CN106928153A - A kind of PARA FORMALDEHYDE PRILLS(91,95) has cobalt complex of electro catalytic activity and preparation method thereof - Google Patents
A kind of PARA FORMALDEHYDE PRILLS(91,95) has cobalt complex of electro catalytic activity and preparation method thereof Download PDFInfo
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- CN106928153A CN106928153A CN201710181530.4A CN201710181530A CN106928153A CN 106928153 A CN106928153 A CN 106928153A CN 201710181530 A CN201710181530 A CN 201710181530A CN 106928153 A CN106928153 A CN 106928153A
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- cobalt complex
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- formaldehyde prills
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
- C07D239/52—Two oxygen atoms
- C07D239/54—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals
- C07D239/545—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals with other hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/553—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals with other hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms with halogen atoms or nitro radicals directly attached to ring carbon atoms, e.g. fluorouracil
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1815—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
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- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
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Abstract
There is cobalt complex of electro catalytic activity and preparation method thereof the invention discloses a kind of PARA FORMALDEHYDE PRILLS(91,95), the cobalt complex is a kind of electrocatalysis material with exact space structure, its chemical formula is CoC8H12N6O12, construction unit is [Co (C4H2N3O4)2(H2O)4], crystallographic system is anorthic system, and space group is P 1, and cell parameter is α=97.141 °, β=108.592 °, γ=115.555 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.There is the PARA FORMALDEHYDE PRILLS(91,95) preparation method of the cobalt complex of electro catalytic activity to be：5 nitroorotic acid potassium monohydrates are chemically reacted with the cobalt ions with electro catalytic activity, a kind of cobalt complex is obtained.The preparation method is simple to operate, with low cost, is adapted to large-scale production.Cobalt complex PARA FORMALDEHYDE PRILLS(91,95) obtained by the present invention has good electro catalytic activity, has potential application prospect as electrocatalysis material.
Description
Technical field
The invention belongs to technical field of material chemistry, and in particular to a kind of PARA FORMALDEHYDE PRILLS(91,95) have electro catalytic activity cobalt complex and its
Preparation method.
Background technology
Electro-catalysis is a kind of catalytic action that can speed up the charge transfer reaction on electrode and electrolyte interface.Electro-catalysis
Effect includes two aspects of electrode reaction and catalytic action, therefore elctro-catalyst must simultaneously have both functions：One can lead
Electricity and ratio relatively freely transmit electronics；Two can carry out effective catalytic activation effect to substrate.Current electro-catalysis is mainly used in
The electro-catalysis treatment of sewage；The Electrocatalysis Degradation of chromate waste water；The electrolytic desulfurization of flue gas and feed coal；Electro-catalysis is removed simultaneously
NOxAnd SO2；The aspects such as the electroreduction of carbon dioxide.From suitable electrode material, the speed of electrode reaction can be accelerated.It is real
Test result of study and show that some transistion metal compounds or complex PARA FORMALDEHYDE PRILLS(91,95) or hydrogen peroxide have good electro catalytic activity,
For example, Ran Fanmin etc. discloses a kind of PARA FORMALDEHYDE PRILLS(91,95) has compound of electrochemical response and preparation method thereof, grant number CN
103396458B；Zhao Yayun etc. discloses a kind of cobalt complex to hydrogen peroxide with electro catalytic activity, grant number：
CN103467367B；Lee's magnitude disclose it is a kind of there is copper complex of electro catalytic activity and preparation method thereof to hydrogen peroxide,
Grant number：CN 103467498B.There is good electrocatalysis characteristic based on some transistion metal compounds, can be repaiied as electrode
Exterior material is fabricated to sensor for detecting some toxic and harmfuls.
