CN106831886A - A kind of electrochemical sensor material for detecting urea and preparation method thereof - Google Patents

A kind of electrochemical sensor material for detecting urea and preparation method thereof Download PDF

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Publication number
CN106831886A
CN106831886A CN201710181541.2A CN201710181541A CN106831886A CN 106831886 A CN106831886 A CN 106831886A CN 201710181541 A CN201710181541 A CN 201710181541A CN 106831886 A CN106831886 A CN 106831886A
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urea
electrochemical sensor
sensor material
preparation
cobalt
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CN106831886B (en
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华璐钦
李星
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Ningbo University
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Ningbo University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F15/00Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
    • C07F15/06Cobalt compounds
    • C07F15/065Cobalt compounds without a metal-carbon linkage
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13Crystalline forms, e.g. polymorphs

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  • Organic Chemistry (AREA)
  • Pyridine Compounds (AREA)

Abstract

The invention discloses a kind of electrochemical sensor material for detecting urea and preparation method thereof, the electrochemical sensor material is a kind of with the cobalt complex for determining space structure, and its chemical formula is CoC15H15N5O9, construction unit is [Co (C5HN3O6)(C10H8N2)(H2O)2]·H2O, crystallographic system is anorthic system, and space group is P 1, and cell parameter isα=90.800 °, β=102.747 °, γ=91.518 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.The preparation method of the cobalt complex is:2, the 2 ' second bipyridines with the big π keys of conjugation, 5 nitroorotic acid potassium are mixed according to a certain percentage with the cobalt ions with electro catalytic activity and is chemically reacted, a kind of cobalt complex is obtained.The preparation method is simple to operate, with low cost, is adapted to large-scale production.Obtained cobalt complex of the invention has good electro catalytic activity to urea, has potential application prospect as electrochemical sensing material.

