• 专利标题:   Preparing molecular imprinted estrogenic endocrine disruptor involves hydrothermal synthesis of magnetic graphene by dissolving ferric chloride hydrate in ethylene glycol to obtain mixture, which is agitated in ultrasonic agitator.
  • 专利号:   CN103641944-A, CN103641944-B
  • 发明人:   HUANG Y, LI P, LI Y, WU J, KOU X, LI J
  • 专利权人:   UNIV TIANJIN POLYTECHNIC
  • 国际专利分类:   B01J020/26, B01J020/30, C08F002/38, C08F212/36, C08F220/06, C08J009/28, G01N027/26
  • 专利详细信息:   CN103641944-A 19 Mar 2014 C08F-212/36 201434 Pages: 9 Chinese
  • 申请详细信息:   CN103641944-A CN10677176 13 Dec 2013
  • 优先权号:   CN10677176

▎ 摘  要

NOVELTY - Molecular imprinted estrogenic endocrine disruptor preparation involves hydrothermal synthesis of magnetic graphene by dissolving ferric chloride hydrate in ethylene glycol to obtain mixture, which is agitated in an ultrasonic agitator to obtain yellow transparent solution, which is mixed with graphene oxide and anhydrous sodium acetate, with continuous stirring for 30 minutes in a stainless steel vessel. The obtained solution is placed in an oven at 200 degrees C for 8-24 hours, and then obtained product is separated using magnetic separator to obtain product. USE - Method for preparing molecular imprinted estrogenic endocrine disruptor (claimed). DETAILED DESCRIPTION - Molecular imprinted estrogenic endocrine disruptor preparation involves hydrothermal synthesis of magnetic graphene by dissolving ferric chloride hydrate in ethylene glycol to obtain mixture, which is agitated in an ultrasonic agitator to obtain yellow transparent solution, which is mixed with graphene oxide and anhydrous sodium acetate with continuous stirring for 30 minutes in a stainless steel vessel. The obtained solution is placed in an oven at 200 degrees C for 8-24 hours, and then obtained product is separated using magnetic separator to obtain product. The obtained product is washed with deionized water and ethanol, and then dried for 12 hours to obtain product. Magnetic graphene bromide is prepared by mixing sodium hydroxide and sodium chlorate in an ultrasonic mixer for l-2 hours to obtain mixture. The obtained mixture is kept to obtain precipitate, which is isolated and washed for three times with anhydrous ethanol, and then dried in a vacuum oven to give carboxylated magnetic graphene. Carboxylated magnetic graphene is mixed with ethyl bromoacetate and anhydrous toluene under nitrogen atmosphere to obtain mixture. The obtained mixture is mixed with trimethylamine at 100 degrees C for 24-48 hours to obtain product, which is washed with toluene, ethanol and diethyl ether three times. The obtained product is dried in vacuum to obtain product. Reversible addition-fragmentation chain-transfer polymerization is performed by mixing magnetic grapheme with phenylmagnesium bromide in tetrahydrofuran in an ultrasonic dispersor to obtain mixture. The obtained mixture is heated with carbon disulfide in an oil bath at 40 degrees C for 2-4 hours to obtain solution. The obtained solution is mixed with magnetic graphene bromide under nitrogen gas atmosphere at 60 degrees C for 24-72 hours to obtain mixture. The obtained mixture is mixed with hydrochloric acid, and then washed with distilled water, tetrahydrofuran, ethanol three times to obtain product, which is dried in vacuum to obtain reversible addition-fragmentation chain transfer agent, which is mixed with acetonitrile, estrogen, methacrylic acid and divinylbenzene in an oil bath at 50-80 degrees C for 24 hours to obtain product. The obtained product is washed with chloroform, methanol, acetone for 3 times to obtain product, which is mixed with glacial acetic acid and ethanol in molar ratio of 2:8 to obtain mixture. The obtained mixture is dried in vacuum to obtain desired product.