CN105214726A - A kind of preparation of the Nanometer Copper composite for catalytic reduction - Google Patents
A kind of preparation of the Nanometer Copper composite for catalytic reduction Download PDFInfo
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- CN105214726A CN105214726A CN201510630100.7A CN201510630100A CN105214726A CN 105214726 A CN105214726 A CN 105214726A CN 201510630100 A CN201510630100 A CN 201510630100A CN 105214726 A CN105214726 A CN 105214726A
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- polyetheramine
- catalytic reduction
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- copper composite
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Abstract
The invention discloses a kind of preparation of the Nanometer Copper composite for catalytic reduction, and its catalytic reduction performance tested: by polyetheramine distilled water or anhydrous alcohol solution for subsequent use; Copper sulphate and NaOH are dissolved with foregoing polyethers amine aqueous solution respectively, then both mixing, prepare the turbid liquid of Kocide SD at ambient temperature.Polyphenol to be joined in the turbid liquid of above-mentioned Kocide SD 40 ~ 100
oc reacts 30 ~ 120min, and the mol ratio of Kocide SD and polyphenol is 1:0.8 ~ 4; Add quantitative polyetheramine afterwards and react 4 ~ 12h again, the mol ratio of polyetheramine total amount and polyphenol is 1:0.8 ~ 1.2.Product is washed, centrifugal, dry, namely obtain the Nanometer Copper composite of phenol amine polymer parcel.The composite obtained is used for p-nitrophenol, methylene blue, the catalytic reduction of rhodamine B.Preparation method of the present invention is simple, and material source is extensive, and reaction condition is gentle, and solvent environment is friendly, is convenient to promote the use of.
Description
Technical field
The present invention relates to nano-functional material technical field, particularly relate to a kind of preparation method of the Nanometer Copper composite for catalytic reduction.
Background technology
Copper nano material replaces noble metal gold, silver preparing in advanced lubrication oil additive, electrocondution slurry, effective catalyst and antiseptic etc. and can greatly reducing costs as the important raw material of industry, has broad application prospects.But because the chemical property of Nanometer Copper is very active, expose oxidized very soon in atmosphere, existence and stability and the problem such as dispersiveness is poor, therefore the copper preparation method of nano material of stability and favorable dispersibility, size and morphology controllable and performance study thereof have become the study hotspot of field of nanometer material technology.
The method of copper nano material that what development in recent years was got up prepare mainly contains physical vaporous deposition, electrochemical deposition method, metallo-organic compound thermal decomposition method, solution phase chemical reduction, hydro-thermal method and microemulsion method etc.Along with people are to the development of deepening continuously of being familiar with of nano material and nanosecond science and technology, nano material preparation is no longer confined to simple nano particle, and has the nano composite material transition of specific function to design and controlledly synthesis gradually.Research shows that the compound of nano particle effectively can not only avoid the agglomeration traits of single nano particle, but also can give full play to the excellent properties of nano particle, improves its action effect.The combination of out-phase storeroom is carried out in the formation of nano composite material usually by the effect such as chemical bond or electrostatic attraction.Composite respectively has different physicochemical properties mutually, can not only improve the stability of nano material, and all shows the cooperative effect made new advances in optics electricity magnetics biology etc.Therefore the Synthesis and application of nano composite material one of focus becoming current research.
High molecule nano composite material is a kind of advanced composite material (ACM) by various nano unit and high-molecular organic material composite molding in every way.By the type of its compound, three kinds are broadly divided into common nano particle polymer composite: nanoparticle and nanoparticle compound, composite nano film and nanoparticle and conventional blocks compound.Nano particle in macromolecule matrix can dispersed also can non-homogeneous dispersion; Possible ordered arrangement, the also unordered arrangement of possibility; The main geometric parameters of compound system comprises self geometric parameter, spatial distributed parameters and the volume fraction of nano unit.
