A kind of high cross-linking degree polymer microspheres with super macropores and preparation method thereof

A technology with high cross-linking degree and polymer is applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc. It can solve the problems of low cross-linking degree of polymer microspheres and difficulty in preparing polymer microspheres, etc. Achieving the effect of wide range of polymerization temperature, mild reaction and high degree of cross-linking

Active Publication Date: 2020-06-16
北京博尔赛谱生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that the existing suspension polymerization method is difficult to prepare polymer microspheres above the micron scale, and other methods need to use a large amount of surfactants, and a complicated cleaning process is required after the preparation, and the obtained polymer microspheres have a low degree of crosslinking and other technical problems, the present invention provides a highly cross-linked polymer microsphere with super macropores and a preparation method thereof, which not only can make the average pore diameter of the prepared polymer microsphere controllable within the range of 980-3900nm , the mass transfer rate of large-sized biomolecules is greatly improved, and the polymerization temperature range is wide, the preparation time is short, there is no need to use a large amount of surfactant in the preparation process, and no complicated cleaning process is required after the preparation. At the same time, the prepared polymer micro The ball has a high degree of cross-linking, can withstand the operating pressure of 3-10MPa, and can continue to trigger ATRP polymerization (Atom Transfer Radical Polymerization, atom transfer radical), which is convenient for further derivation into various functional media, so it can be used in the rapid separation and purification of biological macromolecules The field has good application prospects, especially suitable for the separation and purification of large-sized vaccine particles

Method used

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  • A kind of high cross-linking degree polymer microspheres with super macropores and preparation method thereof
  • A kind of high cross-linking degree polymer microspheres with super macropores and preparation method thereof
  • A kind of high cross-linking degree polymer microspheres with super macropores and preparation method thereof

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preparation example Construction

[0032] A preparation method of highly cross-linked polymer microspheres with super large pores, comprising the steps of:

[0033] Step A, dissolving stabilizer and surfactant in deionized water to form a homogeneous solution to obtain an aqueous phase solution.

[0034] Step B, dissolving the vinyl monomer and divinyl crosslinking agent in the porogen solution, filling nitrogen and deoxygenating, adding an atom transfer radical polymerization initiator system, making the atom transfer radical polymerization initiator The system accounts for 8% of the sum of the moles of the vinyl monomer and the divinyl crosslinking agent to form a uniform solution and obtain an oil phase solution.

[0035] Step C. Add the oil phase solution to the water phase solution under the conditions of nitrogen filling and stirring, and the volume ratio of the oil phase solution to the water phase solution is 1:9 to 1:4 And carry out a temperature-rising polymerization reaction, the reaction temperature ...

Embodiment 1

[0048] A preparation method of highly cross-linked polymer microspheres with super large pores, comprising the steps of:

[0049] Step a1. Preparation of aqueous phase solution: Dissolve 6 g of polyvinyl alcohol with a molecular weight range of 60,000 and 3.3 g of sodium dodecylbenzenesulfonate in 100 mL of deionized water, and stir until uniform and transparent to form a uniform solution to obtain an aqueous phase solution.

[0050] Step b1, oil phase solution preparation: according to the volume ratio of glycidyl methacrylate (GMA) and ethylene glycol dimethacrylate (EDMA) is 1:10, and the total volume of GMA and EDMA and porogen The volume ratio is 1:4, GMA and EDMA are dissolved in the porogen solution, stirred until uniform and transparent, and after filling nitrogen and deoxygenating, add atom transfer radical polymerization initiator system (in this atom transfer radical In the polymerization initiator system, cuprous chloride and 2,2-bipyridine are used as the ligand s...

Embodiment 2

[0054] A preparation method of highly cross-linked polymer microspheres with super large pores, comprising the steps of:

[0055] Step a2, preparation of aqueous phase solution: Dissolve 6 g of polyvinyl alcohol with a molecular weight of 60,000 and 6 g of sodium stearate in 100 mL of deionized water, and stir until uniform and transparent to form a uniform solution to obtain an aqueous phase solution.

[0056] Step b2, oil phase solution preparation: according to the volume ratio of styrene (St) and polyethylene glycol dimethacrylate (PEGDMA) is 1:6, and the volume ratio of the total volume of St and PEGDMA and porogen is Dissolve St and PEGDMA in the porogen solution at a ratio of 1:5, stir until uniform and transparent, and after filling nitrogen and deoxygenating, add the atom transfer radical polymerization initiator system (in this atom transfer radical polymerization initiator In the system, copper bromide and tetramethylethylenediamine (TMEDA) are used as the ligand sy...

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Abstract

The invention discloses a polymer microsphere with super large pores and a high cross-linking degree and a preparation method thereof, comprising: dissolving a stabilizer and a surfactant in deionized water to prepare an aqueous phase solution. The vinyl monomer and the divinyl crosslinking agent are dissolved in the porogen solution, and after nitrogen filling and oxygen exhausting, an atom transfer radical polymerization initiator system is added to prepare an oil phase solution. Under the conditions of filling nitrogen and keeping stirring, the oil phase solution is added to the water phase solution, and the temperature rise polymerization reaction is carried out. The reaction temperature is 50-100 ° C, and the reaction time is 13-24 hours; Filter and wash to remove unreacted residues to obtain polymer microspheres. The invention can not only make the average pore size of the polymer microspheres controllable within 980-3900nm, but also does not need to use a large amount of surfactant, and does not need complicated cleaning process after the preparation, and has good application prospects in the field of rapid separation and purification of biological macromolecules. It is especially suitable for the separation and purification of large-sized vaccine particles.

Description

technical field [0001] The invention relates to the field of polymer microsphere materials, in particular to a polymer microsphere with super large pores and a high crosslinking degree and a preparation method thereof. Background technique [0002] Polymer microspheres refer to polymer particles with a spherical shape and a particle size ranging from tens of nanometers to hundreds of microns. As a biochemical separation medium, polymer microspheres have the advantages of high mechanical strength, stable chemical properties, good acid and alkali resistance, and can be operated under high pressure. Therefore, polymer microspheres have good prospects in the application field of chromatographic media. [0003] Since the separation objects in biochemical separation applications are biomacromolecules, and these biomacromolecules have the characteristics of large molecular size and complex structure, etc., they are easily inactivated and denatured during separation and purification...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F261/04C08F220/32C08F222/14C08F291/08C08F212/08C08F271/02C08F212/36C08F287/00C08F2/18B01J13/14B01J20/26
CPCB01J13/14C08F2/18C08F261/04C08F271/02C08F283/065C08F287/00B01J20/264C08F2438/01C08F212/08C08F222/103C08F220/325C08F222/102
Inventor 张荣月李恒靳海波何广湘
Owner 北京博尔赛谱生物科技有限公司
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