CN109019659B - Synthesis method of chiral copper oxide nanoparticles - Google Patents
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- CN109019659B CN109019659B CN201810971848.7A CN201810971848A CN109019659B CN 109019659 B CN109019659 B CN 109019659B CN 201810971848 A CN201810971848 A CN 201810971848A CN 109019659 B CN109019659 B CN 109019659B
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Abstract
A method for synthesizing chiral copper oxide nano particles, belonging to the technical field of synthetic chemistry. Under the mild condition of non-hydrothermal, the copper oxide precursor is acted by a reducing agent and chiral molecules to form monodisperse nano-scale copper oxide particles, and the method mainly comprises the steps of synthesis of the copper oxide precursor and synthesis of chiral copper oxide nanoparticles with different ligands. The invention solves the problem of synthesizing the chiral copper oxide nano particles under the non-organic phase and non-hydrothermal condition and develops the synthesis technology of the nano chiral copper oxide nano particles with regular appearance for the first time. In addition, the synthesized chiral copper oxide nano particles are very stable and have wide biological application prospect.
Description
Technical Field
The invention relates to a method for synthesizing chiral copper oxide nanoparticles, belonging to the technical field of synthetic chemistry.
Background
Chirality is derived from the fact that substances and mirror images of the substances cannot coincide, the substances are basic attributes of the nature, a chiral environment is also formed in an organism, and basic units of amino acids of proteins in the organism are all D-shaped, so that the study of the chiral substances has important significance for the organism. As is well known, metal oxides play an important role in the field of catalysis, and particularly, transition metal oxides are increasingly widely applied in the fields of solar cells, electrocatalysis and the like. Therefore, it becomes very significant to research the development of chiral catalysis of chiral transition metal oxides in organisms. The synthesis method of the chiral copper oxide nano-particles with the nano-scale is not reported.
Disclosure of Invention
The invention aims to overcome the defects and provide a method for synthesizing chiral copper oxide nanoparticles.
According to the technical scheme provided by the invention, the synthesis method of the chiral copper oxide nanoparticles forms monodisperse nano-scale copper oxide particles by using a reducing agent and chiral molecules to act on a copper oxide precursor under a non-hydrothermal mild condition, and comprises the main steps of synthesis of the copper oxide precursor and synthesis of chiral copper oxide nanoparticles with different ligands.
The copper oxide precursor is synthesized by the steps of firstly adding 3M L of ultrapure water into a 5M L system, then mixing copper chloride with the concentration of 0.2M and the concentration of 50-200 mu L with sodium hydroxide solution with the concentration of 0.1M according to the molar ratio of copper chloride to sodium hydroxide of 4:5, ensuring that the pH value of the mixed solution is above 12, and uniformly mixing to obtain the copper oxide precursor.
The synthesis steps of the chiral copper oxide nano particle with penicillamine as ligand are as follows:
(1) adding trisodium citrate into the synthesized copper oxide precursor colloid; wherein, the molar ratio of the copper chloride to the trisodium citrate is 1:1, and the copper chloride and the trisodium citrate are fully mixed until the colloidal solution becomes clear;
(2) after clarification, adding penicillamine according to the molar ratio of copper chloride to penicillamine of 1:0.5-5, mixing uniformly, and immediately adding fresh 0.1M sodium borohydride solution, wherein NaBH4:CuCl2The molar ratio is 5:4, the solution color is changed into dark brown after uniform mixing, when the solution color is changed into dark red, isopropanol with the volume of 7 times is added, the reaction is stopped by centrifuging at the rotating speed of not less than 7000r/min for 6-10min, and the precipitate is resuspended in ultrapure water with the same volume after centrifuging, so that the chiral copper oxide nano particles are obtained.
The synthesis of the chiral copper oxide nano particle with phenylalanine-cysteine as ligand is as follows:
(1) adding trisodium citrate into the synthesized copper oxide precursor colloid; wherein, the molar ratio of the copper chloride to the trisodium citrate is 1:1, and the copper chloride and the trisodium citrate are fully mixed until the colloidal solution becomes clear;
(2) after clarification, adding phenylalanine-cysteine Phe-Cys into copper chloride at a molar ratio of phenylalanine-cysteine of 1:0.5-5, mixing uniformly, and immediately adding fresh 0.1M sodium borohydride solution, wherein NaBH4:CuCl2The molar ratio is 5:4, the solution color is changed into dark brown after uniform mixing, when the solution color is changed into dark red, isopropanol with the volume of 7 times is added, the reaction is stopped by centrifuging for 6-10min at the rotating speed of not less than 7000r/min, and the precipitate is resuspended in ultrapure water with the same volume after centrifuging, so that the chiral copper oxide nano particles are obtained.
Characterizing the chiral copper oxide nanoparticles: and characterizing the chiral copper oxide nano particles by one or more of a transmission electron microscope, an ultraviolet spectrometer, a circular dichroism spectrometer and a laser dynamic light scattering instrument.
