A preparing method of a monodisperse phenolic resin carbon microbead

A technology of phenolic resin and phenolic resin liquid is applied in the field of preparation of monodisperse phenolic resin carbon microspheres, which can solve the problems of difficulty in precise control of product particle size, high drying temperature and curing temperature, poor sphericity of microspheres, etc. The use of chemical reagents, the reduction of production costs, and the effect of easy adjustment of size

Active Publication Date: 2015-08-12
ENERGY RES INST OF SHANDONG ACAD OF SCI
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Problems solved by technology

The drying temperature and curing temperature obtained by this method are high, the sphericity of the microspheres is not good, the particle size is uncontrollable, and the particle size distribution is not uniform.
[0006] It can be seen that the existing technology still has shortcomings

Method used

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  • A preparing method of a monodisperse phenolic resin carbon microbead
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  • A preparing method of a monodisperse phenolic resin carbon microbead

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preparation example Construction

[0046] The preparation method of monodisperse phenolic resin carbon microsphere provided by the invention can comprise the following steps:

[0047] (1) the water-soluble phenolic resin that the viscosity is 5-1000mp s, solid content is 30-60% is used as dispersed phase solution; Surfactant is mixed with difficult volatile oil, is mixed with surfactant mass percentage concentration is 1%-10% organic solution is used as the continuous phase solution; the dispersed phase solution and the continuous phase solution are respectively loaded into syringes, the syringes are respectively placed on micro-injection pumps, and the syringes are connected to microchannels for reaction device, and then respectively inject the dispersed phase solution and the continuous phase solution into the microchannel reactor through the micro-injection pump, so that the dispersed phase solution and the continuous phase solution flow into the microchannel reactor, and the dispersed phase solution and the ...

Embodiment 1

[0053] Weigh 2.0g EM90 and add it into a beaker containing 100mL mineral oil, stir slowly with a magnet, and filter to obtain a continuous phase solution; commercially available water-soluble phenolic resin with a viscosity of 60mp s and a solid content of 47% is filtered, A dispersed phase solution is obtained. The two solutions were respectively loaded into 20mL syringes, placed on a micro-injection pump, and connected to a microchannel reactor. The flow direction of the phase solution is reversed (such as Figure 1b shown), and set the flow rate of the dispersed phase solution to be 0.5mL / h, and the flow rate of the continuous phase solution to be 5mL / h, so that the two phases meet at the nozzle of the collection tube in the microchannel reactor, and continuously generate uniform phenolic resin liquid drop. Use a collector equipped with liquid paraffin to collect the generated droplets, put them in an oven for temperature-programmed solidification, keep at 70°C for 1.5h, ...

Embodiment 2

[0055] The paraffin wax solution containing EM90 with a mass percent concentration of 2% is used as the continuous phase solution, and the water-soluble phenolic resin with a viscosity of 15mp·s and a solid content of 47% is used as the dispersed phase solution. The inlet diameter of the microchannel reactor used is 160 μm, and the outlet diameter is 200 μm. Reverse the flow direction of the dispersed phase solution and the continuous phase solution (such as Figure 1b shown). The flow rate of the dispersed phase solution was controlled to be 0.5 mL / h, and the flow rate of the continuous phase solution was 3 mL / h. Other steps and parameters are the same as in Example 1. The phenolic resin droplets with a particle diameter of about 180 μm were obtained. The particle size of the obtained monodisperse phenolic resin microspheres is 115 μm, the particle size deviation CV<3%, and the particle size is uniform.

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Abstract

A preparing method of a monodisperse phenolic resin carbon microbead is provided. The method includes following steps of: forming water-in-oil phenolic resin liquid drops in a micro-channel reactor by a microfluidic liquid drop technique; preparing the phenolic resin liquid drops into phenolic resin microbeads by thermocuring; washing and separating the phenolic resin microbeads to obtain a monodisperse phenolic resin microbead; and subjecting the monodisperse phenolic resin microbead to high-temperature carbonization in an inert atmosphere to form the monodisperse phenolic resin carbon microbead. The method overcomes the defects in the prior art, namely complex processes, difficulty in accurate control of product particle sizes, irregular morphology, and the like, and has advantages of simple and rapid preparation process, controllable microbead particle size, uniform particle size, good degrees of sphericity, and the like.

Description

technical field [0001] The invention relates to a preparation method of monodisperse phenolic resin carbon microspheres, in particular to a controllable and rapid preparation method of monodisperse phenolic resin carbon microspheres by using microfluidic droplet technology, and belongs to the technical field of carbon microspheres. Background technique [0002] Carbon microspheres not only have high thermal stability, chemical stability, modifiability, and biocompatibility, but also have some characteristics superior to granular carbon, such as good fluidity, high packing density, and high mechanical strength. Therefore, carbon microspheres are widely used in the fields of electrode materials, adsorbents, catalyst supports, and drug carriers. [0003] The use of phenolic resin oligomers to prepare thermosetting microspheres has the characteristics of low impurity content, controllable structure, and abundant raw materials. The preparation of carbon microspheres using it as a...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 王立秋王建梅李艳许敏孔湉湉
Owner ENERGY RES INST OF SHANDONG ACAD OF SCI
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