CN103523816B - Silver chloride material with zigzag particle morphology and solid-gas phase interface self-assembling synthetic method thereof - Google Patents
Silver chloride material with zigzag particle morphology and solid-gas phase interface self-assembling synthetic method thereof Download PDFInfo
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- CN103523816B CN103523816B CN201310520235.9A CN201310520235A CN103523816B CN 103523816 B CN103523816 B CN 103523816B CN 201310520235 A CN201310520235 A CN 201310520235A CN 103523816 B CN103523816 B CN 103523816B
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- silver chloride
- spination
- hydrochloric acid
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Abstract
The invention provides a silver chloride material with zigzag particle morphology and a solid-gas phase interface self-assembling synthetic method thereof and relates to the silver chloride material with zigzag particle morphology and a preparation method thereof. The objective of the invention is to overcome the problem that formation of special morphology of silver chloride cannot be controlled without addition of a stabilizing agent in the prior art. According to the invention, low-concentration silver nitrate in high-concentration hydrochloric acid undergoes layer-upon-layer self-assembling in a solid-gas phase interface at a certain temperature by using hydrogen chloride and silver nitrate volatilized into a gas phase so as to produce silver chloride with zigzag particle morphology. The silver chloride with zigzag particle morphology prepared in the invention is used for preparation of a precursor for a high-efficiency photocatalysis material Ag@AgCl.
Description
Technical field
The invention belongs to new material technology field, the present invention relates to a kind of silver chloride material with spination pattern and preparation method thereof.
Background technology
Silver chloride is the presoma of a kind of important photocatalyst material Ag@AgCl, and the silver chloride of preparing can obtain Ag@AgCl surface plasma photocatalyst material by photoreduction legal system.Photocatalyst material refers to by this material, the required catalyzer of photochemical reaction occurring under the effect of light, photochemical catalysis has the hydrogen manufacturing of photolysis water, the functions such as photodegradation organic pollutant and photoreduction carbonic acid gas, utilize photocatalyst material low-density sun power can be changed into the Hydrogen Energy that high-density easily stores, can utilize the various organic and inorganic pollutant in sun power degraded and mineralising environment, can also utilize sun power that carbon dioxide reduction is become to organic low-carbon alkanes, reduce the content of carbonic acid gas isothermal chamber gas in atmosphere, organic low-carbon alkanes can also be served as fuel, aspect the solution energy and environmental problem, there iing important application prospect.The Ag AgCl preparing taking silver chloride as presoma has important application in photocatalysis field, it is a kind of photocatalyst material efficiently, prepare Cubic AgCl particle, the Ag particle growth of finding reduction after photoreduction is attached on cubical eight drift angles, and Ag particle is preferentially reduced and obtains at the drift angle place of AgCl particle surface.Therefore silver chloride has multangular pattern and will strengthen the photocatalysis performance of [email protected] prior art can be prepared this special appearance silver chloride, as CN102698776A discloses a kind of silver chloride particle of preparing flower-like structure, need to add its patterns of means control such as stablizer.Therefore prior art can not form special appearance by the method control silver chloride that does not add stablizer.
Summary of the invention
The object of the invention is to solve prior art can not be by not adding the method control silver chloride of stablizer to form the problem of special appearance, and a kind of method of solid and gas phase interface method self assembly spination silver chloride is provided.
The invention provides a kind of silver chloride material with spination granule-morphology, chemical formula is AgCl, the spination that granule-morphology is.A kind of method that simultaneously the invention provides solid and gas phase interface method self assembly spination silver chloride, its concrete method is as follows:
One, weigh: be 1:(45～55 according to the mol ratio of hydrogenchloride in Silver Nitrate and concentrated hydrochloric acid) take Silver Nitrate powder and concentrated hydrochloric acid;
Two, by the concentrated hydrochloric acid thin up taking to 2.8mol/L～3.2mol/L, and be transferred in the still lining 6 of reactor;
Three, the test tube 4 that Silver Nitrate powder 2 is housed is put into the still lining 6 of reactor, utilized the interior HCl1 of test tube 4 and Silver Nitrate powder 2 interfaces that hydrochloric acid 3 evaporate into that chemical reaction occurs;
Four, by reactor 5 good seals, reaction at least 24 hours under 45～55 DEG C of conditions;
Five,, after being dried through deionized water wash 4～6 times and by product, obtain having the silver chloride material powder of spination granule-morphology.