High molecule nano composite material has many advantages as photochemical catalyst.First be that nano particle diameter is wherein very little, specific area is large, photocatalysis efficiency is high, chemical reactivity is high; Secondly, nanoparticle dispersion often has the transparency in media as well, easily uses optical instrument to observe the change of Charger transfer, proton translocation, semiconductor energy level structure and surface density of states between interface; 3rd, nano particle, using high polymer as matrix, can play high catalytic activity and the selecting catalytic performance of nano particle, and the stabilization again by high polymer makes it to have long-term stability.
Summary of the invention
The object of this invention is to provide the compound that a kind of simple and rapid utilization contains phenolic hydroxyl group and amido and prepare Nanometer Copper composite, this composite is to p-nitrophenol, and methylene blue, rhodamine B has good catalytic reduction ability.
The step of the method for the invention is as follows: after polyetheramine distilled water or absolute ethyl alcohol or the dissolving of both mixed solvents, dissolve copper sulphate and NaOH respectively in duplicate, then both are mixed with the turbid liquid of Kocide SD.Then polyphenol and polyetheramine are added successively and be obtained by reacting product.End product is washed, centrifugal, dry, namely obtain the Nanometer Copper composite with catalytic performance of phenol amine polymer parcel.
Further, in described step, dispersant is polyetheramine.
Further, the polyphenol in described step refers at least one in catechol or hydroquinones.
Further, in described step, polyetheramine is one in polyetheramine D230 or polyetheramine D400 or its mixture.
Further, the reaction temperature after adding polyphenol, polyetheramine in described step is 40 ~ 100
oc.
Further, after adding polyphenol in described step, adding the reaction time before polyetheramine is 30 ~ 120min.
Further, enter in described step more polyphenol add polyetheramine again after reaction time be 4 ~ 12h.
Further, in described step, the mol ratio of Kocide SD and polyphenol is 1:0.8 ~ 4.
Further, in described step, the mol ratio of polyetheramine total amount and polyphenol is 1:0.8 ~ 1.2.
The method tool preparing Nanometer Copper composite of the present invention has the following advantages: with low cost, preparation method is simple, reaction condition is gentle, solvent environment is friendly.
Accompanying drawing explanation
Fig. 1 is composite catalysis p-nitrophenol absorbance curve over time;
Fig. 2 is composite catalysis rhodamine B absorbance curve over time.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described.Following examples are intended to the present invention instead of limitation of the invention further are described.
Embodiment 1:
(1) Nanometer Copper composite is prepared
0.2g polyetheramine D230 is distributed in 50ml distilled water, ultrasonic dissolution, be divided into two parts for subsequent use.Take 0.25g Salzburg vitriol and 0.08g NaOH is dissolved in two parts of polyetheramine D230 solution respectively.Under room temperature magnetic agitation, sodium hydroxide solution is poured in copper-bath, form the turbid liquid of Kocide SD.This turbid liquid is placed in single port bottle, is placed on 80
oin C oil bath pan, magnetic agitation, takes rapidly 0.11g catechol and adds in single port bottle, and condensing reflux stirs.After 1h, take 0.03g polyetheramine D230 and add in reactant liquor, continue to stir.Reaction stopped after 6h, product is centrifugal, and washing, puts into vacuum drying chamber 30
oc is dry.
(2) catalytic performance of Nanometer Copper composite is studied
Take 2.5mg composite, join in 10ml distilled water for subsequent use; Taking 4.2mg p-nitrophenol joins in 250ml distilled water for subsequent use; Taking 24mg sodium borohydride joins in 10ml distilled water for subsequent use.The aqueous solution getting 1.5ml composite joins in 2.5ml p-nitrophenyl phenol solution, then measures 0.5ml sodium borohydride solution and adds wherein, with its catalytic performance of ultraviolet specrophotometer tracing detection.