Formaldehyde is largely distributed as a kind of important Organic Ingredients in material, is a kind of the primary of destruction cell protein
Skin, respiratory tract and internal organ can all be caused damage by matter poisonous substance, anaesthetize nervous centralis, cause pulmonary edema, kidney failure etc..At present
Analysis Methods for Formaldehyde mainly has AAS, electrochemical assay, liquid chromatography, sensor method etc..For example use Raman
Spectral detection formaldehyde (Zhang Qianxuan, Guan Xuchun, Cui Houxin, a kind of apparatus and method of formaldehyde examination, application publication number CN
102749318), the method operation, analysis are excessively complicated.Also use method (Liu Dongfang, ginger of heat sensing nature examination formaldehyde
Wind, Ma Xiaocong, formaldehyde gas sensor, application publication number CN 101825604A), when the method is used, heating electrode group is necessary
Gas sensing layer is heated into very high temperature (300 DEG C) could normally detect, power consumption is big, and security is poor.
The present invention discloses a kind of PARA FORMALDEHYDE PRILLS(91,95) has the compound of electro catalytic activity, can be used as electrode modified material, preparative
Can be stable, can be used to prepare electrochemical sensor of Rapid Detection of Formaldehyde etc..Compound prepared by the present invention is cobalt complex,
Its PARA FORMALDEHYDE PRILLS(91,95) has good electro catalytic activity, has potential application prospect in electro-catalysis sensing detection.
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 reaction condition is gentle, preparation process
Simply, with low cost, PARA FORMALDEHYDE PRILLS(91,95) has cobalt complex of electro catalytic activity and preparation method thereof.
The present invention is for the solution technical scheme taken of above-mentioned technical problem：The cobalt that a kind of PARA FORMALDEHYDE PRILLS(91,95) has electro catalytic activity is matched somebody with somebody
Position compound (abbreviation complex), the complex has certain space structure, and its construction unit is [Co (C4H2N3O4)2(H2O)4], its chemistry
Formula is CoC8H12N6O12, crystallographic system is anorthic system, and space group is P-1, and cell parameter is
α=97.141 °, β=108.592 °, γ=115.555 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.
A kind of above-mentioned PARA FORMALDEHYDE PRILLS(91,95) has the preparation method of the cobalt complex of electro catalytic activity, comprises the following steps：
(1) a certain amount of hydration cobaltous dichloride and 5- nitroorotic acid potassium monohydrates are weighed, is placed in beaker, according to Co
(II) ion and the ratio of the amount of substance of 5- nitroorotic acid potassium are 1:1~2 ratio is added, and add water 10~15mL, and heat, stir
Mixing dissolves it, obtains reacting mixture solution；
(2) above-mentioned reacting mixture solution is transferred into 25mL has the stainless steel cauldron of polytetrafluoroethyllining lining
In, it is placed in air dry oven after sealed reactor, 100~120 DEG C of heating responses 24~72 hours, reaction end is cooled to room
Temperature, opens reactor and obtains brownish red bulk crystals；
(3) brownish red bulk crystals are taken out, natural air drying, obtains final product described cobalt complex.
Preferably, it is described participate in reaction material be chemistry it is pure, it is described hydration cobaltous dichloride be six hydration cobaltous dichlorides.
Compared with prior art, the advantage of the invention is that：
The nitroorotic acid that will be conjugated with rigid plane carries out hydro-thermal with the cobalt ions with electrochemical catalysis activity
Reaction is learned, the carboxyl of 5- nitroorotic acids is sloughed in the reaction, and be coordinated with cobalt ions using its nitrogen, form new cobalt coordinationization
Compound, its construction unit has rigid conjugate property, is conducive to electron transition and energy transmission, so that compound has well
Photoelectric activity so that PARA FORMALDEHYDE PRILLS(91,95) is presented has good electro catalytic activity.Prepared cobalt complex has accurate space
Structure and accurate molecular formula, have potential application prospect as electro catalytic activity material.