Description

A kind of electrochemical sensor material for detecting urea and preparation method thereof
Technical field
The invention belongs to technical field of material chemistry, and in particular to a kind of electrochemical sensor material for detecting urea and its Preparation method.
Background technology
Urea (Urea), also known as phosphoamide (Carbamide), the simplest organic compound being made up of C, N, O, H One of.Also known as urea, the diamides of carbonic acid, molecular formula is H2NCONH2, it is a kind of white crystal, molecular mass 60.Urea is used as one Neutral fertilizer is planted, is also current nitrogen content highest nitrogenous fertilizer.Urea is applied to various soil and plant.It is easy to maintain, user Just, the destruction to soil is small, is a kind of larger chemical nitrogen fertilizer of current usage amount.Industrial ammonia and carbon dioxide exist Certain condition urea synthesis.
Biology is with the chemical substance urea synthesis such as carbon dioxide, water, aspartic acid and ammonia.Promote the metabolism of urea synthesizing on the way Footpath is a kind of anabolism, is called urea cycle, and also known as " ornithine circulation ", this process expends energy, but very necessary.Because containing Nitrogenous wastes has toxicity, and is common metabolism product, it is necessary to be eliminated.Urea cycle is mammal and amphibian Drain the main path of nitrogenous metabolic waste.
Urea is the main nitrogenous end-product of mammal and some fish vivo protein metabolic breakdowns.Urea is in liver Blood (concentration in human body is in 2.5-7.5 μm of ol/L) is incorporated after generation, finally by kidney by urine ejection, a small amount of urea is by sweat Discharge.Contain urea in the urine of mammal, amphibian and some fishes.
Detect that the content of internal urea can be with anticipation human health status, or assisted diagnosis some diseases.Urea is due to dividing Son amount is small, and dissolving is easy to again, and extension is very big, therefore the urea concentration basic in cerebrospinal fluid, dropsy of serous cavity, saliva, sweat Cause.Plasma wrea concentration is mainly influenceed by renal function and protein intake and catabolism situation.Acute renal failure, chronic renal Inflammation, renal arteriosclerosis, chronic pyelonephritis, nephrophthisis, kidney neoplasms late period etc., when renal function is slightly damaged, urea can be caused to contain Amount increases, and to renal failure, especially uremia diagnosis has special value, and can determine whether the state of an illness.Therefore, to the quick of urea Effective detection seems great meaning.
Current clinical labororatory determines urea most common method has diacetyl-oxime method, neutralization titration, enzyme coupling ultraviolet AAS and o-phthalaldehyde method.Report about Electrochemical Detection urea is very few.Electrochemical analysis detection have it is simple, Fast, the advantages of sensitivity is high, causes the great interest of people in recent years.
The present invention, by simple hydro-thermal reaction, is prepared for one kind with cobalt acetate, bipyridyl and nitroorotic acid as raw material Cobalt complex, the compound has good electro catalytic activity to urea, can be as the modification material of chemical electrode Material, processability is excellent, detect quick electrochemical sensor etc..Cobalt compound prepared by the present invention is used as detection urea Electrochemical sensor material, has potential application prospect in electro-catalysis sensing detection urea.
The content of the invention
The technical problems to be solved by the invention are directed to prior art, there is provided a kind of electrochemistry for detecting urea is passed Sensor material and preparation method thereof.
The present invention is for the solution technical scheme taken of above-mentioned technical problem:A kind of electrochemistry for detecting urea is passed Sensor material, the electrochemical sensor material is a kind of cobalt complex (abbreviation complex), and the complex has what is determined Space structure, construction unit is [Co (C5HN3O6)(C10H8N2)(H2O)2]·H2O, its chemical formula is CoC15H15N5O9, crystallographic system is Anorthic system, space group is P-1, and cell parameter is α= 90.800 °, β=102.747 °, γ=91.518 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.
A kind of above-mentioned preparation method for detecting the electrochemical sensor material of urea, comprises the following steps:
(1) to adding appropriate 5- nitroorotic acid potassium monohydrate, 2,2 '-bigeminy pyrrole in 25mL polytetrafluoroethyllining linings Pyridine and hydration cobalt acetate, are subsequently adding 8~15mL of distilled water, stir, and obtain reactant mixture;
(2) above-mentioned polytetrafluoroethyllining lining is sealed, is put into stainless steel cauldron, stainless steel cauldron is put into baking oven In, then 100~125 DEG C of 48~72h of heating response naturally cool to room temperature, open reactor and obtain brown color bulk crystals;
(3) brown color bulk crystals are taken out, natural air drying, obtains final product described electrochemical sensor material.
Preferably, it is described participate in reaction material be chemistry it is pure, it is described hydration cobalt acetate be four hydration cobalt acetates.
It is preferred that the mol ratio of the 5- nitroorotic acids potassium monohydrate, 2,2 '-second bipyridine and hydration cobalt acetate is 1: 1: 1~1.5.
Compared with prior art, the advantage of the invention is that:
With conjugatedπbond 2,2 '-second bipyridine, nitroorotic acid and the cobalt ions with electrochemical catalysis activity are entered Row chemical reaction, is obtained new bipyridyl, nitroorotic acid cobalt complex, and the compound has as electro catalytic activity material There are accurate space structure (Fig. 1) and accurate molecular formula;Cobalt ions can utilize 3d tracks that the coordination of stabilization is formed with part Key, is conducive to electronics to transmit, and promotes the carrying out of electrochemical reaction, so as to present have good electro catalytic activity to urea. Prepared cobalt complex has potential application prospect as electro-catalysis chemical sensor material.
Brief description of the drawings
Fig. 1 is 2,2 '-second bipyridine of the invention, the construction unit figure of 5- nitroorotic acid cobalt complexes;
Fig. 2 is 2,2 '-second bipyridine of the invention, 5- nitroorotic acids cobalt complex to urea electrochemical catalysis response diagram (a:Naked glass electrode, b:Glass electrode after complex decorating, c:Glass electrode after complex decorating and to add urea molten Liquid).
Specific embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment 1:
To in 25mL polytetrafluoroethyllining linings add 5- nitroorotic acid potassium monohydrate (0.5mmol, 0.1286g), 2, 2 '-second bipyridine (0.5mmol, 0.0781g), and Co (Ac)2·4H2O (0.5mmol, 0.1245g), and add distilled water 15mL, Stirring, obtains reactant mixture;Polytetrafluoroethyllining lining is sealed, is put into stainless steel cauldron, stainless steel cauldron is put into In baking oven, then 100 DEG C of heating response 72h naturally cool to room temperature, open reactor and obtain brown color bulk crystals;Take out brilliant Body, natural air drying obtains final product described cobalt complex.
Embodiment 2:
To in 25mL polytetrafluoroethyllining linings add 5- nitroorotic acid potassium monohydrate (0.1mmol, 0.0257g), 2, 2 '-second bipyridine (0.1mmol, 0.0156g), and Co (Ac)2·4H2O (0.15mmol, 0.0374g), and add distilled water 8mL, Stirring, obtains reactant mixture;Polytetrafluoroethyllining lining is sealed, is put into stainless steel cauldron, stainless steel cauldron is put into In baking oven, then 125 DEG C of heating response 48h naturally cool to room temperature, open reactor and obtain brown color bulk crystals;Take out brilliant Body, natural air drying obtains final product described cobalt complex.
Embodiment 3:
To in 25mL polytetrafluoroethyllining linings add 5- nitroorotic acid potassium monohydrate (0.2mmol, 0.0514g), 2, 2 '-second bipyridine (0.2mmol, 0.0216g), and Co (Ac)2·4H2O (0.25mmol, 0.0623g), and add distilled water 10mL, Stirring, obtains reactant mixture;Polytetrafluoroethyllining lining is sealed, is put into stainless steel cauldron, stainless steel cauldron is put into In baking oven, then 115 DEG C of heating response 60h naturally cool to room temperature, open reactor and obtain brown color bulk crystals;Take out brilliant Body, natural air drying obtains final product described cobalt complex.
Tan crystals obtained in embodiment 1-3 are carried out into structured testing with Single Crystal X-ray, as a result shows that the brown color is brilliant Body is cobalt complex, its construction unit as shown in figure 1, its molecular formula is CoC15H15N5O9, construction unit is [Co (C5HN3O6)(C10H8N2)(H2O)2]·H2O, crystallographic system is anorthic system, and space group is P-1, and cell parameter isα=90.800 °, β=102.747 °, γ=91.518 °, cobalt ions It is the octahedra geometric configuration of hexa-coordinate.
By obtained cobalt complex CoC15H15N5O9Electrocatalysis characteristic test is carried out to urea, the change is as a result shown Compound has good electro-catalysis response performance (such as Fig. 2) to urea.