Embodiment 2:
(1) Nanometer Copper composite is prepared
0.4g polyetheramine D400 is distributed in 100ml distilled water, ultrasonic dissolution, be divided into two parts for subsequent use.Take 0.32g anhydrous cupric sulfate and 0.16g NaOH is dissolved in two parts of polyetheramine D400 solution respectively, then under room temperature magnetic agitation, sodium hydroxide solution is poured in copper-bath, prepare the turbid liquid of Kocide SD.This turbid liquid is placed in single port bottle, is placed on 60
oin C oil bath pan, magnetic agitation, takes rapidly 0.22g hydroquinones and adds in single port bottle, and condensing reflux stirs.After 1h, take 0.4g polyetheramine D400 and add in reactant liquor, continue to stir.Reaction stopped after 4h, product is centrifugal, and washing, puts into vacuum drying chamber 35
oc is dry.
(2) catalytic performance of Nanometer Copper composite is studied
By 2.5mg composite, join in 10ml distilled water for subsequent use; Taking 4.2mg p-nitrophenol joins in 250ml distilled water for subsequent use; Taking 24mg sodium borohydride joins in 10ml distilled water for subsequent use.The aqueous solution getting 750 μ l composites joins in 2.5ml p-nitrophenyl phenol solution, then measures 0.5ml sodium borohydride solution and adds wherein, with its catalytic performance of UV spectrophotometer measuring.
Embodiment 3:
(1) Nanometer Copper composite is prepared
0.3g polyetheramine D230 is distributed in 50ml absolute ethyl alcohol, ultrasonic dissolution, be divided into two parts for subsequent use.Take 0.32g anhydrous cupric sulfate and 0.16g NaOH is dissolved in two parts of polyetheramine D230 solution respectively, under room temperature magnetic agitation, sodium hydroxide solution is poured in copper-bath, prepare the turbid liquid of Kocide SD.This turbid liquid is placed in single port bottle, is placed on room temperature magnetic stirrer.Taking rapidly 0.22g catechol adds in single port bottle, and condensing reflux stirs.After 1h, take 0.16g polyetheramine D230 and add in reactant liquor, continue to stir.Reaction stopped after 12h, product is centrifugal, and washing, puts into vacuum drying chamber 30
oc is dry.
(2) catalytic performance of Nanometer Copper composite is studied
By 2.5mg composite, join in 10ml distilled water for subsequent use; Taking 5.0mg rhodamine B joins in 250ml distilled water for subsequent use; Taking 24mg sodium borohydride joins in 10ml distilled water for subsequent use.The aqueous solution getting 1ml composite joins in 2.5ml rhodamine B solution, then measures 0.5ml sodium borohydride solution and adds wherein, at its catalytic performance of UV spectrophotometer measuring.
Embodiment 4:
(1) Nanometer Copper composite is prepared
0.3g polyetheramine D400 is distributed in 100ml ethanol water, ultrasonic dissolution, be divided into two parts for subsequent use.Take 0.5g Salzburg vitriol and 0.16g NaOH is dissolved in two parts of polyetheramine D400 solution respectively, then under room temperature magnetic agitation, sodium hydroxide solution is poured in copper-bath, form Kocide SD suspension.This suspension is placed in single port bottle, is placed on 50
oin C oil bath pan, take rapidly 0.55g hydroquinones and add in single port bottle, condensing reflux stirs.After 45min, take 1.7g polyetheramine D400 and add in reactant liquor, continue to stir.Reaction stopped after 8h, product is centrifugal, and washing, puts into vacuum drying chamber 30
oc is dry.
(2) catalytic performance of Nanometer Copper composite is studied
2.5mg composite is joined in 10ml distilled water for subsequent use; Taking 5.0mg methylene blue joins in 250ml distilled water for subsequent use; Taking 24mg sodium borohydride joins in 10ml distilled water for subsequent use.The aqueous solution getting 1ml composite joins in 2.5ml methylene blue solution, then measures 0.5ml sodium borohydride solution and adds wherein, at its catalytic performance of UV spectrophotometer measuring.
