CN104275200A - Preparation method of ZnS/Ni2P composite micro-sphere with core-shell structure - Google Patents

Preparation method of ZnS/Ni2P composite micro-sphere with core-shell structure Download PDF

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CN104275200A
CN104275200A CN201410476102.0A CN201410476102A CN104275200A CN 104275200 A CN104275200 A CN 104275200A CN 201410476102 A CN201410476102 A CN 201410476102A CN 104275200 A CN104275200 A CN 104275200A
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CN104275200B (en
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刘淑玲
王正奇
仝建波
杜经武
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Shaanxi University of Science and Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract

The invention provides a preparation method of a ZnS/Ni2P composite micro-sphere with a core-shell structure. The preparation method comprises the following steps: firstly, preparing zinc sulfide powder; secondly, by taking the zinc sulfide powder, a soluble nickel salt and yellow phosphorus as main raw materials, slowing down a releasing speed of nickel ions by a chelation effect of citric acid on the nickel ions; and synthesizing the ZnS/Ni2P composite microsphere with the core-shell structure under the effect of a surfactant sodium dodecyl sulfate (SDS) at a low temperature under a hydrothermal condition. The preparation method is simple and feasible; and conditions are easy to control, the repeatability is good and post-period heat treatment is not needed. When the ZnS/Ni2P composite micro-sphere is subjected to a photocatalytic performance test, the photocatalytic performance is better than that of single zinc sulfide, so that the ZnS/Ni2P composite micro-sphere has a certain application potential in the aspect of photocatalytically degrading dyestuff wastewater.

