CN104402944A - Neodymium-copper-glutamic acid-imidazole monocrystal complex and preparation method thereof - Google Patents
Neodymium-copper-glutamic acid-imidazole monocrystal complex and preparation method thereof Download PDFInfo
- Publication number
- CN104402944A CN104402944A CN201410646356.2A CN201410646356A CN104402944A CN 104402944 A CN104402944 A CN 104402944A CN 201410646356 A CN201410646356 A CN 201410646356A CN 104402944 A CN104402944 A CN 104402944A
- Authority
- CN
- China
- Prior art keywords
- neodymium
- copper
- glutamic acid
- imidazoles
- title complex
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a neodymium-copper-glutamic acid-imidazole monocrystal complex and a preparation method thereof, and the complex is composed of a rare earth metal neodymium, a transition metal copper, an amino acid glutamic acid and imidazole. The preparation process of the complex comprises: firstly respectively reacting neodymium oxide and copper oxide with perchloric acid to prepare a neodymium perchlorate solution and a copper perchlorate solution, mixing the two solutions and reacting at 40-80 DEG C for 1-10 h, then adding glutamic acid, using an alkali solution to adjust the pH to be 4-8, then reacting at 40-80 DEG C for 1-10 h, and then adding imidazole, reacting at 40-80 DEG C for 1-10 h, and putting for a period for obtain the crystal. The technology is simple, the ligand selection is scientific, the synthesized rare-earth amino acid monocrystal complex is definite and novel in structure, the monocrystal structure also provides a new basis scientific basis for a crystal database, and the complex has relatively strong fluorescent property.
Description
Technical field
The present invention relates to a kind of rare-earth transition metal amino acid monocrystalline title complex, relate in particular to neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex and preparation method thereof; Belong to technical field of material.
Background technology
The research of Rare Earth-Amino Acid Complexes is long-standing.Along with the continuous expansion of rare earth in agricultural, medical science and biomolecules research application, cause the extensive entered environment of rare earth, and entered in organism by number of ways.Rare earth has many biochemical functions, the biological effect that it causes and biochemical change are diversified, it can produce restraining effect to effect multiple in organism, affect the biological activity of various enzyme, metabolism of fat and nucleic acid to exchange, high concentration rare earth is understood lesion wire Mitochondria Membrane and causes oxidative chain disorderly.For this reason, people urgently wish biological action and the remote effect in vivo thereof of understanding rare earth.
Comprise many biogenic metallic elements in transition metal, known that most transition metal all has good ligancy, and carry out Gospel for mankind's health care belt.Title complex as platinum has significant antitumour activity, the complex salt of gold can treat rheumatic arthritis, and copper, iron oxine title complex there is anti-microbial activity etc., to deep understanding and the grasp of these concerns about bio inorganic chemistry rules, wholesome effect will be produced to the development of medical science and life science.In addition, in the last few years, find that rare earth has broad application prospects in medical, it had blood coagulation resisting function, and can be used for preventing and treating thrombus disease, sterilizing ability is strong, and toxic side effect is little, and easy cleaning is not infected with skin, can be used as burn medicine.Large quantity research shows, but light rare earths has cancer protective effect on cancer risk.
Amino acid is a large amount of class bio-ligand existed in organism, be the basic structural unit of protein, enzyme etc., research rare earth and transition metal and amino acid whose interaction are by for exploring the metabolism in vivo of rare earth and transition metal and biological effect provides basic.For this reason, in recent years, the research of rare earth and transition metal amino acid coordination compound is always by people are paid attention to, and development rapidly especially nearly ten years.After rare earth ion enters organism the various effects that play all relate to rare earth and protein, the effect of the biomacromolecules such as enzyme, amino acid, peptide are the essentially consist unit of various biomacromolecule in human body; And rare earth element and transition metal have visibly different out-shell electron configuration, make rare earth ion when with various dissimilar ligands, present colourful coordination behavior and crystalline structure.Therefore the research of the bio-molecular interaction such as rare earth and amino acid, peptide, protein has attracted domestic and international large quantities of researcher, but is also in blank for research and development such as Rare Earth Amino-Acid monocrystalline title complexs at present.
Summary of the invention
The present invention is directed to above-mentioned problems of the prior art, a kind of rare-earth transition metal amino acid monocrystalline title complex is provided, solve in prior art and be also in blank problem.
