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Preparation method for particle diameter controllable millimeter-scale polyurea monodisperse microsphere

A monodisperse microsphere, millimeter-scale technology, applied in the field of preparing polymer monodisperse microspheres and millimeter-scale polyurea monodisperse microspheres, can solve the problems of complex post-processing process, low monomer conversion rate and high production cost, To achieve the effect of simple post-processing steps, simple post-processing process, low production cost and energy consumption

Inactive Publication Date: 2014-11-19
UNIV OF JINAN
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  • Description
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Problems solved by technology

[0006] Aiming at the deficiencies of the prior art, the present invention provides a low-cost, pollution-free method for preparing millimeter-sized polyurea microspheres with controllable particle size by sedimentation polymerization, so as to solve the problem of preparing polymer microspheres by the existing sedimentation polymerization technology. There are problems such as low monomer conversion rate, serious pollution, high production cost and complicated post-treatment process

Method used

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  • Preparation method for particle diameter controllable millimeter-scale polyurea monodisperse microsphere
  • Preparation method for particle diameter controllable millimeter-scale polyurea monodisperse microsphere
  • Preparation method for particle diameter controllable millimeter-scale polyurea monodisperse microsphere

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Experimental program
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Effect test

Embodiment 1

[0045] Add 400 g of 0.1% ethylenediamine aqueous solution (liquid level height 10 cm, the same below) into a 500 mL beaker with a height of 15 cm, and then place the beaker in a constant temperature water bath at 70 ° C until the system temperature is constant at 70 ° C , use a syringe pump to drop 20mL of toluene diisocyanate monomer into the ethylenediamine aqueous solution at a rate of 130mL / h through a needle with an inner diameter of 250μm, and continue to keep warm for 4h after the addition is completed. Then the product was filtered and dried in an oven at 80° C. for 10 h to obtain the polyurea microsphere product.

[0046] The average particle size of the obtained polyurea microspheres is 0.66mm, the particle size polydispersity coefficient is 1.011, and the specific surface is 118.68m 2 / g, the porosity is 48.2%, and its scanning electron micrograph is as follows figure 1 As shown, the microsphere cross-sectional scanning electron micrograph ( figure 2 ) shows tha...

Embodiment 2

[0048] Add 400 g of triethylenetetramine aqueous solution with a mass fraction of 0.1% to a 500 mL beaker with a height of 15 cm, and then place the beaker in a constant temperature water bath at 60 ° C. After the temperature is constant, use a syringe pump to inject 130 mL Add 20 mL of toluene diisocyanate monomer dropwise to the triethylenetetramine aqueous solution at a speed of 1 / h, and continue the heat preservation reaction for 3 h after the dropwise addition is completed. Then the product was filtered and dried in an oven at 80° C. for 10 h to obtain the polyurea microsphere product.

[0049] The average particle size of the obtained polyurea microspheres is 0.68mm, the particle size polydispersity coefficient is 1.008, and the specific surface is 109.56m 2 / g, the porosity is 45.5%, and the optical microscope photos of the microspheres are as follows image 3 shown.

Embodiment 3

[0051] Add 400g of distilled water to a 500mL beaker with a height of 15cm, and then place the beaker in a constant temperature water bath at 50°C. After the temperature is constant, use a syringe pump to drop into the water at a rate of 50mL / h 20mL of toluene diisocyanate monomer, after the dropwise addition, continue to keep warm for 3h. Then the product was filtered and dried in an oven at 80° C. for 10 h to obtain the polyurea microsphere product.

[0052] The average particle size of the obtained polyurea microspheres is 0.30mm, the particle size polydispersity coefficient is 1.005, and the specific surface is 149.83m 2 / g, the porosity is 57.3%, the infrared spectrum of the microspheres is as follows Figure 4 shown.

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Abstract

The invention relates to a preparation method for a particle diameter controllable millimeter-scale polyurea monodisperse microsphere. The preparation method comprises the following steps: isocyanate compound is adopted as a monomer and is squeezed through syringe needles or capillary tubes to form liquid drops and the liquid drops are added into water or a polyamine aqueous solution for sedimentation and polymerization; during the settlement process of the liquid drops, the monomers on the surfaces of the liquid drops react with the water or the polyamine aqueous solution rapidly to form a gelatin layer or callus and the stability of particles is maintained. According to the method, as water is adopted as the dispersion medium, no pollution is generated; the polymerization reaction can be conducted under lower temperature, the equipment is simple and the manufacturing cost is low; the obtained microsphere is free from residual monomer and the post-processing is simple; no surface modified agent or pore-foaming agent is needed, porous polyurea microsphere with rich amino on the surface is prepared in one step; the method can be used in the fields of enzyme immobilization, chemocatalysis, dye, adsorption and separation of heavy metal ions and the like.

Description

technical field [0001] The invention relates to a method for preparing polymer monodisperse microspheres, in particular to a method for preparing millimeter-sized polyurea monodisperse microspheres with controllable particle size through sedimentation polymerization, and belongs to the field of functional polymer materials. Background technique [0002] Polymer monodisperse microspheres have been widely used in the fields of chromatographic analysis, chemical catalysis, drug release and enzyme immobilization. Due to the large size and low specific surface area of ​​millimeter-scale polymer monodisperse microspheres, it has the characteristics of simple separation operation and low chromatographic column pressure when used as chromatographic packing, which is conducive to industrial mass application. Therefore, millimeter-scale polymer monodisperse microspheres have important application prospects. At present, such microspheres are generally prepared by suspension polymeriza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C08G18/76B01J13/14
CPCB01J13/14C08G18/302C08G18/3228C08G18/7614C08G18/7671C08G2110/0083
Inventor 姜绪宝张飞龙朱晓丽孔祥正
Owner UNIV OF JINAN
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