Advantage of the present invention:
The invention provides a kind of silver chloride material with spination granule-morphology, its special appearance having is conducive to utilize the photocatalysis of its Ag@AgCl material preparing, and the inventive method can utilize solid and gas phase interface self-assembling reaction control layer by layer silver chloride to form spination pattern under the condition that does not add stablizer.The inventive method synthesis technique is simple, and composing observable by XRD figure, to go out sample purity good without dephasign, and XRD peak is high higher than its degree of crystallinity of 7000 explanations by force.
Brief description of the drawings
Fig. 1 is reaction unit figure, and in figure: 1 for evaporateing into HCl in gas phase from hydrochloric acid, and 2 be Silver Nitrate powder, and 3 is hydrochloric acid, and 4 is test tube, and 5 is reactor, 6 is reactor, and still serves as a contrast; Fig. 2 is that the spination silver chloride material powder XRD figure that obtains of embodiment 1 is composed, and in Fig. 2, XRD diffraction peak and crystal face data and PCPDS:31-1238 standard card match; Fig. 3 is the SEM collection of illustrative plates that embodiment 1 obtains spination silver chloride material powder; Fig. 4 is MO photocatalytic activity (C/C
0)-time (T) curve.
Embodiment
Embodiment one: a kind of silver chloride material with spination granule-morphology in this embodiment, chemical formula is AgCl, the spination that its granule-morphology is.
Embodiment two: in conjunction with Fig. 1, present embodiment is described, a kind of solid and gas phase interface method self assembling process of synthesizing of spination silver chloride material in this embodiment, specifically carry out according to following steps:
One, weigh: be 1:(45～55 according to the mol ratio of hydrogenchloride in Silver Nitrate and concentrated hydrochloric acid) take Silver Nitrate powder and concentrated hydrochloric acid;
Two, by the concentrated hydrochloric acid thin up taking to 2.8mol/L～3.2mol/L, and be transferred in the still lining 6 of reactor;
Three, the test tube 4 that Silver Nitrate powder 2 is housed is put into the still lining 6 of reactor, utilized the interior HCl1 of test tube 4 and Silver Nitrate powder 2 interfaces that hydrochloric acid 3 evaporate into that chemical reaction occurs;
Four, by reactor 5 good seals, reaction at least 24 hours under 45～55 DEG C of conditions;
Five,, after being dried through deionized water wash 4～6 times and by product, obtain having the silver chloride material powder of spination granule-morphology.
Embodiment three: in this embodiment, a kind of solid and gas phase interface method self assembling process of synthesizing of spination silver chloride material is in step 1 in Silver Nitrate and hydrochloric acid that in the difference of embodiment two mol ratio of hydrogenchloride is 1:50.All the other are identical with embodiment two.
Embodiment four: in this embodiment, a kind of solid and gas phase interface method self assembling process of synthesizing of spination silver chloride material is in step 3 that in the difference of embodiment two concentrated hydrochloric acid thin up is to 3.0mol/L.All the other are identical with embodiment two.
Embodiment five: in this embodiment, a kind of solid and gas phase interface method self assembling process of synthesizing of spination silver chloride material is that in the difference of embodiment two to four step 4 reacts 24 hours under 50 DEG C of conditions.All the other are identical with embodiment two to four.
Embodiment
By the following examples technical solution of the present invention is described further, but is not limited to the content of embodiment.
Embodiment 1
One, take 0.102g Silver Nitrate and put into small test tube;
Two, the dilute hydrochloric acid that the concentrated hydrochloric acid that is 60% by massfraction is 3mol/L by its dilution with distilled water in proportion;
Three, measuring 10ml concentration is that the dilute hydrochloric acid of 3mol/L packs in still lining, then the small test tube that Silver Nitrate is housed is put into still lining;
Four,, by autoclave good seal, under 50 DEG C of conditions, react 24 hours;
Five, the product of the acquisition in small test tube, through deionized water wash 6 times and after super-dry, finally obtains the powder of sample.
Test and obtain the XRD data of embodiment 1 product and by data drafting pattern 1 by XRD, the XRD diffraction peak of product and crystal face data and PCPDS:31-1238 standard card match as can be seen from Figure 1, prove that it is pure phase AgCl crystal, diffraction peak has also proved that higher than 7000 it has high-crystallinity by force.
Take embodiment 1 product by scanning electronic microscope, as shown in Figure 3, proved that it has spination pattern.
