Preparation method of polymer microsphere with liquid carbon dioxide as medium

A liquid carbon dioxide and polymer technology, which is applied in the field of polymer microsphere preparation, can solve the problems of restricted carbon dioxide fluid and high reaction pressure in the reaction process, and achieve the effects of good hydrophobicity and low surface energy, lower pressure and shorter time

Inactive Publication Date: 2013-06-12
SHANGHAI WEIKAI CHEM +1
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  • Abstract
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Problems solved by technology

However, the traditional polymerization reaction needs to be carried out under heating conditions (for example, above 50°C), and the reaction temperature is higher than the critical temperature of carbon dioxide (31.3°C). Therefore, carbon dioxide must be in a supercritical state, and correspondingly, the reaction pressure usually needs to be higher. (≥200bar), the expensive equipment cost and slow reaction process restrict the practical application of carbon dioxide fluid in the preparation of microspheres

Method used

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  • Preparation method of polymer microsphere with liquid carbon dioxide as medium
  • Preparation method of polymer microsphere with liquid carbon dioxide as medium
  • Preparation method of polymer microsphere with liquid carbon dioxide as medium

Examples

Experimental program
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Effect test

Embodiment 1

[0037] 1. Synthesis of stable dispersant

[0038] Azobisisobutyronitrile (AIBN for short) thermal initiator (0.04g, 0.00025mol), BPTTC (0.24g, 0.0010mol) and HFPMA (13.6g, 0.034mol) were dissolved in 10ml of trifluorotoluene, under nitrogen atmosphere , heated to 60°C, and reacted for 48 hours. The polymer was precipitated from solution with methanol, filtered, and dried in a vacuum oven at 45°C for 24 hours. The molecular weight of the obtained stable dispersant was 16200 g / mol.

[0039] 2. Preparation of polymer microspheres

[0040] In the preparation of polymer microspheres with liquid carbon dioxide as the medium of the present embodiment, the light-induced dispersion polymerization is carried out in a 40ml autoclave (such as figure 1 As shown), the quartz glass A above the autoclave is used as a light-transmitting window, and a 3W LED is used as a light source. The reaction kettle was placed in an ice-water bath C with a magnetic stirrer D underneath. The polymerize...

Embodiment 2

[0042] Compared with Example 1, in this example, the amount of the stabilizing dispersant is increased to 10wt%, and the types and amounts of the remaining reagents and the implementation process are the same as in Example 1. The scanning electron micrograph (SEM) of the obtained product is shown in figure 2 ,Depend on figure 2 It can be seen that the obtained polymer product is a regular spherical shape, there is no obvious adhesion between the microspheres, and the particle size of the microspheres is basically 1-10 microns, which is suitable as an additive for coating products.

Embodiment 3

[0044] Compared with Example 1, in this example, the amount of stabilizing dispersant is increased to 15wt%, and the types and amounts of other reagents and the implementation process are the same as in Example 1. The scanning electron micrograph (SEM) of the obtained product is shown in figure 2 ,Depend on figure 2 It can be seen that the obtained polymer product is a regular spherical shape, there is no obvious adhesion between the microspheres, and the particle size of the microspheres is basically 1-10 microns, which is suitable as an additive for coating products.

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Abstract

The invention discloses a preparation method of a polymer microsphere with liquid carbon dioxide as a medium. The method includes the steps of: adding a polymerization monomer, a photoinitiator and a stable dispersant into a reaction kettle, introducing a carbon dioxide gas to conduct emptying, then injecting liquid carbon dioxide, when the temperature and pressure in the reaction kettle become constant, irradiating the inside of the reaction kettle by an initiating light source, letting a reaction to undergo under a temperature ranging from -20 to 30DEG C and a pressure of 20-70bar for 0.5-5h; at the end of the reaction, bringing the temperature back to room temperature, washing the polymer precipitated to the bottom of the reaction kettle by liquid carbon dioxide, and removing the residual polymerization monomer, thus obtaining the polymer microsphere. The method provided in the invention introduces a photo-initiation technology into dispersion polymerization with carbon dioxide as the medium, greatly reduces the carbon dioxide system pressure, and shortens the time of polymerization reaction, thereby significantly reducing the cost of high-pressure reaction equipment and improving the production efficiency. The prepared microsphere has good hydrophobic property and low surface energy, and can be effectively enriched on a coating surface in coating application.

Description

technical field [0001] The invention relates to a preparation method of polymer microspheres, in particular to a preparation method of polymer microspheres using liquid carbon dioxide as a medium. Background technique [0002] Polymer microspheres refer to polymer materials or polymer composite materials with a diameter ranging from nanometers to micrometers and a spherical or approximately spherical geometric shape. Due to its special size and structure, polymer microspheres have long had special and important applications in the fields of electronic information, biomedical technology and coatings. [0003] Polymer microspheres can be synthesized by means of emulsion polymerization, precipitation polymerization and dispersion polymerization. These polymerization processes all need to be carried out in reaction medium (such as alcohols, ethers and other organic solvents). Carbon dioxide fluid is a green solvent, which has the advantages of non-toxic, environmentally friend...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/12C08F2/46
CPCC08F2/46C08F2/12C08F2/48C08F118/04C08F120/14C08F120/18C08F120/20C08F122/14
Inventor 虞明东袁慧雅
Owner SHANGHAI WEIKAI CHEM
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