Claims (4)

1. a kind of electrochemical sensor material for detecting urea, it is characterised in that the electrochemical sensor material is a kind of With the cobalt complex for determining space structure, its chemical formula is CoC15H15N5O9, construction unit is [Co (C5HN3O6) (C10H8N2)(H2O)2]·H2O, crystallographic system is anorthic system, and space group is P-1, and cell parameter isα=90.800 °, β=102.747 °, γ=91.518 °, cobalt ions It is the octahedra geometric configuration of hexa-coordinate.
2. a kind of preparation method of the as claimed in claim 1 electrochemical sensor material for being used to detect urea, its feature exists In comprising the following steps:
(1) to added in 25mL polytetrafluoroethyllining linings appropriate 5- nitroorotic acid potassium monohydrate, 2,2 '-second bipyridine and Hydration cobalt acetate, is subsequently adding 8~15mL of distilled water, stirs, and obtains reactant mixture;
(2) above-mentioned polytetrafluoroethyllining lining is sealed, is put into stainless steel cauldron, stainless steel cauldron is put into baking oven, 100~125 DEG C of 48~72h of heating response, then naturally cool to room temperature, open reactor and obtain brown color bulk crystals;
(3) brown color bulk crystals are taken out, natural air drying, obtains final product described electrochemical sensor material.
3. the preparation method for detecting the electrochemical sensor material of urea according to claim 2, it is characterised in that The mol ratio of the 5- nitroorotic acids potassium monohydrate, 2,2 '-second bipyridine and hydration cobalt acetate is 1: 1: 1~1.5.
4. the preparation method for detecting the electrochemical sensor material of urea according to claim 2, it is characterised in that It is described participate in reaction material be chemistry it is pure, it is described hydration cobalt acetate be four hydration cobalt acetates.
CN201710181541.2A 2017-03-24 2017-03-24 A kind of electrochemical sensor material and preparation method thereof for detecting urea Active CN106831886B (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103435659A (en) * 2013-08-12 2013-12-11 宁波大学 Cobalt complex with electrochemical catalytic activity

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103435659A (en) * 2013-08-12 2013-12-11 宁波大学 Cobalt complex with electrochemical catalytic activity

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
M. JOHN PLATER等,: "Hydrothermal crystallisation of metal (II) orotates(M_/nickel,cobalt, manganese or zinc). Effect of 2,2-bipyridyl, 2,2-dipyridyl amine, 1-methyl-3-(2-pyridyl)pyrazole, phenanthroline and 2,9-Dimethyl -1,10-phenanthroline upon structure", 《INORGANICA CHIMICA ACTA》 *

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