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Composite GMA (Glycidyl Methacrylate)/ZrO2 copolymer microsphere as well as preparation and application thereof

A technology of copolymers and microspheres, applied in the direction of mobile adsorbent separation, organic chemistry, etc., can solve the problems that have not been seen in the application of expanded bed matrix, and achieve the effect of easy control and scale-up production, low cost and fast separation speed

Active Publication Date: 2010-10-27
XIAN RADAR HEALTHCARE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the expanded bed matrix has been successfully applied to the extraction of inclusion bodies, monoclonal antibodies, E. Application Reports in Product Separation and Purification

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) 17.5g ZrO 2 , 400ml of toluene and 17.5g of stearic acid were mixed, stirred and heated to 95°C for 3 hours, and dried to obtain surface-modified ZrO 2 ;

[0024] 2) Add 1.25g of gelatin, 5g of sodium chloride and 250ml of deionized water into a 1L three-neck flask equipped with a stirrer, a condenser and a thermometer, heat up to 55°C and stir for 1.5h;

[0025] 3) 1g of surface-modified ZrO 2 Add to the mixed solution containing 100ml GMA, 10ml DVB, 0.5g BPO, 45.5ml toluene and 4.5ml n-heptane, stir to obtain a stable dispersed polymer phase solution;

[0026] 4) Add the polymer phase solution obtained in step 3) to the dispersed phase solution obtained in step 2), adjust the stirring speed to 300rpm, keep the speed constant, react at 55°C for 1.5h, heat up to 85°C for 10h, and solidify Obtain white microspheres, wash with hot water, extract with acetone to remove the porogen, and vacuum-dry to constant weight to obtain copolymer microspheres, and add 60 g of co...

Embodiment 2

[0031] 1) 52.5g ZrO 2 , 400ml of toluene and 17.5g of stearic acid were mixed, stirred and heated to 85°C for 5 hours, and dried to obtain surface-modified ZrO 2 ;

[0032] 2) Add 7.5g of gelatin, 25g of sodium chloride and 250ml of deionized water into a 1L three-neck flask equipped with a stirrer, condenser and thermometer, and heat up to 65°C and stir for 0.5h;

[0033] 3) 16g surface-modified ZrO 2 Add to the mixed solution containing 100ml GMA, 100ml DVB, 1.5g BPO, 85ml toluene and 65ml n-heptane, stir to obtain a stable dispersed polymer phase solution;

[0034] 4) Add the polymer phase solution obtained in step 3) to the dispersed phase solution obtained in step 2), adjust the stirring speed to 500rpm, keep the speed constant, react at 65°C for 0.5h, heat up to 95°C for 6h, and solidify to obtain The white microspheres were washed with hot water, extracted with acetone to remove the porogen, and vacuum-dried to constant weight to obtain copolymer microspheres; and 30...

Embodiment 3

[0039] 1) 35g ZrO 2 , 400ml of toluene and 17.5g of stearic acid were mixed, stirred and heated to 90°C for 4 hours, and dried to obtain surface-modified ZrO 2 ;

[0040] 2) Add 3.75g of gelatin, 12.5g of sodium chloride and 250ml of deionized water into a 1L three-necked flask equipped with a stirrer, condenser and thermometer, and heat up to 60°C and stir for 1 hour;

[0041] 3) 12g surface-modified ZrO 2 Add to the mixed solution containing 100ml GMA, 40ml DVB, 1.2g BPO, 62.5ml toluene and 62.5ml n-heptane, stir to obtain a stable dispersed polymer phase solution;

[0042] 4) Add the polymer phase solution obtained in step 3) to the dispersed phase solution obtained in step 2), adjust the stirring speed to 400rpm, keep the speed constant, react at 60°C for 1h, heat up to 90°C for 8h, and solidify to obtain The white microspheres were washed with hot water, extracted with acetone to remove the porogen, dried in vacuum to constant weight to obtain copolymer microspheres; a...

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Abstract

The invention relates to a composite GMA (Glycidyl Methacrylate) / ZrO2 copolymer microsphere as well as preparation and application thereof. In the microsphere, the grain size is 120 to 400mu m, the core component is ZrO2, and the shell components are GMA and DVB (Divinylbenzene); and the microsphere contains 0.5 to 14 percent by mass of ZrO2 and 50 to 70 percent by mass of GMA and the balance of DVB. The preparation method of the composite GMA / ZrO2 copolymer microsphere comprises the following steps of: mixing a polymerization phase containing GMA, DVB, surface-modified ZrO2, BPO (Benzoyl Peroxide), toluene and n-heptane with a dispersed-phase aqueous solution containing gelatin and sodium chloride, and heating and solidifying to form a microsphere; then immobilizing Beta-CD (Cyclodextrin) under the existence of NaH, KI and Bu4NBr by taking the microsphere as a vector to obtain the composite GMA / ZrO2 copolymer microsphere. The microsphere has regular sphere, high density, acid-base resistance and good hydrophilcity and can be applied to separating and purifying granatum polyphenol from a granatum extract as an expanded bed adsorption matrix.

Description

technical field [0001] The present invention relates to a kind of composite GMA / ZrO 2 Copolymer microsphere, its preparation method and the application of the copolymer microsphere in the separation and purification of natural product (pomegranate peel polyphenol). Background technique [0002] Expanded Bed Adsorption (EBA) technology is a new protein separation and purification technology developed in the 1990s. It can directly capture the target product from fermentation broth, cell culture fluid or homogenate, and integrate solid-liquid separation, concentration and initial purification into one unit operation. This not only reduces the operation steps, improves the product yield, but also reduces the purification cost and capital investment. It is known as the first new unit operation that has appeared in recent years. Expanded bed adsorption technology combines the advantages of packed bed and fluidized bed, while overcoming some defects of packed bed and fluidized be...

Claims

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Application Information

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IPC IPC(8): B01D15/02C07G99/00
Inventor 相阳袁其朋宋航彬张剑锋
Owner XIAN RADAR HEALTHCARE CO LTD
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