Preparation method of macroporous long alkyl side chain acrylic acid ester-styrene-ethylene dimethacrylate crosslinking copolymerization microballoon

A technology of ethylene glycol dimethacrylate and acrylate, which is applied in the field of macroporous cross-linked copolymer microspheres and their preparation, can solve the problems of complex effects of influencing factors and unreported problems, and achieve low production cost and spherical shape. The effect of good temperature and easy temperature control

Inactive Publication Date: 2011-11-09
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, people have used this method to prepare polymer microspheres with heterogeneous structure in a variety of monomer systems, and studied the effects of water phase composition, crosslinking agent and porogen in the system on the polymer microspheres. morphology and pore structure, but the previous studies on acrylate porous microspheres mostly focused on trimethylolpropane methacrylate, 2-hydroxyethyl methacrylate, ethylene glycol dimethacrylate, Short side chain monomer systems such as (meth) acrylates, and research on long-chain acrylate polymers are all concentrated in the field of low-crosslinking and high oil-absorbing resins, and research on heterogeneous (porous) long-chain acrylate polymers research, so far unreported
And because the effect of influencing factors in the process of preparing porous resin by suspension method is very complicated, and there is no general theory to determine the optimal reaction conditions of a certain suspension polymerization reaction system, so different reaction systems need to be targeted. sex studies

Method used

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  • Preparation method of macroporous long alkyl side chain acrylic acid ester-styrene-ethylene dimethacrylate crosslinking copolymerization microballoon

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Weigh 3.75g of lauryl acrylate, 3.75g of styrene, 7.5g of ethylene glycol dimethacrylate, and 15g of n-octanol, and mix them evenly. Dissolve 0.15g of benzoyl peroxide in the above mixture to form an oil phase. Add 695% polyvinyl alcohol aqueous solution to 2% NaCl aqueous solution to prepare the aqueous phase required for the reaction. Using the suspension polymerization method, first add the water phase solution into a 1000mL four-port reactor equipped with a condenser, an electric stirrer and a heating device, and pass in nitrogen gas, then add the oil phase solution after 30 minutes, and stir at a speed of 300r / min. Heating to 85°C, constant temperature reaction for 10 hours to obtain a bead copolymer, the product was filtered and washed with deionized water at 60-70°C, then extracted with acetone for 24 hours, and finally dried in a vacuum oven at 60°C to constant weight. The total hole area of ​​the product is 148.84m 2 / g, the total pore volume is 1.15mL / g, the ...

Embodiment 2

[0020] Weigh 4.5g of lauryl acrylate, 4.5g of styrene, 9g of ethylene glycol dimethacrylate, and 12g of n-octanol, and mix them evenly. Dissolve 0.15g of benzoyl peroxide in the above mixture to form an oil phase. Add 6 g of 5% polyvinyl alcohol aqueous solution to 2% NaCl aqueous solution to prepare the aqueous phase required for the reaction. Using the suspension polymerization method, first add the water phase solution into a 1000mL four-port reactor equipped with a condenser, an electric stirrer and a heating device, and feed nitrogen, then add the oil phase solution after 30 minutes, and stir at a speed of 300r / min. Heating to 85°C, constant temperature reaction for 10 hours to obtain a bead copolymer, the product was filtered and washed with deionized water at 60-70°C, then extracted with acetone for 24 hours, and finally dried in a vacuum oven at 60°C to constant weight. The total hole area of ​​the product is 127.75m 2 / g, the total pore volume is 0.704mL / g, the poros...

Embodiment 3

[0022] Weigh 3.75g of tetradecyl acrylate, 3.75g of styrene, 7.5g of ethylene glycol dimethacrylate, and 12g of liquid paraffin, mix well, and dissolve 0.15g of benzoyl peroxide in the above mixture to form an oil phase. Add 6 g of 5% polyvinyl alcohol aqueous solution to 2% NaCl aqueous solution to prepare the aqueous phase required for the reaction. Using the suspension polymerization method, first add the water phase solution into a 1000mL four-port reactor equipped with a condenser, an electric stirrer and a heating device, and pass in nitrogen gas, then add the oil phase solution after 30 minutes, and stir at a speed of 300r / min. Heating to 85°C, constant temperature reaction for 10 hours to obtain a bead copolymer, the product was filtered and washed with deionized water at 60-70°C, then extracted with acetone for 24 hours, and finally dried in a vacuum oven at 60°C to constant weight. The total hole area of ​​the product is 33m 2 / g, the total pore volume is 1.65mL / g, ...

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Abstract

The invention provides a preparation method of macroporous long alkyl side chain acrylic acid ester-styrene-ethylene dimethacrylate crosslinking copolymerization microballoon. The invention relates to macroporous long alkyl side chain acrylic acid ester-styrene-ethylene dimethacrylate crosslinking copolymerization microballoon and a preparation method thereof. In the preparation method, oil-soluble benzoyl peroxide is an initiator, long alkyl side chain acrylic acid ester, styrene and ethylene dimethacrylate are monomers, a suspension polymerization method is employed, an aqueous solution containing a dispersant and salt is water phase, and the monomers containing the initiator and a pore forming agent are mixed as stable oil phase. Under protection of nitrogen, the oil phase is stirred and subjected to a polymerization reaction at a certain temperature, and a resultant is subjected to filtering, washing, Soxhlet extraction, and vacuum drying treatments to obtain the macroporous crosslinking copolymerization microballoon. The above synthetic method has the advantages of safety, easy separation of products, low production cost, easy control of temperature, stable product quality the like, and is suitable for large scale industrial production. Since having porous and hydrophobic characteristics, the hydrophobic macroporous microballoon disclosed in the invention has a substantial advantage in removing enriched hydrophobic organic pollutants in water, which is a prospective environment friendly adsorption material and can be effectively used for processing relative organic waste water. The hydrophobic macroporous microballoon also has potential application value in fields of catalyst and drug carrier, bioseparation and the like.

Description

technical field [0001] The invention relates to the field of crosslinked copolymerized polymer materials, in particular to a macroporous crosslinked copolymerized microsphere containing long alkyl side chain acrylate and a preparation method thereof. Background technique [0002] Recently, porous cross-linked acrylate copolymer microspheres have been widely used in chromatographic column fillers, resin catalysts, catalyst supports, biological separation (US20080311399A1), dialysis separation, drug carriers (WO2009073193A2), water treatment and purification, ion recovery (CN101314124A), adsorption materials ( CN101543764A) and other applications in many fields have aroused people's general attention. These applications mainly take advantage of the porous structure and high surface area of ​​copolymerized microspheres. Since the 1950s, Dusek K, Kunin R, and Millar JR et al. have prepared polymer microspheres with a porous structure by means of suspension polymerization. So f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F220/18C08F222/14C08F2/20C08J9/04C08J3/12
Inventor 栾兆坤李烨彭先佳贾智萍
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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