Swelling copolymerization preparation method of N-vinyl pyrrolidone and divinylbenzene monodisperse microsphere

A technology of vinylpyrrolidone and divinylbenzene, which is applied in the field of polymer chemistry and can solve problems such as application limitations

Active Publication Date: 2012-03-21
天津博纳艾杰尔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are mainly the following two methods for this kind of solid phase extraction filler: one is a macroporous copolymer formed by suspension polymerization of two monomers, lipophilic divinylbenzene and hydrophilic N-vinylpyrrolidone; the other is Styrene and divinylbenzene are used as monomers to suspend and polymerize into white balls in a certain proportion, then chloromethylated, and then functionalized with pyrrolidone; both polymerization methods are suspension polymerization, and suspension polymerization is carried out under strong stirring Disperse the monomer into countless small liquid droplets with a wide particle size distribution. After the reaction, sieving balls becomes a very critical step. The particle size distribution after sieving is also relatively wide, which limits its application.

Method used

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  • Swelling copolymerization preparation method of N-vinyl pyrrolidone and divinylbenzene monodisperse microsphere
  • Swelling copolymerization preparation method of N-vinyl pyrrolidone and divinylbenzene monodisperse microsphere
  • Swelling copolymerization preparation method of N-vinyl pyrrolidone and divinylbenzene monodisperse microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 10.8g of polyvinylpyrrolidone and 600ml of absolute ethanol into a 1000ml four-neck flask, stir until the polyvinylpyrrolidone is completely dissolved, raise the temperature to 70°C under the protection of nitrogen, and then add 150g of styrene dissolved in 3.8g of azobisisobutyronitrile solution for 24 hours. Filter, wash with absolute ethanol, dry to constant weight, and set aside.

[0029] Gained polystyrene microspheres have good monodispersity, and the particle diameter is 5.0um, and its scanning electron microscope photo is as follows: figure 1 shown.

Embodiment 2

[0031] In a 1000ml four-neck flask, add 40g of the monodisperse microspheres prepared in Example 1 into 250ml of water containing 0.3g of hydroxypropylmethylcellulose, stir and heat to 40°C, and stir at 40°C for 3 hours.

[0032] After mixing 60g of divinylbenzene, 50g of N-vinylpyrrolidone, 80g of toluene and 1.2g of azobisisobutyronitrile, add 200ml of water containing 0.1g of hydroxypropyl methylcellulose and 1g of TritonX-405, mix and emulsify in It was slowly added dropwise into the solution at 40° C. for a total of 5 hours, and then the swelling was continued for 8 hours, and then 100 g of 1% hydroxypropylmethylcellulose aqueous solution was added. Heating to 88°C, the polymerization reaction was carried out for 12 hours.

[0033] Finally, conventional methods such as filtration, lotion, re-filtration, drying, and pore extraction agent are used to recover the copolymerized microspheres. The particle size of the obtained copolymerized microspheres is concentrated between...

Embodiment 3

[0035] In a 1000ml four-neck flask, add 40g of the monodisperse microspheres prepared in Example 1 into 200ml of water containing 0.3g of hydroxypropylmethylcellulose, stir and heat to 40°C, and stir at 40°C for 3 hours.

[0036] After mixing 60g of divinylbenzene, 50g of N-vinylpyrrolidone, 80g of toluene and 1.2g of azobisisobutyronitrile, add 200ml of water containing 0.1g of hydroxypropyl methylcellulose and 1g of TritonX-405, mix and emulsify in It was slowly added dropwise into the solution at 40° C. for a total of 5 hours, and then the swelling was continued for 8 hours, and then 100 g of 1% hydroxypropylmethylcellulose aqueous solution was added. Heating to 88°C, the polymerization reaction was carried out for 2 hours.

[0037] Lower the temperature and prepare emulsion 2 at the same time. After mixing 30g of divinylbenzene, 30g of N-vinylpyrrolidone, 40g of toluene, 20g of n-heptane and 0.8g of azobisisobutyronitrile, add 0.1g of hydroxypropylmethylcellulose Mix and ...

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Abstract

The invention provides a preparation method of an N-vinyl pyrrolidone and a divinylbenzene copolymerization monodisperse microsphere, which takes the polystyrene monodisperse microsphere that is prepared from dispersion polymerization as a seed, the N-vinyl pyrrolidone, acrylic ester and other comonomers are guided during the swelling copolymerization process, so the corresponding copolymerization microsphere is produced. The copolymerization microsphere which is prepared from the method has easily-controlled state and performance, and meanwhile, the uniformity and productivity of the product size distribution are increased.

Description

technical field [0001] The invention relates to the field of polymer chemistry, in particular to the preparation of N-vinylpyrrolidone and divinylbenzene copolymerized microspheres by a seed swelling method. Background technique [0002] The solid phase extraction packing containing vinylpyrrolidone has both hydrophilic and hydrophobic groups, and has a relatively balanced adsorption effect on various polar and non-polar compounds, and its adsorption capacity and sample capacity are much higher than those of C18 bonded Silica gel can be widely used in the extraction, enrichment and purification of various compounds. At present, there are mainly the following two methods for this kind of solid phase extraction filler: one is a macroporous copolymer formed by suspension polymerization of two monomers, lipophilic divinylbenzene and hydrophilic N-vinylpyrrolidone; the other is Styrene and divinylbenzene are used as monomers to suspend and polymerize into white balls in a certai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F2/00C08J9/28C08L25/08C08F212/36C08F226/10
Inventor 周丽王洪伟汪群杰
Owner 天津博纳艾杰尔科技有限公司
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