Another object of the present invention is the preparation method providing a kind of rare-earth transition metal amino acid monocrystalline title complex.
Technical scheme of the present invention is as follows:
A kind of rare-earth transition metal amino acid monocrystalline title complex, by rear earth element nd, transition metal copper, L-glutamic acid and imidazoles composition; Its crystal is trigonal system, and spacer is R3, and unit cell parameters is a=b=15.8830, c=23.491, α=β=90 °, γ=120 °, V=5132.1 (8)
3, Z=3.
The preparation method of rare-earth transition metal amino acid monocrystalline title complex, comprises the steps:
First Neodymium trioxide and cupric oxide and perchloric acid are reacted and be mixed with the neodymium perchlorate of 0.1 ~ 1 M and the solution of cupric perchlorate, according to neodymium: the mixed in molar ratio of copper=1:3 ~ 1:9, L-glutamic acid is added at 40 ~ 80 DEG C of reaction 1 ~ 10 h, mol ratio neodymium: L-glutamic acid=1:3 ~ 1:9, adjust at 40 ~ 80 DEG C of reaction 1 ~ 10 h after the value of pH=4 ~ 8 with alkaline solution, then add imidazoles, mol ratio neodymium: imidazoles=1:3 ~ 1:9, after 40 ~ 80 DEG C of reaction 1 ~ 10 h, placement for some time obtains crystal.
Described neodymium perchlorate and the compound method of cupric perchlorate comprise the steps, take Neodymium trioxide or cupric oxide 10.00 g, add high chloro acid solution 40 ~ 50 mL of volume ratio 1:1, filter out insolubles, be settled to 250 mL, then be 0.1 ~ 1 M by the concentration of volumetry demarcation neodymium perchlorate or cupric perchlorate solution.
The concentration of described neodymium perchlorate or cupric perchlorate solution is preferably 0.4 ~ 0.6 M.
Molar ratio in described neodymium, copper, L-glutamic acid, imidazoles preparation process, neodymium: copper: L-glutamic acid: imidazoles=1:5 ~ 7:5 ~ 7:5 ~ 7.
Described title complex temperature of reaction is 50 ~ 70 DEG C.
The described title complex reaction times is 1 ~ 10 h, is preferably 3 ~ 7 h.
In the preparation process of described title complex, adjust ph is 5 ~ 7.
In a word, method disclosed by the invention has following advantage: simple process, part selects science, the Rare Earth Amino-Acid monocrystalline complex structure of synthesis is clear and definite, novel, its single crystal structure is also simultaneously for crystal data storehouse provides new basic science foundation, and this title complex of fluorescence spectrum spectrogram result has stronger photoluminescent property.
Accompanying drawing explanation
Fig. 1 is the single cell structure figure of the rare-earth transition metal amino acid coordination compound monocrystalline obtained according to preparation method of the present invention.
Fig. 2 is the packed structures figure of the rare-earth transition metal amino acid coordination compound monocrystalline obtained according to preparation method of the present invention.
Fig. 3 is the rare-earth transition metal amino acid coordination compound monocrystalline fluorescence spectrum figure obtained according to preparation method of the present invention.
Embodiment
Embodiment 1
The preparation of neodymium perchlorate solution: take Neodymium trioxide 10.00 g, adds the high chloro acid solution 40 ~ 50mL of volume ratio 1:1, filters out insolubles, be settled to 250 mL, demarcates its concentration with the EDTA standardized solution demarcated; The concentration of neodymium perchlorate solution is 0.4 ~ 0.6 M.
The preparation of cupric perchlorate solution: take cupric oxide 10.00 g, adds high chloro acid solution 40 ~ 50 mL of volume ratio 1:1, filters out insolubles, be settled to 250 mL, demarcate its concentration with the Zn standardized solution demarcated; The concentration of cupric perchlorate solution is 0.4 ~ 0.6 M.