Description

A kind of nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes
Technical field
The present invention relates to photocatalysis technology field, relate in particular to a kind of nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes.
Background technology
Semiconductor nano/micron material has quantum size effect, skin effect and macro quanta tunnel effect, present the performance of many excellences, and have broad application prospects in luminescent material, nonlinear optical material, light sensor material and catalysis material etc.ZnS is as a kind of important broad stopband II-VI group compound semiconductor materials, and under room temperature, its energy gap is 3.66eV.Because it has good fluorescent effect and electroluminescent function, it presents potential application in all many-sides such as electroluminescent device, light emitting diode (LED), solar cell, sensor, flat-panel monitors.And having high energy conversion efficiency due to ZnS, it can as efficient photochemical catalyst, is used for degraded organic polluting water, reduction toxic heavy metal etc.Thus make the research of its preparation and property become the focus of people's concern.
But going deep into along with research, find that one-component nano material makes its application in a lot of field all receive restriction to a certain degree due to the unicity of its function, and the compound of two or more semi-conducting material on nanoscale may produce some new characteristic, increase new function, and then make the research of the preparation and property of nano composite material become the focus of nanometer material science research.In recent years, transition metal phosphide, as a kind of high activity, high stability and the new catalytic material with anti-sulfur poisonous performance, because it is in all many-sided application, has caused and has paid close attention to widely.In transition metal phosphide, take nickel phosphide as typical case especially, nickel phosphide not only presents good application in catalysis, and can also undermine waterproof material as anticorrosive, wear-resistant, nickel phosphide presents potential application prospect.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of this invention is to provide a kind of nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes, simple and easy to do, obtained ZnS/Ni 2p complex microsphere has superior photocatalysis performance.
In order to achieve the above object, the technical scheme that the present invention takes is:
A kind of nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes, comprises the following steps:
1) zinc sulphide microballoon is prepared: by 1mmol Zn (CH 3cOO) 22H 2o is dissolved in 15mL distilled water, under magnetic agitation, continue to add 0.45mL glacial acetic acid, magnetic agitation in a moment, 1.5mmol thiocarbamide is added again in system, continue to be stirred to solution water white transparency, gained solution being transferred to 20mL liner is in the reactor of polytetrafluoroethylene (PTFE), at 170 DEG C, react 8h in insulating box, question response terminates, and naturally cools, centrifugation, with distilled water and absolute ethyl alcohol, sample is washed respectively, in 60 DEG C of dry 6h in vacuum drying chamber, obtain white zinc sulfide powder;
2) ZnS/Ni is prepared 2p complex microsphere: by step 1) obtained zinc sulfide powder is dissolved under magnetic stirring and fills in the polytetrafluoroethylene (PTFE) reactor of 13 ~ 16mL distilled water, add water soluble nickel salt wherein, stir a moment, add citric acid again, continue the system that is stirred to evenly after, add lauryl sodium sulfate (SDS), continue the system that is stirred to evenly after add yellow phosphorus, reaction system is placed in insulating box in 160 DEG C ~ 200 DEG C reaction 16 ~ 20h, question response terminates, naturally cool, centrifugation, use distilled water respectively, benzene and absolute ethyl alcohol wash sample, then product is placed in the dry 18 ~ 24h of vacuum drying chamber of 50 ~ 70 DEG C, obtain the ZnS/Ni of grey 2p powder.
Described water soluble nickel salt is one or more in nickel nitrate, nickelous sulfate, nickel chloride, nickel acetate.
The compactedness of described polytetrafluoroethylene (PTFE) should control 70% ~ 80%.
Described zinc sulfide powder: water miscible nickel salt: citric acid: the mol ratio of yellow phosphorus is 3:1.5:[1.5 ~ 4.5]: [1.5 ~ 4.5].
The nucleocapsid structure ZnS/Ni prepared by said method 2p composite inorganic membranes can be used as photocatalyst for degrading waste water from dyestuff.
ZnS/Ni of the present invention 2the formation mechenism of P complex microsphere: first, before reaction, the Ni in solution 2+first carry out complexing with citric acid; Secondly, in course of reaction, Ni 2+can enter in solution by slow releasing, and zinc sulphide current potential that microsphere surface is with is negative potential, by electrostatic interaction, Ni 2+be adsorbed on the surface of zinc sulphide microballoon.Finally, under hydrothermal conditions, Ni 2p nano particle is formed gradually and is coated on the surface of zinc sulphide microballoon.
Beneficial effect of the present invention:
The raw material that the inventive method adopts is simple and easy to get, and method is simple, and condition is easy to control.Solvent for use is water, cheap and environmental protection.
The ZnS/Ni that the present invention is finally formed 2p complex microsphere pattern is good, and can find out Ni by scanning 2p nano particle is coated on the surface of zinc sulphide microballoon uniformly.
The ZnS/Ni that the present invention obtains 2p complex microsphere presents the more superior photocatalysis performance of more independent zinc sulphide microballoon.
Below illustrate effect of the present invention, photocatalysis performance test process is as follows:
