computer control to directly process solid powder raw materials Sintering into solid parts has the advantages of efficient use of materials and high manufacturing efficiency. After years of rapid development, SLS technology has been widely used in various fields such as automobiles, household appliances, aerospace, medical biology, etc. It is one of the more mature 3D printing technologies at present. [0003] As a typical thermoplastic semi-crystalline polymer material, polyamide powder has excellent mechanical proper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/14C08L77/06C08L35/06B29C64/153B01J13/06B33Y10/00
CPCC08J3/14B29C64/153B01J13/06B33Y10/00C08J2377/06C08J2435/06
Inventor 雷伟健梁亚涛朱红芳李桂林余如媛戚良明刘华夏
Owner POLYROCKS TECH&RES CO LTD