• 专利标题:   Complex material useful for detecting and identifying stannous ions and ferrous ions in fields of environment and life sciences, and preparing fluorescence sensor based on layered double hydroxides for detecting silver ion comprises graphene oxide and 1-aminopyrene.
  • 专利号:   CN113930236-A
  • 发明人:   GUO E, YANG L, MAO X, ZHANG J, GUO W
  • 专利权人:   FUJIAN HAINING ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
  • 国际专利分类:   C09K011/06, C09K011/65, G01N021/64
  • 专利详细信息:   CN113930236-A 14 Jan 2022 C09K-011/06 202268 Chinese
  • 申请详细信息:   CN113930236-A CN11181996 11 Oct 2021
  • 优先权号:   CN11181996

▎ 摘  要

NOVELTY - Complex material comprises graphene oxide and 1-aminopyrene. The complex material is prepared by (i) (a) synthesizing 1-nitropyrene, and (b) taking 1-nitropyrene into three-necked flask, adding ethanol and palladium/carbon, slowly heating system, taking hydrazine hydrate into dropping funnel, slowly dropping hydrazine hydrate into reaction system, carrying out reaction, closing oil bath, removing reaction device, cooling product to room temperature, centrifuging by centrifuge, pouring supernatant, and washing with absolute ethanol to obtain 1-aminopyrene, and (ii) taking graphene oxide and 1-aminopyrene into flask, adding tetrahydrofuran as reaction solvent, carrying out reaction, reducing temperature to room temperature, centrifuging by centrifuge, taking out supernatant, washing with ethanol solution for twice, ultrasonically vibrating, and introducing it in vacuum drying box for drying. USE - The material is useful for detecting and identifying stannous ions and ferrous ions in the fields of environment and life sciences, and in preparing fluorescence sensor based on layered double hydroxides for detecting silver ion (all claimed). ADVANTAGE - The material: has a strong ability to identify stannous ions and ferrous ions; and achieves excellent fluorescence recognition of the target stannous ions and ferrous ions. DETAILED DESCRIPTION - Complex material comprises graphene oxide and 1-aminopyrene. The complex material is prepared by (i) (a) synthesizing 1-nitropyrene by taking 2 g dried pyrene, introducing into 50 ml glacial acetic acid solution, using ultrasonic disperser for dispersing for 5 minutes, introducing well-dispersed solution into three-necked flask, mixing with stirrer on low speed, introducing 11 ml concentrated nitric acid into dropping funnel, placing dropping funnel on side of neck, slowly dropping concentrated nitric acid to three-necked flask at room temperature for 1 hour, turning on stirrer to medium speed, carrying out reaction for 1 hour, adding 100 ml water to reaction system, canceling stirring, allowing to stand, filtering to obtain crude product, adding acetic acid for washing product, introducing it in vacuum drying box to dry, drying, and grinding obtained yellow-brown solid, and (b) taking 500 mg 1-nitropyrene into three-necked flask, adding 100 ml ethanol and 0.5 g palladium/carbon, slowly heating the system at 70degreesC, taking 10 ml hydrazine hydrate into the dropping funnel, slowly dropping hydrazine hydrate into the reaction system for 2 hours, carrying out the reaction for 1 hour, closing oil bath, removing reaction device, cooling product to room temperature, centrifuging by centrifuge, pouring the supernatant, and washing with absolute ethanol for 2-3 times to obtain 1-aminopyrene, and (ii) taking 100 mg graphene oxide and 100 mg 1-aminopyrene into flask, adding 100 ml tetrahydrofuran as reaction solvent, carrying out reaction at 60degreesC for 72 hours, reducing temperature to room temperature, centrifuging by centrifuge, taking out the supernatant, washing with ethanol solution for twice, ultrasonically vibrating, introducing it in vacuum drying box for drying to obtain the pyrene-containing graphene oxide complex, which is labeled as GO-g-Py. INDEPENDENT CLAIMS are also included for: a fluorescence sensors based on layered double hydroxides, comprising magnesium-aluminum hydrotalcite and the pyrene-containing graphene oxide complex material; preparing the fluorescence sensor based on layered double hydroxides, comprising (I) taking 2.44 g magnesium chloride hexahydrate in a 50 ml beaker, adding 20 ml deionized water to dissolve, setting the volume to 50 ml, taking 0.966 g aluminum chloride hexahydrate in the 50 ml beaker, adding 20 ml deionized water to dissolve, setting the volume to 50 ml, taking 0.363 g anhydrous sodium carbonate in the 50 ml beaker, adding 20 ml deionized water to dissolve, setting the volume to 50 ml, taking 0.48 g sodium hydroxide, dissolving it in the 50 ml beaker, adding 30 ml deionized water to dissolve, and setting the volume to 100 ml, and (II) measuring 30 ml prepared aluminum chloride solution, adding it to the three-necked flask containing 30 ml sodium carbonate solution, installing a reflux device in the middle neck, installing a dropping funnel containing 30 ml magnesium chloride solution on the left, installing the dropping funnel containing 50 ml sodium hydroxide solution on the right, setting the temperature of the constant temperature water bath to 65degreesC, installing a magnetic stirring device, starting the reaction, slowly adding magnesium chloride solution to the reaction system, and slowly adding the GO-g-Py product prepared above to the reaction system, adjusting the pH value to 10, keeping it constant, finishing dropping the solution, stopping stirring, raising the temperature to 70degreesC for aging for 24 hours, filtering the washed product and drying at 70 degreesC for 12 hours to obtain product, and labeling GO-g-Py/LDHS; and use of fluorescence sensor based on layered double hydroxides in silver ion detection, comprising (1) taking 0.0293 g GO-g-Py/LDHS complex material, configuring it into a 50 ml solution, uniformly dispersing under ultrasonic waves, and configuring 10-3 mol/l different kinds of metal ions, (2) taking 2 ml metal ion solution and 1 ml GO-g-Py/LDHS complex material to 5 ml for detecting, and (3) exciting at 380 nm, where the width of the fluorescence slit used is 10 nm, where silver (II) ion played a significant role in weakening the fluorescence intensity of GO-g-Py/LDHS complexes.