First 1 × 10 is prepared -5the pyronine B solution 150mL of mol/L, then gets the zinc sulfide powder and ZnS/Ni prepared above 2the each 0.050g of P powder, add in the 100mL small beaker filling 50mL pyronine B dye solution respectively, give in a beaker in addition and only add 50mL dye solution as reference, above-mentioned 3 beakers are placed in ultrasonic cleaner in the dark ultrasonic 20min, in dark surrounds, 20min is stirred under magnetic stirring again in homemade camera bellows, to make system reach adsorption/desorption balance, stir rear sampling once.Then open 40W quartz uv lamp, carry out photocatalytic degradation experiment under magnetic stirring, get a sample every 15min, collect solution and catalyst respectively through centrifugal, sample six times altogether, utilize the absorbance of the solution collected by ultraviolet-visible spectrophotometer mensuration.Wherein, ZnS/Ni 2the photocatalytic degradation of P powder as shown in Figure 1, as can be seen from Figure 1, the ZnS/Ni prepared by the present invention 2p composite inorganic membranes is after ultraviolet lighting 90min, and reach about 80% to the degradation rate of pyrrole Luo Hong solution, its degradation effect shows ZnS/Ni 2the good photocatalysis performance of P powder tool and may be used for photocatalytic degradation of dye waste water.
Accompanying drawing explanation
Fig. 1 is ZnS/Ni of the present invention 2the photocatalytic degradation figure of P powder.
The ZnS/Ni of Fig. 2 obtained by embodiment 1 2the XRD figure of P complex microsphere.
Fig. 3 (a) zinc sulphide microballoon, (b) ZnS/Ni obtained by embodiment 1 2the SEM figure of P composite inorganic membranes.
The ZnS/Ni of Fig. 4 obtained by embodiment 6 2the XRD figure of P compound.
Detailed description of the invention
Below by way of specific embodiment, the present invention is further illustrated.
Embodiment 1
A kind of nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes, comprises the following steps:
1) zinc sulphide microballoon is prepared: by 1mmol Zn (CH 3cOO) 22H 2o is dissolved in 15mL distilled water, under magnetic agitation, continue to add 0.45mL glacial acetic acid, magnetic agitation in a moment, 1.5mmol thiocarbamide is added again in system, continue to be stirred to solution water white transparency, gained solution being transferred to 20mL liner is in the reactor of polytetrafluoroethylene (PTFE), in insulating box, 8h is reacted at 170 DEG C, question response terminates, naturally cool, centrifugation, with distilled water and absolute ethyl alcohol, sample is washed respectively, in 60 DEG C of dry 6h in vacuum drying chamber, obtain white powder, with reference to Fig. 3, by x-ray diffractometer and SEM, white powder is characterized, known products therefrom is the zinc sulphide of micro-sphere structure,
2) ZnS/Ni is prepared 2p complex microsphere: by 0.3mmol step 1) obtained zinc sulphide is dissolved under magnetic stirring and fills in the polytetrafluoroethylene (PTFE) reactor of 16mL distilled water, add 0.15mmol nickel chloride wherein, after stirring 15min, add 0.3mmol citric acid again, after continuation stirring 15min is even to system, add 0.1g SDS, continue the system that is stirred to evenly after add 0.15mmol yellow phosphorus, reaction system is placed in insulating box in 180 DEG C of reaction 16h, question response terminates, naturally cool, centrifugation, use distilled water respectively, benzene and absolute ethyl alcohol wash sample, then product is placed in the dry 24h of vacuum drying chamber of 60 DEG C, obtain the ZnS/Ni of grey 2p powder.
By utilizing Japanese Rigaku D/Max-3c type X-ray powder diffractometer, copper target Cu K α japan Hitachi S-4800 type SEM characterizes the structure of products therefrom, pattern, and with reference to Fig. 2, Fig. 3, known products therefrom is the homogeneous ZnS/Ni of pattern 2p complex microsphere.
Embodiment 2
Utilize step 1 in embodiment 1) prepared by zinc sulfide powder as raw material, in step 2) in, do not add lauryl sodium sulfate (SDS), other conditions remain unchanged, by phenetic analysis, products therefrom is containing a small amount of impurity, and the ZnS/Ni in the relative embodiment 1 of its pattern 2p complex microsphere is more mixed and disorderly.
Embodiment 3
Utilize step 1 in embodiment 1) prepared by zinc sulfide powder as raw material, in step 2) in, changing the consumption of citric acid is 0.15mmol, and other conditions remain unchanged.By phenetic analysis, products therefrom is ZnS/Ni 2p complex microsphere.Using the red B solution of pyrroles as photocatalytic degradation of dye, after illumination 90min, its degradation rate reaches 76%.
Embodiment 4
Utilize step 1 in embodiment 1) prepared by zinc sulfide powder as raw material, in step 2) in, changing the consumption of citric acid is 0.45mmol, and other conditions remain unchanged.By phenetic analysis, products therefrom is ZnS/Ni 2p complex microsphere.Irradiate 90min under uviol lamp after, 55% is reached to the degradation rate of the red B solution of pyrroles.
Embodiment 5
Utilize step 1 in embodiment 1) prepared by zinc sulfide powder as raw material, in step 2) in, reaction temperature is changed into 160 DEG C, keeps other conditions constant.By phenetic analysis, products therefrom is ZnS/Ni 2p complex microsphere.Irradiate 90min under uviol lamp after, 57% is reached to the degradation rate of the red B solution of pyrroles.
Embodiment 6
Utilize step 1 in embodiment 1) prepared by zinc sulfide powder as raw material, in step 2) in, reaction temperature is changed into 200 DEG C, keeps other conditions constant.With reference to Fig. 4, by phenetic analysis, products therefrom is ZnS/Ni 2p complex microsphere.Irradiate 90min under uviol lamp after, 78% is reached to the degradation rate of the red B solution of pyrroles.
Above description has been described in detail to specific embodiments of the invention, and the product phenomenon of different embodiments is described, but just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the present invention.

