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Preparation method of polymer microspheres with uniform particle size

A polymer microsphere and particle size technology, which is applied in the field of preparation of uniform particle size polymer microspheres, can solve the problems of limited popularization, integration, instability, etc., achieve rapid swelling of polymerized monomers, reduce production costs, reduce pollution effect

Inactive Publication Date: 2020-09-15
南京亘闪生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in the above-mentioned two-step swelling method, acetone needs to be added as a co-solvent during swelling, so the seed microspheres are extremely fragile, and problems such as instability, rupture, and fusion will occur during the swelling process, resulting in too long time for swelling, which is difficult for industrialization. production, which limits its promotional use

Method used

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  • Preparation method of polymer microspheres with uniform particle size
  • Preparation method of polymer microspheres with uniform particle size
  • Preparation method of polymer microspheres with uniform particle size

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preparation example Construction

[0032] Such as Figure 1-6 , a method for preparing polymer microspheres with uniform particle size, comprising the following steps:

[0033] (1) Preparation of swelling monomer: take equimolar equivalents of acrylamide and phenylboronic acid,

[0034] The reaction is carried out under the condition of water phase or in the presence of an emulsifier to obtain an aqueous solution of a new compound formed by coordination of the acrylamide substance and the phenylboronic acid substance, and the water solubility of the aqueous solution of the new compound is greater than 2g / 100mL.

[0035] (2) Preparation of activated seed microspheres: Add the new compound in step (1) to the seed, after swelling at room temperature, select potassium persulfate or sodium bisulfite redox initiation system, and initiate the new compound in the seed at room temperature. Polymerize to obtain activated seed microspheres with uniform particle size, and set aside.

[0036] (3) Preparation of oil phase:...

Embodiment 1

[0050] Preparation of seed microspheres

[0051] Take 1.2 g of polyvinylpyrrolidone (PVP) and dissolve it in a mixture of 90 mL of ethanol and 10 mL of deionized water, add it to a 250 mL three-necked flask with a reflux condenser, and add 0.4 g of azobis A solution of 25 g of isobutyronitrile (AIBN) in styrene was polymerized at 70 °C for 8 h; the product was centrifuged at a speed of 4 000 r / m, the supernatant liquid was decanted, washed with absolute ethanol, and washed with 0.25% decathene Dialkyl sodium sulfate solution replaces ethanol, and is made into 0.25% sodium lauryl sulfate solution of 5% solid content, obtains the polystyrene microsphere primary seed that particle size is 2.5 microns, CV value 2.1%.

Embodiment 2

[0053] Preparation of seed microspheres

[0054] Dissolve 0.265g of sodium chloride (NaCl) in 500g of distilled water, then add 45g of monomeric styrene (St) into the three-necked flask, blow nitrogen to drive oxygen for 15 minutes under stirring at 350rpm, then raise the temperature to 70°C, and reach temperature equilibrium , add 5g of 10% potassium persulfate KPS aqueous solution, and start polymerization; under the protection of nitrogen, the polymerization time is 24 hours, after the reaction is completed, cool to room temperature, and obtain the primary seeds of polystyrene microspheres with a particle size of 580nm and a CV value of 2.3%. .

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Abstract

The invention discloses a preparation method of polymer microspheres with uniform particle size, and relates to the field of polymer microspheres. Acrylamide substances are introduced into seed microspheres to react with phenylboronic acid substances, polymerization is performed to generate a new heat-sensitive compound to activate the seeds, and seed microspheres which are swelled, a polymerizable monomer, a cross-linking agent, a pore-foaming agent, an initiator and the like are heated to a polymerization temperature, and are polymerized to obtain the polymer microspheres with uniform particle size. The method has the advantages of being simple in design of the seed microspheres, short in total reaction time, high in swelling multiple, high in recovery rate and the like, the production cost is reduced, the environmental pollution is reduced, and the market application value is very high.

Description

technical field [0001] The invention relates to the field of polymer microspheres, more specifically, it relates to a method for preparing polymer microspheres with uniform particle diameter. Background technique [0002] There are many methods to prepare polymer microspheres, such as suspension polymerization method, seed swelling method, dispersion polymerization method, etc. Suspension polymerization can generate particles with a particle size ranging from 50 μm to 1mm, but the size distribution is wide, and it generally needs to be graded. Ugelstad et al. invented a new and effective method for preparing monodisperse, large-diameter polymer microspheres—the two-step swelling method. This method can be used to obtain a particle size of 1-100 μm with a standard deviation < 2% porous polymer microspheres. [0003] The theoretical basis of the two-step swelling method is to use a water-insoluble low-molecular-weight solvent that can greatly improve the swelling capacity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F257/02C08F212/08C08F2/16C08J9/28
CPCC08F257/02C08F2/16C08J9/28C08J2351/00C08F212/08
Inventor 任连兵仲玉
Owner 南京亘闪生物科技有限公司
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