The preparation of title complex: according to neodymium: the mixed in molar ratio of copper=1:6, by above-mentioned cupric perchlorate solution and the mixing of neodymium perchlorate solution, after 60 DEG C of reaction 5 h, with mol ratio neodymium: L-glutamic acid=1:6 adds L-glutamic acid, adjust at 60 DEG C of reaction 3 h after the value of pH=4 ~ 8 with alkaline solution, then add imidazoles, mol ratio neodymium: imidazoles=1:6, after 60 DEG C of reaction 3 h, after placing for some time, obtain crystal; Its crystal is trigonal system, and spacer is R3, and unit cell parameters is a=b=15.8830, c=23.491, α=β=90 °, γ=120 °, V=5132.1 (8)
3, Z=3.
The mensuration of title complex: get complex monocrystal obtained above, adopt following methods to measure its structure cell, the crystallographic data Bruker Smart-1000 CCD single crystal diffractometer of title complex is collected, and adopts Mo Ka ray, wavelength is 0.071073 nm, collected at room temperature data.All calculating all uses SHELXTL-97 program to complete, and the crystallographic data of title complex is in table 1 and table 2.
embodiment 2
First Neodymium trioxide and cupric oxide and perchloric acid are reacted and be mixed with the neodymium perchlorate of 0.1 M and the solution of cupric perchlorate, according to neodymium: the mixed in molar ratio of copper=1:3, L-glutamic acid is added at 40 DEG C of reaction 10 h, mol ratio neodymium: L-glutamic acid=1:3, react 10 h with after alkaline solution adjustment pH=4 value at 40 DEG C, then add imidazoles, mol ratio neodymium: imidazoles=1:3, after 40 DEG C of reaction 10 h, placement for some time obtains crystal.Other step is with embodiment 1.
embodiment 3
First Neodymium trioxide and cupric oxide and perchloric acid are reacted and be mixed with the neodymium perchlorate of 1 M and the solution of cupric perchlorate, according to neodymium: the mixed in molar ratio of copper=1:9, L-glutamic acid is added at 80 DEG C of reaction 1 h, mol ratio neodymium: L-glutamic acid=1:9, react 1 h with after alkaline solution adjustment pH=8 value at 80 DEG C, then add imidazoles, mol ratio neodymium: imidazoles=1:9, after 80 DEG C of reaction 1 h, placement for some time obtains crystal.Other step is with embodiment 1.
embodiment 4
First Neodymium trioxide and cupric oxide and perchloric acid are reacted the solution of neodymium perchlorate and the 0.6M cupric perchlorate being mixed with 0.4M, according to neodymium: the mixed in molar ratio of copper=1:5, L-glutamic acid is added at 50 DEG C of reaction 7 h, mol ratio neodymium: L-glutamic acid=1:7, react 3h with after alkaline solution adjustment pH=5 value at 70 DEG C, then add imidazoles, mol ratio neodymium: imidazoles=1:5, after 60 DEG C of reaction 4 h, placement for some time obtains crystal.Other step is with embodiment 1.
embodiment 5
First Neodymium trioxide and cupric oxide and perchloric acid are reacted and be mixed with the neodymium perchlorate of 0.5M and the solution of cupric perchlorate, according to neodymium: the mixed in molar ratio of copper=1:7, L-glutamic acid is added at 70 DEG C of reaction 5h, mol ratio neodymium: L-glutamic acid=1:5, react 7 h with after alkaline solution adjustment pH=8 value at 50 DEG C, then add imidazoles, mol ratio neodymium: imidazoles=1:7, after 50 DEG C of reaction 6 h, placement for some time obtains crystal.Other step is with embodiment 1.
embodiment 6
First Neodymium trioxide and cupric oxide and perchloric acid are reacted the solution of neodymium perchlorate and the 0.2M cupric perchlorate being mixed with 0.8M, according to neodymium: the mixed in molar ratio of copper=1:4, L-glutamic acid is added at 60 DEG C of reaction 6h, mol ratio neodymium: L-glutamic acid=1:8, react 6 h with after alkaline solution adjustment pH=6 value at 60 DEG C, then add imidazoles, mol ratio neodymium: imidazoles=1:8, after 70 DEG C of reaction 5 h, placement for some time obtains crystal.
Above about specific descriptions of the present invention, be only not limited to the technical scheme described by the embodiment of the present invention for illustration of the present invention.Those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent replacement, to reach identical technique effect.Needs are used, all in protection scope of the present invention as long as meet.
