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Method for rapidly preparing monodisperse polyvinyl alcohol microspheres at normal temperature

A technology of polyvinyl alcohol microspheres and polyvinyl alcohol, applied in chemical instruments and methods, gel preparation, chemical/physical/physicochemical processes, etc., can solve the problem of inability to achieve fast and convenient preparation of PVA microspheres and long curing time , high curing temperature and other issues

Active Publication Date: 2019-07-09
ENERGY RES INST OF SHANDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can prepare PVA microspheres with uniform particle size and good sphericity, the curing time is too long, the curing temperature is high, and the washing process is complicated.
[0005] It can be seen that the existing technology cannot realize the rapid and convenient preparation of PVA microspheres at room temperature. Therefore, it is of great significance to further improve the preparation process and develop a preparation method that can quickly and conveniently prepare monodisperse PVA microspheres at room temperature.

Method used

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  • Method for rapidly preparing monodisperse polyvinyl alcohol microspheres at normal temperature
  • Method for rapidly preparing monodisperse polyvinyl alcohol microspheres at normal temperature
  • Method for rapidly preparing monodisperse polyvinyl alcohol microspheres at normal temperature

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Embodiment 1

[0071] This embodiment provides a method for rapidly preparing monodisperse polyvinyl alcohol microspheres at room temperature, and the structure of the microchannel reactor it adopts is as follows: Figure 4 shown.

[0072] The microchannel reactor includes a droplet generation zone, a fluid convection mixing zone in the droplet, and a droplet pre-crosslinking solidification zone, wherein:

[0073] The channel in the droplet generation area has a width of 100 microns and a height of 150 microns, which is a flow-focused micro channel, including two dispersed phase channels and two continuous phase channels;

[0074] The length L of the channel of the fluid convective mixing zone in the droplet is 6654 microns and the width W 1 is 200 microns and a height of 150 microns,

[0075] The length L of the channel in the droplet pre-crosslinking curing zone 3 4000 microns, width W 2 is 1000 microns and a height of 150 microns;

[0076] The channels in the fluid convective mixing ...

Embodiment 2

[0092] This embodiment provides a method for rapidly preparing monodisperse polyvinyl alcohol microspheres at room temperature, and the structure of the microchannel reactor it adopts is as follows: figure 2 shown.

[0093] The microchannel reactor includes a droplet generation zone, a fluid convection mixing zone in the droplet, a droplet pre-crosslinking solidification zone, and a collection bottle (not shown), wherein:

[0094] The width of the channel in the droplet generation area is 300 microns, and the height is 300 microns. It is a T-shaped micro channel, including two dispersed phase channels and two continuous phase channels;

[0095] The length of the channel of the fluid convective mixing zone in the droplet is 13000 microns, the width is 700 microns, and the height is 300 microns,

[0096] The length of the channel in the droplet pre-crosslinking curing zone is 6000 microns, the width is 5600 microns, and the height is 300 microns;

[0097] The Z-shaped curved ...

Embodiment 3

[0106] The microchannel reactor provided in Example 2 was used to prepare monodisperse polyvinyl alcohol microspheres according to the steps in Example 2, the difference being that the continuous phase solution was prepared as follows: 5.0 grams of Span 80 was added to 100 mL of mineral oil and mixed evenly. as a continuous phase solution. The polyvinyl alcohol microspheres obtained in the experiment are in the shape of hazelnuts, and the particle diameter is 160±10 microns. Its scanning electron microscope picture is shown in Figure 7 .

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Abstract

The invention provides a method for rapidly preparing monodisperse polyvinyl alcohol microspheres at normal temperature. The method is carried out by adopting a micro-channel reactor, wherein the micro-channel reactor comprises a liquid drop generation region, a liquid drop internal fluid convection mixing region and a liquid drop pre-crosslinking curing region; and channels of the liquid drop internal fluid convection mixing region comprise a linear channel and a non-linear channel. The method comprises the following steps: pumping a polyvinyl alcohol aqueous solution, a mixed aqueous solution of a cross-linking agent and a catalyst, and an oil phase into the micro-channel reactor to form water-in-oil droplets; rapidly and fully mixing the three components in liquid drops in the liquid drop internal fluid convection mixing region, and then performing a pre-crosslinking reaction in the liquid drop pre-crosslinking curing region to form gel microspheres with linear hemiacetal; carryingout deep crosslinking on the gel microspheres in a collection bottle to obtain an acetal product and further to form polyvinyl alcohol microspheres with a three-dimensional network structure; and conducting washing and separating on the polyvinyl alcohol microspheres to obtain the monodisperse polyvinyl alcohol microspheres. The microsphere has the advantages of controllable particle size, uniformparticle size, good sphericity and the like.

Description

technical field [0001] The invention relates to a method for rapidly preparing monodisperse polyvinyl alcohol microspheres at normal temperature, and belongs to the technical field of polymer microsphere preparation. Background technique [0002] Monodisperse polymer microspheres have uniform particle size and regular morphology, and are widely used in drug targeting and controllable sustained-release carriers, templating agents, adsorption and separation agents, etc., especially PVA microspheres due to their excellent Chemical and thermal stability, chemical modifiability, biocompatibility, etc., have a wide range of applications in medicine, materials, electronics and other fields. The preparation of PVA microspheres by emulsification and cross-linking polymerization of PVA oligomers has the characteristics of simple preparation process, controllable process, and cheap raw material prices. It has become a research hotspot to prepare PVA microspheres with uniform particle s...

Claims

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Application Information

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IPC IPC(8): C08J3/12C08J3/24C08J3/075C08L29/04B01J19/00
CPCB01J13/0065B01J19/0093C08J3/075C08J3/12C08J3/24C08J2329/04
Inventor 王建梅王立秋王建春王雪莹李艳田寒梅侯延进许敏
Owner ENERGY RES INST OF SHANDONG ACAD OF SCI
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