CN107583656A - A kind of self-supporting Cu/CuI catalysis materials and preparation method thereof - Google Patents
A kind of self-supporting Cu/CuI catalysis materials and preparation method thereof Download PDFInfo
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- CN107583656A CN107583656A CN201710825152.9A CN201710825152A CN107583656A CN 107583656 A CN107583656 A CN 107583656A CN 201710825152 A CN201710825152 A CN 201710825152A CN 107583656 A CN107583656 A CN 107583656A
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Abstract
The invention belongs to photocatalysis technology field, and a kind of method for preparing self-supporting Cu/CuI catalysis materials is disclosed, comprised the following steps：(1) copper mesh is placed in hydrochloric acid and impregnated, then be placed in ethanol and clean；(2) copper mesh after cleaning is put into closed container, then adds a certain amount of solid-state iodine particle in a reservoir, sealed certain time, obtain self-supporting Cu/CuI catalysis materials.Self-supporting Cu/CuI catalysis materials prepared by the present invention have excellent photocatalysis performance and self-supporting characteristic, catalyst is easily isolated and is reclaimed after application, reduce catalysis cost, and can realize low cost, large-scale production.
Description
Technical field
The invention belongs to photocatalysis technology field, more particularly, to a kind of self-supporting Cu/CuI catalysis materials and its
Preparation method.
Background technology
Industrialized development, the quickening of urbanization, while human lives' quality is improved, also depend on for existence to us
Environment brings pollution.Under this situation, the processing of water pollution problems is to the strategic most important of national sustainable development.Light is urged
Agent technology, because it effectively can administer sewage using solar energy clean energy resource, while equipment is simple, raw material is saved, in sewage
Improvement aspect has a wide range of applications and significant advantage.However, the photochemical catalyst studied at present because of its powder morphology face
The problem of facing separation and cumbersome removal process, if catalyst and organic solution separation do not only result in the secondary dirt of solution thoroughly
Dye can also cause damage to the quality of catalyst, therefore it is current photocatalysis to develop the catalysis material with self-supporting characteristic
The Research Challenges in degraded field.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of self-supporting Cu/CuI photocatalysis materials
Material and preparation method thereof, this method have simple, quick, efficient, energy-conservation, and obtained Cu/CuI catalysis materials have self-supporting
With the characteristic of self-supporting.
To achieve the above object, according to one aspect of the present invention, there is provided one kind prepares self-supporting Cu/CuI photocatalysis
The method of material, it is characterised in that comprise the following steps：
(1) copper mesh is first placed in hydrochloric acid to impregnate to be placed in ethanol again and cleaned, to remove the oxide layer on copper mesh surface；
(2) copper mesh after step (1) is cleaned is put into closed container, then solid-state iodine particle is added in closed container,
It is 0.5h~4h solid-state iodine particle is carried out iodination reaction and iodination reaction time with copper mesh, then obtains self-supporting Cu/CuI light and urge
Change material, wherein, the mass ratio of solid-state iodine particle and copper mesh is 1:1~1:4.
Preferably, the mesh number of the copper mesh is 200 mesh, string diameter 0.051mm, aperture 0.076mm.
Preferably, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid.
Preferably, the ethanol for cleaning copper mesh is absolute ethyl alcohol, and specification is pure to analyze.
Preferably, the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
According to another aspect of the present invention, a kind of self-supporting Cu/CuI catalysis materials are additionally provided, by the above method
It is prepared.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：
1) present invention obtains Cu/CuI catalysis materials using normal temperature iodide process, this method have it is simple, quick, efficient,
The characteristics of energy-conservation, and low cost, large-scale production can be realized.
2) the obtained Cu/CuI catalysis materials of the present invention have a characteristic of self-supporting and self-supporting, after the completion of catalytic reaction
It is easily recycled, to environment non-secondary pollution, and it is reusable.
Brief description of the drawings
Fig. 1 is self-supporting Cu/CuI catalysis material preparation flow figures of the present invention；
Fig. 2 is the XRD spectrum of self-supporting Cu/CuI catalysis materials of the present invention；
Fig. 3 is the Cu/CuI catalysis material SEM photographs of embodiment 1；
Fig. 4 is the Cu/CuI catalysis material SEM photographs of embodiment 2；
Fig. 5 is the Cu/CuI catalysis material SEM photographs of embodiment 3；
Fig. 6 is the Cu/CuI catalysis material SEM photographs of embodiment 4；
Fig. 7 is influence of the different iodate times to catalysis material performance of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Conflict can is not formed each other to be mutually combined.