Claims (10)
1., for a preparation for the Nanometer Copper composite of catalytic reduction, it is characterized in that following steps:
Polyetheramine, as after dispersant dissolution with solvents, dissolves copper sulphate and NaOH respectively in duplicate, both is mixed to get the turbid liquid of Kocide SD, add polyphenol and polyetheramine successively again, washing, centrifugal, drying, namely obtains a kind of Nanometer Copper composite for catalytic reduction.
2. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, is characterized in that described dispersant is polyetheramine.
3. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, is characterized in that the solvent of described polyetheramine is distilled water, absolute ethyl alcohol or the two mixed solvent.
4. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, is characterized in that described polyphenol is at least one in catechol or hydroquinones.
5. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, is characterized in that described polyetheramine is one in polyetheramine D230 or polyetheramine D400 or its mixture.
6. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, reaction temperature when adding polyphenol, polyetheramine described in it is characterized in that is 40 ~ 100
oc.
7. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, adding the polyphenol post-reacted reaction time described in it is characterized in that is 30 ~ 120min.
8. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, adding the polyetheramine post-reacted time after adding polyphenol described in it is characterized in that is 4 ~ 12h.
9. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, is characterized in that the thing mass ratio of described Kocide SD and polyphenol is 1:0.8 ~ 4.
10. the preparation of a kind of Nanometer Copper composite for catalytic reduction as claimed in claim 1, is characterized in that the thing mass ratio of described polyetheramine total amount and polyphenol is 1:0.8 ~ 1.2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664944A (en) * | 2016-02-19 | 2016-06-15 | 中国环境科学研究院 | Cu catalyst based on metal organic framework, preparation method and application |
| CN109926089A (en) * | 2019-03-22 | 2019-06-25 | 三峡大学 | The preparation method and application of the stable copper nanocatalyst of porphyrin |
| CN115722268A (en) * | 2022-11-18 | 2023-03-03 | 武汉工程大学 | Sponge-loaded nano copper-silver alloy composite material and preparation method and application thereof |
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| CN104004186A (en) * | 2014-05-16 | 2014-08-27 | 福州大学 | Hollow copper sulphide/polypyrrole nanometer compound and application thereof |
| CN104475056A (en) * | 2014-11-25 | 2015-04-01 | 齐鲁工业大学 | Preparation method of clomiphene polymer capable of adsorbing heavy metal ions and application of clomiphene polymer |
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Patent Citations (3)
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| WO2011042620A1 (en) * | 2009-10-08 | 2011-04-14 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Formation of metal particles on a solid oxide substrate having two separate grafted chemical functions |
| CN104004186A (en) * | 2014-05-16 | 2014-08-27 | 福州大学 | Hollow copper sulphide/polypyrrole nanometer compound and application thereof |
| CN104475056A (en) * | 2014-11-25 | 2015-04-01 | 齐鲁工业大学 | Preparation method of clomiphene polymer capable of adsorbing heavy metal ions and application of clomiphene polymer |
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| ADEMIR NEVES等: "Catecholase Activity of a Series of Dicopper(II) Complexes with Variable Cu−OH(phenol) Moieties", 《INORGANIC CHEMISTRY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664944A (en) * | 2016-02-19 | 2016-06-15 | 中国环境科学研究院 | Cu catalyst based on metal organic framework, preparation method and application |
| CN105664944B (en) * | 2016-02-19 | 2018-03-27 | 中国环境科学研究院 | A kind of Cu catalyst, Preparation method and use based on metal organic frame |
| CN109926089A (en) * | 2019-03-22 | 2019-06-25 | 三峡大学 | The preparation method and application of the stable copper nanocatalyst of porphyrin |
| CN115722268A (en) * | 2022-11-18 | 2023-03-03 | 武汉工程大学 | Sponge-loaded nano copper-silver alloy composite material and preparation method and application thereof |
| CN115722268B (en) * | 2022-11-18 | 2024-04-05 | 武汉工程大学 | Sponge-loaded nano copper-silver alloy composite material and preparation method and application thereof |
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Granted publication date: 20171017 Termination date: 20180929 |