Further, the transmission electron microscope with the acceleration voltage of 200 kV is used for characterizing the chiral copper oxide nano particles.
The invention has the beneficial effects that: the invention solves the problem of synthesizing the chiral copper oxide nano particles under the non-organic phase and non-hydrothermal condition and firstly synthesizes the nano-scale chiral copper oxide nano particles with regular appearance. In addition, the synthesized chiral copper oxide nano particles are very stable. Has wide biological application prospect.
Drawings
FIG. 1 is a transmission electron micrograph of chiral copper oxide nanoparticles with penicillamine as the ligand.
Figure 2 ultraviolet absorption spectrum of chiral copper oxide nanoparticles with penicillamine as ligand.
Figure 3 circular dichroism spectra of chiral copper oxide nanoparticles with penicillamine as the ligand.
FIG. 4 is a transmission electron micrograph of chiral copper oxide nanoparticles with phenylalanine-cysteine as the ligand.
FIG. 5 is a graph of the UV absorption spectrum of chiral copper oxide nanoparticles with phenylalanine-cysteine as the ligand.
FIG. 6 circular dichroism spectra of chiral copper oxide nanoparticles with phenylalanine-cysteine as ligand.
Detailed Description
Example 1 Synthesis of chiral copper oxide nanoparticles with Penicillium amine as ligand
The method comprises the following specific steps:
(1) synthesis of copper oxide precursor, first, in 5m L ultrapure water system, 3m L ultrapure water is added, then 0.2 mol/L of copper chloride (CuCl)2) Mixing with 0.1 mol/L sodium hydroxide (NaOH) solution according to the molar ratio of copper chloride to sodium hydroxide of 4:5, and uniformly mixing to obtain a copper oxide precursor;
(2) synthesis of chiral copper oxide nanoparticles with penicillamine as ligand: adding trisodium citrate into the copper oxide precursor colloid synthesized in the step (1), wherein the molar ratio of copper chloride to trisodium citrate is 1:1 (CuCl)2NaCit =1: 1), the colloidal solution gradually becomes clear after mixing uniformly, penicillamine (Pen) is added in a molar ratio of 1:1 after the clarification, and after mixing uniformly, fresh sodium borohydride solution (molar ratio: NaBH4:CuCl2=5: 4), the solution color becomes dark brown after mixing evenly, when the solution color becomes dark red, the reaction is stopped by adding isopropanol with seven times volume, centrifuging for 10min at 8000r/min, suspending the precipitate after centrifugation in ultra-large volumePure water;
(3) characterization of chiral copper oxide nanoparticles: the chiral copper oxide nanoparticles were characterized using a transmission electron microscope (acceleration voltage 200 kV) (FIG. 1). In addition, the chiral copper oxide nanoparticles are also characterized by an ultraviolet spectrometer (fig. 2), a circular dichroism spectrometer (fig. 3), a laser dynamic light scattering instrument and the like. As can be seen from the above characterization means, the monodisperse chiral copper oxide nanoparticles with regular morphology are successfully synthesized in example 1.
Example 2 Synthesis method of chiral copper oxide nanoparticles with phenylalanine-cysteine as ligand
The method comprises the following specific steps:
(1) synthesis of copper oxide precursor, first, in a 5m L ultrapure water system, 3m L ultrapure water and 0.2 mol/L copper chloride (CuCl) were added2) Mixing with 0.1 mol/L sodium hydroxide (NaOH) solution according to the molar ratio of copper chloride to sodium hydroxide of 4:5, and uniformly mixing to obtain a copper oxide precursor;
(2) synthesizing chiral copper oxide nanoparticles with phenylalanine-cysteine as ligand: adding trisodium citrate (molar ratio of copper chloride to trisodium citrate: CuCl) into the copper oxide precursor solution in the step (1)2NaCit =1: 1), the colloidal solution gradually becomes clear after mixing, phenylalanine-cysteine (Phe-Cys) is added at a molar ratio of 1:1 after clarification and mixed uniformly, and fresh sodium borohydride solution is added immediately (molar ratio: NaBH4:CuCl2=5: 4), the color of the solution is changed into dark brown after being mixed evenly, when the color of the solution is changed into dark red, the reaction is stopped by adding isopropanol with seven times of volume, centrifuging for 10min at 8000r/min, and suspending the precipitate in ultrapure water with the same volume after centrifuging;
(3) characterization of chiral copper oxide nanoparticles: the chiral copper oxide nanoparticles were characterized using a transmission electron microscope (acceleration voltage of 200 kV) (FIG. 4). In addition, the chiral copper oxide nanoparticles are also characterized by an ultraviolet spectrometer (fig. 5), a circular dichroism spectrometer (fig. 6), a laser dynamic light scattering instrument and the like. As can be seen from the above characterization means, the monodisperse chiral copper oxide nanoparticles with regular morphology are successfully synthesized in example 2.