Embodiment 1：
As shown in figure 1, first, copper mesh is placed in hydrochloric acid and impregnated；Then, copper mesh is placed in ethanol and cleaned, to remove
The oxide layer on copper mesh surface；Finally, the copper mesh after cleaning is put into closed container, then adds solid-state iodine particle in a reservoir,
The mass ratio of solid-state iodine particle and copper mesh is 1:2, iodate 0.5h, obtain self-supporting Cu/CuI catalysis materials.Wherein, the copper
The mesh number of net is 200 mesh, and string diameter 0.051mm, aperture 0.076mm, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid, cleans the ethanol of copper mesh
For absolute ethyl alcohol, specification is pure to analyze, and the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
Embodiment 2：
As shown in figure 1, first, copper mesh is placed in hydrochloric acid and impregnated；Then, copper mesh is placed in ethanol and cleaned, to remove
The oxide layer on copper mesh surface；Finally, the copper mesh after cleaning is put into closed container, then adds solid-state iodine particle in a reservoir,
The mass ratio of solid-state iodine particle and copper mesh is 1:2, iodate 1h, obtain self-supporting Cu/CuI catalysis materials.Wherein, the copper mesh
Mesh number be 200 mesh, string diameter 0.051mm, aperture 0.076mm, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid, and the ethanol for cleaning copper mesh is
Absolute ethyl alcohol, specification is pure to analyze, and the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
Embodiment 3：
As shown in figure 1, first, copper mesh is placed in hydrochloric acid and impregnated；Then, copper mesh is placed in ethanol and cleaned, to remove
The oxide layer on copper mesh surface；Finally, the copper mesh after cleaning is put into closed container, then adds solid-state iodine particle in a reservoir,
The mass ratio of solid-state iodine particle and copper mesh is 1:2, iodate 2h, obtain self-supporting Cu/CuI catalysis materials.Wherein, the copper mesh
Mesh number be 200 mesh, string diameter 0.051mm, aperture 0.076mm, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid, and the ethanol for cleaning copper mesh is
Absolute ethyl alcohol, specification is pure to analyze, and the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
Embodiment 4：
As shown in figure 1, first, copper mesh is placed in hydrochloric acid and impregnated；Then, copper mesh is placed in ethanol and cleaned, to remove
The oxide layer on copper mesh surface；Finally, the copper mesh after cleaning is put into closed container, then adds solid-state iodine particle in a reservoir,
The mass ratio of solid-state iodine particle and copper mesh is 1:2, iodate 4h, obtain self-supporting Cu/CuI catalysis materials.Wherein, the copper mesh
Mesh number be 200 mesh, string diameter 0.051mm, aperture 0.076mm, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid, and the ethanol for cleaning copper mesh is
Absolute ethyl alcohol, specification is pure to analyze, and the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
Embodiment 5：
As shown in figure 1, first, copper mesh is placed in hydrochloric acid and impregnated；Then, copper mesh is placed in ethanol and cleaned, to remove
The oxide layer on copper mesh surface；Finally, the copper mesh after cleaning is put into closed container, then adds solid-state iodine particle in a reservoir,
The mass ratio of solid-state iodine particle and copper mesh is 1:1, iodate 1h, obtain self-supporting Cu/CuI catalysis materials.Wherein, the copper mesh
Mesh number be 200 mesh, string diameter 0.051mm, aperture 0.076mm, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid, and the ethanol for cleaning copper mesh is
Absolute ethyl alcohol, specification is pure to analyze, and the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
Embodiment 6：
As shown in figure 1, first, copper mesh is placed in hydrochloric acid and impregnated；Then, copper mesh is placed in ethanol and cleaned, to remove
The oxide layer on copper mesh surface；Finally, the copper mesh after cleaning is put into closed container, then adds solid-state iodine particle in a reservoir,
The mass ratio of solid-state iodine particle and copper mesh is 1:4, iodate 1h, obtain self-supporting Cu/CuI catalysis materials.Wherein, the copper mesh
Mesh number be 200 mesh, string diameter 0.051mm, aperture 0.076mm, the hydrochloric acid for impregnating copper mesh is watery hydrochloric acid, and the ethanol for cleaning copper mesh is
Absolute ethyl alcohol, specification is pure to analyze, and the iodination reaction of the copper mesh and solid-state iodine particle is carried out at normal temperatures.
Following emphasis in conjunction with the embodiments 1-4 come the spy of self-supporting Cu/CuI catalysis materials that analyzes this method and obtain
Point.
Fig. 2 is the XRD spectrum of Cu/CuI catalysis materials in embodiment 1-4.By contrasting 0.5,1, the 2 and 4h iodate times
The XRD analysis result of processing can be seen that all diffractive features peaks and both correspond to cubic Cu and cubic CuI, say
Bright catalysis material is by Cu and the phase compositions of CuI two.As the iodate time increases, cubic Cu peak intensity weakens and cubic crystal
Type CuI peak intensity lifting, illustrates Cu and I2Reaction generation CuI chemical reaction is persistently carried out, and CuI content is with the iodate time
Increase and increase.
