Room temperature droplet microreactor and method for preparing zirconia gel microspheres

A microreactor and gel microsphere technology, applied in chemical instruments and methods, zirconia, chemical/physical/physicochemical reactors, etc., can solve the problems of easy blockage of channel nozzles, uneven reaction, etc., and achieve uniformity Improved performance and good uniformity

Active Publication Date: 2018-04-10
UNIV OF SCI & TECH BEIJING +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the two liquid droplets are mixed in the form of point contact, which is easy to cause uneven reaction, and in the continuous preparation process, it is easy to block the channel orifice of the two reaction liquid phases.

Method used

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  • Room temperature droplet microreactor and method for preparing zirconia gel microspheres
  • Room temperature droplet microreactor and method for preparing zirconia gel microspheres
  • Room temperature droplet microreactor and method for preparing zirconia gel microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0100] Example 1: General method

[0101] Using a room temperature droplet microreactor device, the internal phase zirconia precursor sol and the external phase hexamethylenetetramine solution are mixed in the device, and then sheared by the continuous phase silicone oil. The fusion of zirconium sol and the coated form of hexamethylenetetramine solution triggers a gel reaction, and after washing, transparent gel microspheres are obtained. The transparent gel microspheres are sintered at high temperature to obtain zirconia ceramic microspheres. Concrete preparation method comprises the following steps:

[0102] 1) Prepare the microchannel device: use the glass slide as the substrate, insert the conical incident tube and the conical collecting tube from both ends of the square tube and arrange them coaxially, and assemble them in a nested manner. The thin cylindrical tube and the conical incident tube are in the same direction The conical incident tube is coaxially arranged an...

Embodiment 2

[0110] Embodiment 2: Utilize room temperature droplet microreactor to prepare zirconia gel beads

[0111] Prepare zirconium dioxide precursor sol, hexamethylenetetramine solution, and silicone oil containing 2% Dow Corning 749 according to the method in Example 1, and use them as internal phase fluid, external phase fluid, and continuous phase fluid respectively. Wherein, the zirconium dioxide precursor solution contains zirconyl nitrate and yttrium nitrate, and their molar concentrations are 1.063mol / L and 0.093mol / L respectively; the hexamethylenetetramine solution contains hexamethylenetetramine and urea , and their molar concentration is 3.2mol / L; 2% Dow Corning 749 surfactant is added to the silicone oil according to the volume ratio.

[0112] The zirconia precursor solution, the hexamethylenetetramine solution and the silicone oil containing 2% 749 surfactant were packed into 1ml, 1ml and 10ml syringes respectively and connected to the room temperature droplet microreact...

Embodiment 3

[0115] Example 3: Sintering the zirconia gel beads prepared by the room temperature droplet microreactor

[0116] The 160 μm gel microspheres prepared in Example 2 using the room temperature droplet microreactor were transferred to a crucible, placed in a sintering furnace for sintering, and the sintering process was below 600°C, and the temperature was raised at a rate of 0.5°C per minute , and held at 90°C, 240°C, 320°C, 470°C, and 600°C for 1 hour respectively, between 600°C and 1250°C, the temperature was raised at a rate of 1°C per minute, and kept at 1100°C for 1 hour. 1250°C was kept at the highest temperature for 2 hours, then dropped from 1250°C to 850°C at a rate of 8°C per minute, then naturally cooled to room temperature, and the sintering was completed to obtain zirconia ceramic microspheres with a size of 70 μm ( Figure 4 ).

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Abstract

The invention provides a room temperature droplet micro-reactor and a method of producing zirconium dioxide gel microspheres. The room temperature droplet micro-reactor comprises an internal phase fluid inject pipe, an external phase fluid inject pipe, a collection pipe, and a continuous phase fluid inlet pipe. The internal phase fluid inject pipe is provided with a first inlet, a first outlet and an internal phase fluid channel. The external phase fluid inject pipe sleeves outside the internal phase fluid inject pipe. An inlet end of the collection pipe sleeves the external side of an outlet end of the external phase fluid inject pipe. A third outlet is formed by the inner periphery of the collection pipe and the outer periphery of the external phase fluid inject pipe. The continuous phase fluid inlet pipe sleeves the external sides of the external phase fluid inject pipe and the collection pipe. A continuous fluid channel is formed by the inner periphery of the continuous phase fluid inlet pipe and the outer periphery of the external phase fluid inject pipe. The continuous phase fluid inlet pipe is provided with a third inlet and the third outlet. The room temperature droplet micro-reactor can be used for preparing the gel microspheres having excellent sphericity degree and uniformity.

Description

technical field [0001] The invention belongs to the technical field of material synthesis and forming, in particular, the invention relates to a room temperature droplet microreactor and a method for preparing zirconia gel microspheres using the room temperature droplet microreactor. Background technique [0002] Gel microspheres are a new research field in polymer and material science. Due to their designable structure and physicochemical properties, they are widely used as new functional materials in energy, environment, biology and other disciplines. The gel microspheres prepared by the microfluidic method also have good monodispersity, so that they can better meet the requirements of specific applications such as standard metering, drug delivery, and catalytic carriers. [0003] The use of microreactors to initiate the reaction between two liquid phases is an important technical route for the synthesis and preparation of gel microspheres by microfluidic methods. In the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00B01J13/00C01G25/02
CPCB01J13/0091B01J19/0093B01J2219/00797C01G25/02C01P2004/32C01P2004/61
Inventor 陈皓生王培毅梁帅帅满佳李疆刘兵
Owner UNIV OF SCI & TECH BEIJING
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