Claims (6)

1. a nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes, is characterized in that, comprises the following steps:
1) zinc sulphide microballoon is prepared; By 1mmol Zn (CH 3cOO) 22H 2o is dissolved in 15mL distilled water, under magnetic agitation, continue to add 0.45mL glacial acetic acid, magnetic agitation in a moment, 1.5mmol thiocarbamide is added again in system, continue to be stirred to solution water white transparency, gained solution being transferred to 20mL liner is in the reactor of polytetrafluoroethylene (PTFE), at 170 DEG C, react 8h in insulating box, question response terminates, and naturally cools, centrifugation, with distilled water and absolute ethyl alcohol, sample is washed respectively, in 60 DEG C of dry 6h in vacuum drying chamber, obtain white zinc sulfide powder;
2) ZnS/Ni is prepared 2p complex microsphere: by step 1) obtained zinc sulfide powder is dissolved under magnetic stirring and fills in the polytetrafluoroethylene (PTFE) reactor of 13 ~ 16mL distilled water, add water soluble nickel salt wherein, stir a moment, add citric acid again, continue the system that is stirred to evenly after, add lauryl sodium sulfate (SDS), continue the system that is stirred to evenly after add yellow phosphorus, reaction system is placed in insulating box in 160 DEG C ~ 200 DEG C reaction 16 ~ 20h, question response terminates, naturally cool, centrifugation, use distilled water respectively, benzene and absolute ethyl alcohol wash sample, then product is placed in the dry 18 ~ 24h of vacuum drying chamber of 50 ~ 70 DEG C, obtain the ZnS/Ni of grey 2p powder.
2. a kind of nucleocapsid structure ZnS/Ni according to claim 1 2the preparation method of P composite inorganic membranes, is characterized in that: described water soluble nickel salt is one or more in nickel nitrate, nickelous sulfate, nickel chloride, nickel acetate.
3. a kind of nucleocapsid structure ZnS/Ni according to claim 1 2the preparation method of P composite inorganic membranes, is characterized in that: the compactedness of described polytetrafluoroethylene (PTFE) should control 70% ~ 80%.
4. a kind of nucleocapsid structure ZnS/Ni according to claim 1 2the preparation method of P composite inorganic membranes, is characterized in that: described zinc sulfide powder: water miscible nickel salt: citric acid: the mol ratio of yellow phosphorus is 3:1.5:[1.5 ~ 4.5]: [1.5 ~ 4.5].
5. a kind of nucleocapsid structure ZnS/Ni according to claim 1 2the preparation method of P composite inorganic membranes, is characterized in that: the nucleocapsid structure ZnS/Ni prepared by said method 2p composite inorganic membranes is used as photocatalyst for degrading waste water from dyestuff.
6. a kind of nucleocapsid structure ZnS/Ni according to claim 1 2the preparation method of P composite inorganic membranes, is characterized in that, comprises the following steps:
1) zinc sulphide microballoon is prepared: by 1mmol Zn (CH 3cOO) 22H 2o is dissolved in 15mL distilled water, under magnetic agitation, continue to add 0.45mL glacial acetic acid, magnetic agitation in a moment, 1.5mmol thiocarbamide is added again in system, continue to be stirred to solution water white transparency, gained solution being transferred to 20mL liner is in the reactor of polytetrafluoroethylene (PTFE), in insulating box, 8h is reacted at 170 DEG C, question response terminates, naturally cool, centrifugation, with distilled water and absolute ethyl alcohol, sample is washed respectively, in 60 DEG C of dry 6h in vacuum drying chamber, obtain white powder, with reference to Fig. 3, by x-ray diffractometer and SEM, white powder is characterized, known products therefrom is the zinc sulphide of micro-sphere structure,
2) ZnS/Ni is prepared 2p complex microsphere: by 0.3mmol step 1) obtained zinc sulphide is dissolved under magnetic stirring and fills in the polytetrafluoroethylene (PTFE) reactor of 16mL distilled water, add 0.15mmol nickel chloride wherein, after stirring 15min, add 0.3mmol citric acid again, after continuation stirring 15min is even to system, add 0.1g SDS, continue the system that is stirred to evenly after add 0.15mmol yellow phosphorus, reaction system is placed in insulating box in 180 DEG C of reaction 16h, question response terminates, naturally cool, centrifugation, use distilled water respectively, benzene and absolute ethyl alcohol wash sample, then product is placed in the dry 24h of vacuum drying chamber of 60 DEG C, obtain the ZnS/Ni of grey 2p powder.
CN201410476102.0A 2014-09-17 2014-09-17 A kind of nucleocapsid structure ZnS/Ni 2the preparation method of P composite inorganic membranes Expired - Fee Related CN104275200B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105562045A (en) * 2015-12-25 2016-05-11 陕西科技大学 Method for preparing ZnS / Sn4P3 composite
CN106582743A (en) * 2016-12-30 2017-04-26 天津大学 Core-shell structure thionazin composite microspheres and preparation method thereof
CN107308967A (en) * 2016-04-26 2017-11-03 中国科学院理化技术研究所 A kind of photocatalysis Decomposition formic acid hydrogen manufacturing co-catalyst, photocatalytic system and the method for decomposing formic acid hydrogen manufacturing
CN112337491A (en) * 2020-11-17 2021-02-09 北华大学 Preparation method and application of nickel phosphide/indium oxide nanocomposite material applied to bifunctional photocatalysis
CN114132956A (en) * 2021-12-06 2022-03-04 深圳市华科创智技术有限公司 Preparation method of ZnS microspheres

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105562045A (en) * 2015-12-25 2016-05-11 陕西科技大学 Method for preparing ZnS / Sn4P3 composite
CN107308967A (en) * 2016-04-26 2017-11-03 中国科学院理化技术研究所 A kind of photocatalysis Decomposition formic acid hydrogen manufacturing co-catalyst, photocatalytic system and the method for decomposing formic acid hydrogen manufacturing
CN106582743A (en) * 2016-12-30 2017-04-26 天津大学 Core-shell structure thionazin composite microspheres and preparation method thereof
CN112337491A (en) * 2020-11-17 2021-02-09 北华大学 Preparation method and application of nickel phosphide/indium oxide nanocomposite material applied to bifunctional photocatalysis
CN112337491B (en) * 2020-11-17 2023-04-07 北华大学 Preparation method and application of nickel phosphide/indium oxide nanocomposite material applied to bifunctional photocatalysis
CN114132956A (en) * 2021-12-06 2022-03-04 深圳市华科创智技术有限公司 Preparation method of ZnS microspheres

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