Fig. 3-6 is respectively to obtain the SEM of Cu/CuI catalysis materials under the 0.5-4h difference iodate times in embodiment 1-4
Figure.It can be seen that catalysis material surface particles size is at 1 μm or so under the different iodate times.When the iodate time
When being 0.5h, surface particles are in the round and smooth grain shape in edge；When the iodate time increasing to 1h, grain edges are clear, have similar
The shape of triangle occurs；When the iodate time continuing to increase to 2h, grain edges understand and the triangle shape of standard are presented
Shape, wherein triangle are the distinctive microscopic appearances of CuI, and this illustrates copper mesh Surface Creation CuI；Continue to increase when the iodate time
Add, particle is still the triangle of clear-cut margin, and numbers of particles becomes more, size increase.
Fig. 7 is the photocatalysis performance of the self-supporting Cu/CuI catalysis materials prepared in the present invention under the different iodate times
Figure.The catalytic performance of prepared Cu/CuI catalysis materials is characterized by the degraded of rhodamine B (RhB) solution.Specifically
Experimentation is as follows：Cu/CuI catalysis materials are put into equipped with 10mL RhB (2.5 × 10-5Mol/L, will) in the beaker of solution
Beaker dark treatment 30min is balanced with reaching the adsorption-desorption of catalyst and RhB molecules.With power density 100mw/cm2Xenon lamp
(λ=200-400nm) is used as ultraviolet source, is surveyed at interval of 30min with ultraviolet-visible absorption spectroscopy instrument (Mapada, UV-6100)
Measure RhB concentration.Because Cu/CuI catalysis materials of the present invention have good self-supporting characteristic, after the completion of catalytic reaction,
The separation process of catalyst and organic solution and the recycling process of catalyst greatly simplify.As shown in fig. 7, work as iodine
Change short period time, the iodate time photocatalysis performance of more long material is better；But after the iodate time is more than 1h, extend iodine
The change time does not have much affect to the photocatalysis performance of material.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (6)
- A kind of 1. method for preparing self-supporting Cu/CuI catalysis materials, it is characterised in that comprise the following steps：(1) copper mesh is first placed in hydrochloric acid to impregnate to be placed in ethanol again and cleaned, to remove the oxide layer on copper mesh surface；(2) copper mesh after step (1) is cleaned is put into closed container, then solid-state iodine particle is added in closed container, is made solid It is 0.5h~4h that state iodine particle carries out iodination reaction and iodination reaction time with copper mesh, then obtains self-supporting Cu/CuI photocatalysis materials Material, wherein, the mass ratio of solid-state iodine particle and copper mesh is 1:1~1:4.
- 2. a kind of method for preparing self-supporting Cu/CuI catalysis materials according to claim 1, it is characterised in that described The mesh number of copper mesh is 200 mesh, string diameter 0.051mm, aperture 0.076mm.
- A kind of 3. method for preparing self-supporting Cu/CuI catalysis materials according to claim 1, it is characterised in that dipping The hydrochloric acid of copper mesh is watery hydrochloric acid.
- A kind of 4. method for preparing self-supporting Cu/CuI catalysis materials according to claim 1, it is characterised in that cleaning The ethanol of copper mesh is absolute ethyl alcohol, and specification is pure to analyze.
- 5. a kind of method for preparing self-supporting Cu/CuI catalysis materials according to claim 1, it is characterised in that described The iodination reaction of copper mesh and solid-state iodine particle is carried out at normal temperatures.
- 6. a kind of self-supporting Cu/CuI catalysis materials, it is characterised in that as described in any claim in Claims 1 to 5 Method be prepared.
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| CN104163449A (en) * | 2014-08-16 | 2014-11-26 | 贵州大学 | Preparation method of gamma-copper iodide |
| CN105645456A (en) * | 2016-03-30 | 2016-06-08 | 淮北师范大学 | Preparation method of CuI nano-powder |
| CN105825990A (en) * | 2016-03-30 | 2016-08-03 | 淮北师范大学 | Preparation method of CuI-Fe3O4 magnetic nano-composite |
| CN103710750B (en) * | 2013-12-18 | 2018-05-11 | 中国科学院福建物质结构研究所 | A kind of growing method of large scale CuI crystal |
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2017
- 2017-09-14 CN CN201710825152.9A patent/CN107583656A/en active Pending
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| CN103695993A (en) * | 2013-12-18 | 2014-04-02 | 中国科学院福建物质结构研究所 | Growing method for high-quality CuI crystals |
| CN103710750B (en) * | 2013-12-18 | 2018-05-11 | 中国科学院福建物质结构研究所 | A kind of growing method of large scale CuI crystal |
| CN104163449A (en) * | 2014-08-16 | 2014-11-26 | 贵州大学 | Preparation method of gamma-copper iodide |
| CN105645456A (en) * | 2016-03-30 | 2016-06-08 | 淮北师范大学 | Preparation method of CuI nano-powder |
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