文献类型：专利

英文题名：Sulfonic acid-modified strong cationic hyper-crosslinked resin useful in solid phase extraction filler, and obtained by reacting divinylbenzene with 4-chloromethyl styrene and dilute sulfuric acid

作者：HU P;SUN W;ZHANG M;WANG Y;ZHANG H;XU Y

机构：[1]UNIV EAST CHINA SCI & TECHNOLOGY

申请号：CN104693336-A

申请日：2015-03-09

公开日：2015-06-10

语种：英文

收录：DERWENT

摘要：NOVELTY - Sulfonic acid-modified strong cationic hyper-crosslinked resin (I) is claimed. (I) is obtained by reacting divinylbenzene (II) with 4-chloromethyl styrene (III) and dilute sulfuric acid. USE - (I) is useful in solid phase extraction filler (claimed). DETAILED DESCRIPTION - Sulfonic acid-modified strong cationic hyper-crosslinked resin of formula (I) is claimed. (I) is obtained by reacting divinylbenzene of formula (II) with 4-chloromethyl styrene of formula (III) and dilute sulfuric acid. An INDEPENDENT CLAIM is also included for preparation of sulfonic acid-modified cationic hyper-crosslinked resin (I) comprising (i) reacting (II) with (III) in acetonitrile solvent in presence of azobisisobutyronitrile initiator, carrying out ultrasonication and passing nitrogen gas and oxygen gas to remove solvent, heating at 60?C for 46 hours, centrifugating, washing with methanol, toluene and acetone to remove linear structure of raw materials and drying under vacuum to obtain white low degree crosslinking chloromethyl styrene-divinylbenzene copolymer of formula (IV), (ii) dissolving (IV) in dichloroethane solvent, carrying out ultrasonication and passing nitrogen gas and oxygen gas to remove solvent, adding ferric chloride as a catalyst, heating at 80 degrees C for 18 hours, centrifugating, washing with methanol and nitric acid solution of pH 1, removing dichloroethane and ferric chloride in resin, washing, extracting resin with acetone using soxhlet under reflux for 12 hours, cooling to room temperature, centrifugating to remove acetone, washing with methanol and ether and drying under vacuum to obtain yellow high degree crosslinking chloromethyl styrene-divinylbenzene copolymer of formula (V), and (c) dissolving high degree crosslinking chloromethyl styrene-divinylbenzene copolymer in dichloroethane, carrying out ultrasonication and passing nitrogen gas and oxygen gas to remove solvent, heating at 80?C for 4 hours, distilling dichloroethane at 100 degrees C for 2 hours, cooling to room temperature, adding resulting product to ice-brine, centrifugating to remove excess sulfuric acid, washing with 2 mol/l hydrochloric acid and water and drying under vacuum to obtain brown final product (I).