Brief description of the drawings
Fig. 1 is that cobalt complex construction unit figure of the invention (is illustrative clarity, carbon atom and symmetry operation atom out
Without mark)；
Fig. 2 is the electrochemical catalysis response diagram of cobalt complex PARA FORMALDEHYDE PRILLS(91,95) of the invention.
Specific embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1：
Weigh CoCl2·6H2O (0.3mmol, 0.0714g), 5- nitro whey potassium monohydrate (0.3mmol, 0.0772g)
It is placed in beaker, add water 10mL, heating, stirring dissolve it, obtain reacting mixture solution；Reacting mixture solution is turned
In moving on to 25mL there is the stainless steel cauldron of polytetrafluoroethyllining lining, it is placed in air dry oven after sealed reactor, 100 DEG C
Heating response 72 hours, reaction end is cooled to room temperature, opens reactor and obtains brownish red bulk crystals；By brownish red bulk crystals
Take out, natural air drying obtains cobalt complex.
Embodiment 2：
Weigh CoCl2·6H2O (0.3mmol, 0.0714g), 5- nitro whey potassium monohydrate (0.6mmol, 0.154g)
It is placed in beaker, add water 15mL, heating, stirring dissolve it, obtain reacting mixture solution；Reacting mixture solution is turned
In moving on to 25mL there is the stainless steel cauldron of polytetrafluoroethyllining lining, it is placed in air dry oven after sealed reactor, 120 DEG C
Heating response 24 hours, reaction end is cooled to room temperature, opens reactor and obtains brownish red bulk crystals；By brownish red bulk crystals
Take out, natural air drying obtains cobalt complex.
Embodiment 3：
Weigh CoCl2·6H2O (0.2mmol, 0.0475g), 5- nitro whey potassium monohydrate (0.3mmol, 0.0772g)
It is placed in beaker, add water 13mL, heating, stirring dissolve it, obtain reacting mixture solution；Reacting mixture solution is turned
In moving on to 25mL there is the stainless steel cauldron of polytetrafluoroethyllining lining, it is placed in air dry oven after sealed reactor, 110 DEG C
Heating response 48 hours, reaction end is cooled to room temperature, opens reactor and obtains brownish red bulk crystals；By brownish red bulk crystals
Take out, natural air drying obtains cobalt complex.
Cobalt complex obtained in embodiment 1-3 is carried out into structured testing, as a result shows 5- nitros whey during the course of the reaction
The carboxyl of acid is sloughed, and is coordinated with cobalt ions using its nitrogen, forms new cobalt complex.Cobalt obtained by the present invention coordinates
Its chemical formula of thing is CoC8H12N6O12, its construction unit is [Co (C4H2N3O4)2(H2O)4], crystallographic system is anorthic system, space group
It is P-1, cell parameter is α=97.141 °, β=108.592 °, γ=
115.555 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.The construction unit of prepared cobalt complex is as shown in Figure 1
(for illustrative clarity, carbon atom and symmetry operation atom out are not marked).
Obtained cobalt complex PARA FORMALDEHYDE PRILLS(91,95) is carried out into electrocatalysis characteristic test, as a result shows that the complex PARA FORMALDEHYDE PRILLS(91,95) has
Good electrocatalysis characteristic (such as Fig. 2).
Claims (3)
1. a kind of PARA FORMALDEHYDE PRILLS(91,95) has the cobalt complex of electro catalytic activity, it is characterised in that the complex has certain space structure,
Its chemical formula is CoC8H12N6O12, construction unit is [Co (C4H2N3O4)2(H2O)4], crystallographic system is anorthic system, and space group is P-
1, cell parameter isα=97.141 °, β=108.592 °, γ=
115.555 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.
