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Preparation method for millimeter-grade polyacrylonitrile hollow microsphere

A technology of polyacrylonitrile and hollow microspheres, which is applied in the field of functional ceramics and can solve problems such as difficult preparation of polyacrylonitrile hollow microspheres, thinning of the composite fluid layer, and reduction of droplet size.

Active Publication Date: 2019-12-03
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Most of the existing microchannel structures are double T channels, coaxial convection channels, etc., which also contain O 1 , W, O 2 The structure of the three-phase fluid, with the help of O 2 Flow is applied at O 1 The vortex generated by the combined effects of shear force and viscous force on the / W composite fluid realizes the fracture of the composite fluid and the generation of droplets, which can automatically disperse the double droplets in O 2 However, the application of shear force leads to the thinning of the composite fluid layer and the reduction of droplet size, so it is difficult to prepare polyacrylonitrile hollow microspheres with diameters of millimeters

Method used

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  • Preparation method for millimeter-grade polyacrylonitrile hollow microsphere
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  • Preparation method for millimeter-grade polyacrylonitrile hollow microsphere

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preparation example Construction

[0040] The present invention provides a method for preparing millimeter-level polyacrylonitrile hollow microspheres, which includes the following steps:

[0041] S1: Use silicone oil with a viscosity of 450~550mPa.s as the first oil phase O 1 And the second oil phase O 2 ; Take the polyacrylonitrile solution as the water phase W; the first oil phase O 1 And the water phase W are respectively injected into the first syringe and the second syringe;

[0042] On the one hand, the use of high-viscosity silicone oil can meet the viscosity density matching between the phases. On the other hand, the high viscosity of the silicone oil is conducive to the better dispersion of the double droplets during the rotary steaming process and the adjustment of the sphericity. First oil phase O 1 Used to form O with water phase W 1 / W double drop, second oil phase O 2 Used as O during rotary evaporation 1 / W Double drop carrier.

[0043] The first syringe and the second syringe are syringes with a micro...

Embodiment 1

[0086] This embodiment provides a method for preparing millimeter-level polyacrylonitrile hollow microspheres, which includes the following steps:

[0087] S1: With a density of 0.9738g / cm 3 (25℃) Dimethicone with a viscosity of 500mPa.s is the first oil phase O 1 And the second oil phase O 2 ; Take the polyacrylonitrile solution with a molecular weight of 15w as the water phase W (the solvent is DMF, the mass fraction of polyacrylonitrile is 10wt%); the first oil phase O 1 And the water phase W are respectively injected into the first syringe and the second syringe;

[0088] S2: After removing the gas in the microchannel, set the advance rate of the first syringe and the second syringe to 4mL / h and 12mL / h, respectively, and advance the syringes in the order of the second syringe first and then the first syringe, until it can form a uniform Stable O 1 / W double drop, the O 1 / W Double droplets drop into the second oil phase O 2 Collect in a 550mL collection bottle;

[0089] S3: Let ...

Embodiment 2

[0097] This example provides a method for preparing millimeter-level polyacrylonitrile hollow microspheres. Compared with Example 1, the advancing rate of the first syringe in step S2 is changed from 4 mL / h to 6 mL / h, and the other steps are the same as in Example 1. .

[0098] The millimeter-level polyacrylonitrile hollow microspheres prepared in this example were characterized, measured and calculated. The average diameter, sphericity, concentricity, average wall thickness and uniformity of the wall thickness are shown in Table 3, which can be seen from the table. Because the internal phase silicone oil (the first oil phase O 1 ) As the flow rate increases, the diameter of the hollow microspheres increases to 1.8mm; however, the resulting O 1 / W The amount of PAN phase (PAN is polyacrylonitrile, PAN phase is water phase W) in the double droplet is reduced, and the wall thickness is reduced to 60μm, but still meets the ICF size index (International Functional Classification), and...

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Abstract

The invention discloses a preparation method for a millimeter-grade polyacrylonitrile hollow microsphere. The method includes the following steps: firstly selecting high viscosity silicone oil as a first oil phase O1 and a second oil phase O2, and a polyacrylonitrile dissolved solution as a water phase W; forming a uniform and stable O1 / W dual-composition liquid drop by controlling the ejection velocities of a first injector and a second injector, and dropping the liquid drop in a collection bottle containing the second oil phase O2; standing the collection bottle subsequently, and realizing microsphere solidification by rotary evaporation; subsequently soaking the solidified microsphere in low viscosity silicone oil; then replacing the low viscosity silicone oil inside the microsphere through Soxhlet extraction; and finally removing an extraction solvent inside the microsphere through drying to obtain the millimeter-grade polyacrylonitrile hollow microsphere. The hollow microsphere prepared by the preparation method of the invention has a diameter of 1.5-2mm and a wall thickness of 60-130 [mu]m. In addition, the spherical degree, the concentric degree, the wall thickness uniformity, and other properties of the hollow microsphere are better.

Description

Technical field [0001] The invention relates to the technical field of functional ceramics, in particular to a method for preparing millimeter-level polyacrylonitrile hollow microspheres. Background technique [0002] Nuclear fusion generally releases energy from the polymerization of hydrogen isotopes deuterium and tritium into helium, which has more energy reserves and is safe and clean. The energy released by the complete fusion reaction of deuterium extracted from one liter of seawater is equivalent to the energy released by the combustion of 300 liters of gasoline. If controllable nuclear fusion is achieved, it is expected to solve the energy problem facing mankind. [0003] As one of the effective ways to achieve controlled nuclear fusion, inertial restraint has achieved good experimental results on the "National Ignition Device" of the United States and the Shenguang II device of my country. In this research, the design and preparation of the target pellet as a deuterium-tr...

Claims

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Application Information

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IPC IPC(8): B01J13/12
CPCB01J13/125
Inventor 邵长伟许晓颖程军
Owner NAT UNIV OF DEFENSE TECH
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