Compliance test result:
The preparation of Ag@AgCl photocatalyst:
The test 1 AgCl sample ultrasonic obtaining is dispersed in to 100mL, 10mgL
-1in MO solution, irradiate 1h with the 300W xenon lamp (λ>=400nm) that adds spectral filter and obtain Ag@AgCl photocatalyst, collect sample, use after deionized water wash 3～7, dry.
By Ag@AgCl photocatalysis Decomposition tropeolin-D:
First, the Ag@AgCl photocatalyst of getting 0.02g is placed in quartz reactor, then adds the 10mgL of 100mL
-1mO solution, lucifuge stirs 30min.
Open magnetic agitation, open xenon lamp, extract initial reaction liquid, then get the reaction solution of 4mL every 5min, centrifugal 10min, gets supernatant liquid and surveys its absorbancy with UV-Vis respectively, calculates degradation rate and by result drafting pattern 4.
After reaction 40min, the degradation rate of MO reaches more than 90% as can be known from Figure, has good photocatalysis performance.
Claims (4)
1. a solid and gas phase interface method self assembling process of synthesizing with the silver chloride material of spination granule-morphology, is characterized in that concrete preparation method carries out according to the following steps:
One, weigh: be 1:(45～55 according to the mol ratio of hydrogenchloride in Silver Nitrate and concentrated hydrochloric acid) take Silver Nitrate powder and concentrated hydrochloric acid;
Two, by the concentrated hydrochloric acid thin up taking to 2.8mol/L～3.2mol/L, and be transferred in the still lining (6) of reactor;
Three, the test tube (4) that Silver Nitrate powder (2) are housed is put into the still lining (6) of reactor, there is chemical reaction with Silver Nitrate powder (2) interface in the HCl (1) that utilizes hydrochloric acid (3) to evaporate in test tube (4), is the still lining height of hydrochloric acid liquid level < vertical height < reactor that the test tube of Silver Nitrate powder is housed at still lining camber position relationship;
Four, by reactor (5) good seal, reaction at least 24 hours under 45～55 DEG C of conditions;
Five,, after being dried through deionized water wash 4～6 times and by product, obtain having the silver chloride material powder of spination granule-morphology; The described silver chloride materials chemistry formula with spination granule-morphology is AgCl, and its granule-morphology is spination, and size is 100 μ m～200 μ m.
2. according to the solid and gas phase interface method self assembling process of synthesizing of a kind of silver chloride material with spination granule-morphology described in claim 1, it is characterized in that in step 1 in Silver Nitrate and hydrochloric acid that the mol ratio of hydrogenchloride is 1:50.
3. according to the solid and gas phase interface method self assembling process of synthesizing of a kind of silver chloride material with spination granule-morphology described in claim 2, it is characterized in that in step 2 that concentrated hydrochloric acid thin up is to 3.0mol/L.
4. according to the solid and gas phase interface method self assembling process of synthesizing of a kind of silver chloride material with spination granule-morphology described in claim 1,2 or 3, it is characterized in that step 4 reacts 24 hours under 50 DEG C of conditions.
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| CN201310520235.9A CN103523816B (en) | 2013-10-29 | 2013-10-29 | Silver chloride material with zigzag particle morphology and solid-gas phase interface self-assembling synthetic method thereof |
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| CN103523816B true CN103523816B (en) | 2014-12-03 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102698776A (en) * | 2012-05-28 | 2012-10-03 | 华北电力大学 | Method for preparing silver chloride particles with flower-shaped micrometer structures |
| CN102701266A (en) * | 2012-05-28 | 2012-10-03 | 华北电力大学 | Preparation method for leaf-shaped silver chloride particle with micron structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20130192423A1 (en) * | 2012-01-27 | 2013-08-01 | Blue Nano Inc. | Method of producing silver nanowires |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102698776A (en) * | 2012-05-28 | 2012-10-03 | 华北电力大学 | Method for preparing silver chloride particles with flower-shaped micrometer structures |
| CN102701266A (en) * | 2012-05-28 | 2012-10-03 | 华北电力大学 | Preparation method for leaf-shaped silver chloride particle with micron structure |
Non-Patent Citations (2)
| Title |
|---|
| A 3D AgCl Hierarchical Superstructure Synthesized by a Wet Chemical Oxidation Method;Zaizhu Lou et al.;《Chem. Eur. J.》;20121022;第18卷;16090-16096 * |
| Zaizhu Lou et al..A 3D AgCl Hierarchical Superstructure Synthesized by a Wet Chemical Oxidation Method.《Chem. Eur. J.》.2012,第18卷16090-16096. * |
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