Claims (8)
1. neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex, is characterized in that by rear earth element nd, transition metal copper, L-glutamic acid and imidazoles composition; Its crystal is trigonal system, and spacer is R3, and unit cell parameters is a=b=15.8830, c=23.491, α=β=90 °, γ=120 °, V=5132.1 (8)
3, Z=3.
2. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 1, is characterized in that comprising the steps:
First Neodymium trioxide and cupric oxide and perchloric acid are reacted and be mixed with the neodymium perchlorate of 0.1 ~ 1 M and the solution of cupric perchlorate, according to neodymium: the mixed in molar ratio of copper=1:3 ~ 1:9, L-glutamic acid is added at 40 ~ 80 DEG C of reaction 1 ~ 10 h, mol ratio neodymium: L-glutamic acid=1:3 ~ 1:9, adjust at 40 ~ 80 DEG C of reaction 1 ~ 10 h after the value of pH=4 ~ 8 with alkaline solution, then add imidazoles, mol ratio neodymium: imidazoles=1:3 ~ 1:9, after 40 ~ 80 DEG C of reaction 1 ~ 10 h, placement for some time obtains crystal.
3. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 2, it is characterized in that the compound method of described neodymium perchlorate and cupric perchlorate comprises the steps, take Neodymium trioxide or cupric oxide 10.00 g, add high chloro acid solution 40 ~ 50 mL of volume ratio 1:1, filter out insolubles, be settled to 250 mL, then be 0.1 ~ 1 M by the concentration of volumetry demarcation neodymium perchlorate or cupric perchlorate solution.
4. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 2, is characterized in that the concentration of described neodymium perchlorate or cupric perchlorate solution is preferably 0.4 ~ 0.6 M.
5. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 2, is characterized in that the molar ratio in described neodymium, copper, L-glutamic acid, imidazoles preparation process, neodymium: copper: L-glutamic acid: imidazoles=1:5 ~ 7:5 ~ 7:5 ~ 7.
6. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 2, is characterized in that described title complex temperature of reaction is 50 ~ 70 DEG C.
7. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 2, is characterized in that the described title complex reaction times is 3 ~ 7 h.
8. the preparation method of neodymium-copper-L-glutamic acid-imidazoles monocrystalline title complex according to claim 2, is characterized in that in the preparation process of described title complex, adjust ph is 5 ~ 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410646356.2A CN104402944A (en) | 2014-11-15 | 2014-11-15 | Neodymium-copper-glutamic acid-imidazole monocrystal complex and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410646356.2A CN104402944A (en) | 2014-11-15 | 2014-11-15 | Neodymium-copper-glutamic acid-imidazole monocrystal complex and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104402944A true CN104402944A (en) | 2015-03-11 |
Family
ID=52640623
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410646356.2A Pending CN104402944A (en) | 2014-11-15 | 2014-11-15 | Neodymium-copper-glutamic acid-imidazole monocrystal complex and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104402944A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294744A (en) * | 2015-10-20 | 2016-02-03 | 辽宁石油化工大学 | Energy-containing fluorescent material rare earth-glutamic acid-imidazole single crystal complex and preparation method thereof |
| CN106854169A (en) * | 2016-12-30 | 2017-06-16 | 山东大学 | A kind of amino-acid rare earth coordinates high-efficiency fluorescence powder and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031096A (en) * | 2014-06-27 | 2014-09-10 | 广西师范大学 | Isobutanolamine copper and rare earth 6-heteronuclear metal cluster and synthesis method thereof |
| CN104098612A (en) * | 2014-07-01 | 2014-10-15 | 天津师范大学 | 3d-4f heteronuclear metal magnetic complex and preparing method and application thereof |
-
2014
- 2014-11-15 CN CN201410646356.2A patent/CN104402944A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031096A (en) * | 2014-06-27 | 2014-09-10 | 广西师范大学 | Isobutanolamine copper and rare earth 6-heteronuclear metal cluster and synthesis method thereof |