2. a kind of PARA FORMALDEHYDE PRILLS(91,95) as claimed in claim 1 has the preparation method of the cobalt complex of electro catalytic activity, and its feature exists
In comprising the following steps：
(1) a certain amount of hydration cobaltous dichloride and 5- nitroorotic acid potassium monohydrates are weighed, is placed in beaker, according to Co (II)
Ion is 1 with the ratio of the amount of substance of 5- nitroorotic acid potassium:1~2 ratio is added, and add water 10~15mL, and is heated, stirred and make
Its dissolving, obtains reacting mixture solution；
(2) above-mentioned reacting mixture solution is transferred to during 25mL has a stainless steel cauldron of polytetrafluoroethyllining lining, it is close
It is placed in air dry oven after envelope reactor, 100~120 DEG C of heating responses 24~72 hours, reaction end is cooled to room temperature, beats
Drive reactor and obtain brownish red bulk crystals；
(3) brownish red bulk crystals are taken out, natural air drying, obtains final product described cobalt complex.
3. PARA FORMALDEHYDE PRILLS(91,95) according to claim 2 has the preparation method of the cobalt complex of electro catalytic activity, it is characterised in that
It is described participate in reaction material be chemistry it is pure, it is described hydration cobaltous dichloride be six hydration cobaltous dichlorides.
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| CN201710181530.4A CN106928153B (en) | 2017-03-24 | 2017-03-24 | A kind of PARA FORMALDEHYDE PRILLS(91,95) has the cobalt complex and preparation method thereof of electro catalytic activity |
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| CN201710181530.4A CN106928153B (en) | 2017-03-24 | 2017-03-24 | A kind of PARA FORMALDEHYDE PRILLS(91,95) has the cobalt complex and preparation method thereof of electro catalytic activity |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103396458A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Compound with electrochemical response to formaldehyde and preparation method thereof |
| CN103435659A (en) * | 2013-08-12 | 2013-12-11 | 宁波大学 | Cobalt complex with electrochemical catalytic activity |
| CN103467367A (en) * | 2013-09-13 | 2013-12-25 | 宁波大学 | Cobalt complex having electrocatalytic activity on hydrogen peroxide |
| CN103709204A (en) * | 2013-12-09 | 2014-04-09 | 南京信息工程大学 | Cobalt complex, preparation method and application thereof |
| US20140371446A1 (en) * | 2010-07-16 | 2014-12-18 | Abbvie Inc. | Phosphine ligands for catalytic reactions |
| CN104926888A (en) * | 2015-05-29 | 2015-09-23 | 南京信息工程大学 | Cobalt complex and preparation method and application thereof |
| CN106083616A (en) * | 2016-06-03 | 2016-11-09 | 合肥工业大学 | The preparation of a kind of cobalt complex and synthetic method |
-
2017
- 2017-03-24 CN CN201710181530.4A patent/CN106928153B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140371446A1 (en) * | 2010-07-16 | 2014-12-18 | Abbvie Inc. | Phosphine ligands for catalytic reactions |
| CN103396458A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Compound with electrochemical response to formaldehyde and preparation method thereof |
| CN103435659A (en) * | 2013-08-12 | 2013-12-11 | 宁波大学 | Cobalt complex with electrochemical catalytic activity |
| CN103467367A (en) * | 2013-09-13 | 2013-12-25 | 宁波大学 | Cobalt complex having electrocatalytic activity on hydrogen peroxide |
| CN103709204A (en) * | 2013-12-09 | 2014-04-09 | 南京信息工程大学 | Cobalt complex, preparation method and application thereof |
| CN104926888A (en) * | 2015-05-29 | 2015-09-23 | 南京信息工程大学 | Cobalt complex and preparation method and application thereof |
| CN106083616A (en) * | 2016-06-03 | 2016-11-09 | 合肥工业大学 | The preparation of a kind of cobalt complex and synthetic method |
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Application publication date: 20170707 Assignee: Ningbo Science and Technology Innovation Association Assignor: Ningbo University Contract record no.: X2023980033633 Denomination of invention: A cobalt complex with electrocatalytic activity for formaldehyde and a preparation method thereof Granted publication date: 20190416 License type: Common License Record date: 20230317 |