Claims (2)
1. A method for synthesizing chiral copper oxide nano particles is characterized by comprising the following steps: under the mild condition of non-hydrothermal, copper oxide precursors are acted by a reducing agent and chiral molecules to form monodisperse nano-scale copper oxide particles, and the method mainly comprises the steps of synthesizing the copper oxide precursors and synthesizing chiral copper oxide nanoparticles with penicillamine as ligands; the preparation method comprises the following specific steps:
the synthesis of the copper oxide precursor comprises the following steps of firstly adding 3M L of ultrapure water into a 5M L ultrapure water system, mixing 0.2M copper chloride 50-200 mu L with 0.1M sodium hydroxide solution according to the molar ratio of copper chloride to sodium hydroxide of 4:5, ensuring that the pH value of the mixed solution is above 12, and uniformly mixing to obtain a copper oxide precursor colloid;
the synthesis of the chiral copper oxide nano-particle with penicillamine as ligand comprises the following steps:
(1) adding trisodium citrate into the synthesized copper oxide precursor colloid; wherein, the molar ratio of the copper chloride to the trisodium citrate is 1:1, and the copper chloride and the trisodium citrate are fully mixed until the colloidal solution becomes clear;
(2) after clarification, adding penicillamine according to the molar ratio of copper chloride to penicillamine of 1:0.5-5, mixing uniformly, and immediately adding fresh 0.1M sodium borohydride solution, wherein NaBH4:CuCl2The molar ratio is 5:4, the solution color is changed into dark brown after uniform mixing, when the solution color is changed into dark red, isopropanol with the volume of 7 times is added, the reaction is stopped by centrifuging at the rotating speed of not less than 7000r/min for 6-10min, and the precipitate is resuspended in ultrapure water with the same volume after centrifuging, so that the chiral copper oxide nano particles are obtained.
2. A method for synthesizing chiral copper oxide nano particles is characterized by comprising the following steps: under the mild condition of non-hydrothermal, forming monodisperse nano-scale copper oxide particles by the action of a reducing agent and chiral molecules on a copper oxide precursor, wherein the main steps are the synthesis of the copper oxide precursor and the synthesis of chiral copper oxide nanoparticles with phenylalanine-cysteine as a ligand; the preparation method comprises the following specific steps:
the synthesis of the copper oxide precursor comprises the following steps of firstly adding 3M L of ultrapure water into a 5M L ultrapure water system, mixing 0.2M copper chloride 50-200 mu L with 0.1M sodium hydroxide solution according to the molar ratio of copper chloride to sodium hydroxide of 4:5, ensuring that the pH value of the mixed solution is above 12, and uniformly mixing to obtain a copper oxide precursor colloid;
the synthesis of the chiral copper oxide nano-particle with phenylalanine-cysteine as ligand comprises the following steps:
(1) adding trisodium citrate into the synthesized copper oxide precursor colloid; wherein, the molar ratio of the copper chloride to the trisodium citrate is 1:1, and the copper chloride and the trisodium citrate are fully mixed until the colloidal solution becomes clear;
(2) after clarification, adding phenylalanine-cysteine Phe-Cys into copper chloride at a molar ratio of phenylalanine-cysteine of 1:0.5-5, mixing uniformly, and immediately adding fresh 0.1M sodium borohydride solution, wherein NaBH4:CuCl2The molar ratio is 5:4, the solution color is changed into dark brown after uniform mixing, when the solution color is changed into dark red, isopropanol with the volume of 7 times is added, the reaction is stopped by centrifuging for 6-10min at the rotating speed of not less than 7000r/min, and the precipitate is resuspended in ultrapure water with the same volume after centrifuging, so that the chiral copper oxide nano particles are obtained.
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| CN111257387B (en) * | 2020-02-19 | 2021-11-09 | 常州大学 | Preparation method of chiral copper oxide-glycine compound modified electrode applicable to electrochemical chiral recognition |
| CN111517359B (en) * | 2020-04-23 | 2021-08-20 | 江南大学 | Synthesis method of chiral copper sulfide super particle |
| CN111647903B (en) * | 2020-06-02 | 2022-03-29 | 金陵科技学院 | Magnetic field response three-dimensional macroporous chiral copper oxide/foamed nickel material, preparation method and application in photoelectrocatalysis |
| CN113880128A (en) * | 2020-07-01 | 2022-01-04 | 上海大学 | Copper sulfide with chiral optical activity and preparation method thereof |
| CN111994883B (en) * | 2020-09-04 | 2022-02-08 | 江南大学 | Preparation method of ordered chiral copper iron selenide nano-film with near-infrared light response |
| CN112552916A (en) * | 2020-12-29 | 2021-03-26 | 江南大学 | Synthesis method of chiral europium selenide nano particles |
| CN112608335B (en) * | 2020-12-29 | 2021-10-29 | 江南大学 | Synthesis method of chiral europium sulfide nanoparticles |
| CN116115747B (en) * | 2022-12-09 | 2023-10-27 | 江南大学 | Preparation method of chiral metal oxide immune adjuvant and vaccine based on adjuvant |
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