| CN104098612A (en) * | 2014-07-01 | 2014-10-15 | 天津师范大学 | 3d-4f heteronuclear metal magnetic complex and preparing method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| WEN-XIN DU等，: "Syntheses and crystal structures of a series of heptanuclear trigonal prismatic clusters {LnCu6} (Ln=La, Sm, Er) with glycine and imidazole as ligands", 《JOURNAL OF MOLECULAR STRUCTURE》 * |
| 吕雪川，: "稀土氨基酸配合物的合成和热化学性质研究", 《中国科学院研究生院博士学位论文》 * |
| 吕雪川等，: "新型镧三元配合物La(Glu)(Im)6(C104)3·4HCl04·4H20的合成和热化学性质", 《物理化学学报》 * |
| 高肖汉等，: "金属-有机配合物[LaCu6(μ-OH)3(GlY)6Im6](ClO4)6", 《功能材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294744A (en) * | 2015-10-20 | 2016-02-03 | 辽宁石油化工大学 | Energy-containing fluorescent material rare earth-glutamic acid-imidazole single crystal complex and preparation method thereof |
| CN106854169A (en) * | 2016-12-30 | 2017-06-16 | 山东大学 | A kind of amino-acid rare earth coordinates high-efficiency fluorescence powder and preparation method thereof |
| CN106854169B (en) * | 2016-12-30 | 2018-10-09 | 山东大学 | A kind of amino acid-rare earth cooperation high-efficiency fluorescence powder and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102795938B (en) | High-efficiency multielement compound foliage selenium fertilizer and preparation technique thereof | |
| CN113730614B (en) | Lutetium marked nano carrier and preparation method thereof | |
| Fettweis et al. | Lysimeter experiments on the translocation of the carbon-14-labelled nitrification inhibitor 3, 4-dimethylpyrazole phosphate (DMPP) in a gleyic cambisol | |
| CN104402944A (en) | Neodymium-copper-glutamic acid-imidazole monocrystal complex and preparation method thereof | |
| Xing et al. | Environmental impacts of metal and other inorganics on soil and groundwater in China | |
| CN101811902A (en) | Manufacturing process of multifunctional enriched-selenium plant nutrient | |
| Jianmin et al. | Synthesis, crystal and molecular structure of Cd2 (sacch) 4 (Im) 4 | |
| CN105294744A (en) | Energy-containing fluorescent material rare earth-glutamic acid-imidazole single crystal complex and preparation method thereof | |
| CN103936772A (en) | Preparation method of binuclear copper complex with anti-tumor activity | |
| KR101456538B1 (en) | Method for producing ion water containing germanium ion | |
| CN101019555B (en) | Ternary RE-amino acid-vitamin complex as plant growth regulator and its preparation | |
| Patel et al. | Synthesis, characterization, and superoxide dismutase activity of copper (II) complexes with bidentate ligands | |
| CN103143000B (en) | Recombinant human interferon alpha2b preparation | |
| Hoffmann et al. | The Crystal Structure and Magnetic Behavior of [Cu2 (dien) 2CI2](CIO4) 2 | |
| CN104671960A (en) | Amino acid microbial fertilizer | |
| CN101019602A (en) | Composite fertilizer for selenium-rich freshwater pearl | |
| CN103910549B (en) | For solving nutritive medium and the application process thereof of solanaceous vegetables crop fruiting period calcium deficiency | |
| CN101735160A (en) | 4-amino-3,5-bi(mercapto-methyl)-1,2,4-tolyltriazole compound and synthesizing method thereof | |
| Aslanidou et al. | Nutrients Use Efficiency in Coupled and Decoupled Aquaponic Systems | |
| Liu et al. | Synthesis and structures of nine-coordinate K [Dy (Edta)(H2O) 3]· 3.5 H2O,(NH4) 3 [Dy (Ttha)]· 5H2O, and eight-coordinate NH4 [Dy (Cydta)(H2O) 2]· 4.5 H2O complexes | |
| CN102976838A (en) | Nutrient solution for water culture of capsella bursa-pastoris | |
| CN103320387A (en) | Method for establishing mice transplantable breast cancer experimental pulmonary metastasis model | |
| Daugherty et al. | Studies on nitrosamine metabolism I. Subcellular distribution of radioactivity in tumor-susceptible tissues of RFM mice following administration of [14C] dimethylnitrosamine | |
| CN104961802A (en) | Active peptide for treating cancer and application of active peptide | |
| Doni et al. | Zeolite and Winery Waste as Innovative By-Product for Vineyard Soil Management |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150311 |
|
| RJ01 | Rejection of invention patent application after publication |