CN108993551A - A kind of method that solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst - Google Patents
A kind of method that solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst Download PDFInfo
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- CN108993551A CN108993551A CN201810821987.1A CN201810821987A CN108993551A CN 108993551 A CN108993551 A CN 108993551A CN 201810821987 A CN201810821987 A CN 201810821987A CN 108993551 A CN108993551 A CN 108993551A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- -1 hydroxy chloride samarium Chemical compound 0.000 title claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 abstract description 18
- BHXBZLPMVFUQBQ-UHFFFAOYSA-K samarium(iii) chloride Chemical compound Cl[Sm](Cl)Cl BHXBZLPMVFUQBQ-UHFFFAOYSA-K 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 229960004756 ethanol Drugs 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- PEKXKKGDLJPCRA-UHFFFAOYSA-K trichlorosamarium;hydrate Chemical compound O.[Cl-].[Cl-].[Cl-].[Sm+3] PEKXKKGDLJPCRA-UHFFFAOYSA-K 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-N ethanesulfonic acid Chemical compound CCS(O)(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-N 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of methods that solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst, first weighing SmCl3·6H2O dissolves in dehydrated alcohol, obtains solution A；Then solution A is subjected to homogeneous hydro-thermal reaction；Finally to homogeneous hydro-thermal reaction after, product is washed and is dried to obtain Sm (OH)2Cl photochemical catalyst.Material prepared by the present invention has good photocatalysis performance, and the process prepared is simple and convenient.
Description
Technical field
The present invention relates to photochemical catalyst preparation fields, and in particular to a kind of solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst
Method.
Background technique
In today that industry and economy are increasingly flourishing, the problems such as energy shortage, environmental pollution, becomes increasingly severe, people
The new energy material of serious pollution and the exploitation of people's urgent need new energy and preparation environmental protection is caused to environment.
Therefore, it is very urgent with the invention improvement material of environmental problem to find the new material for preparing clean energy resource.
Currently, synthesis Sm (OH)2The method of Cl has hydro-thermal method, [Cyril Jouve, Jerome Marrot, Didier
Riou.β-Sm(OH)2Cl:a nw lamellar variety [J] Acta Crystallographica Section C] original
Material uses SmCl3·6H2O, ethylsulfonic acid prepare Sm (OH) by hydro-thermal method2Cl, needing to adjust PH during preparation is alkali
Property provides OH in reaction process under alkaline condition-, and the reaction time is 48h or so, the reaction time is longer, and preparation process pair
The PH of solution has certain requirement.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst, on overcoming
Defect of the existing technology is stated, material prepared by the present invention has good photocatalysis performance, and the process prepared is simply square
Just.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of method that solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst, comprising the following steps:
1) SmCl is weighed3·6H2O dissolves in dehydrated alcohol, obtains solution A；
2) solution A is subjected to homogeneous hydro-thermal reaction；
3) after to homogeneous hydro-thermal reaction, product is washed and is dried to obtain Sm (OH)2Cl photochemical catalyst.
Further, Sm in solution A3+Concentration be 7mol/L~8mol/L.
Further, solution A is transferred in homogeneous water heating kettle in step 2), is put into homogeneous reactor, packing ratio control
30%~40%.
Further, reaction temperature is 160~180 DEG C in step 3), and the reaction time is 5~12h.
Further, washing in step 3) specifically: by product through deionized water and dehydrated alcohol difference centrifuge washing 4~
6 times.
Further, dry in step 3) specifically: in 60 DEG C of at a temperature of dry 5~7h.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention is with six chloride hydrate samarium (SmCl3·6H2O), ethyl alcohol (C2H5OH) it is Material synthesis Sm (OH)2Cl, molten
Liquid initial stage, there are a large amount of Sm3+Ion, as the progress of reaction promotes ethyl alcohol to ionize out due to the presence of high temperature and high pressure environment
OH-, the OH that ionizes out-Replace SmCl3In Cl-To generate Sm (OH)2Cl crystallite, crystallite are continuous with the continuous progress of reaction
Increase, when solvent reaches saturation state, crystal is precipitated, while with OH-Constantly consumption, ethyl alcohol constantly ionize out OH-, to promote
The continuous progress of reaction, finally synthesizes Sm (OH)2Cl photochemical catalyst, the present invention use solvent hot preparation Sm (OH)2Cl, product
In the OH OH that directly there is ethyl alcohol to separate out in high-temperature electric-It provides, simplifies preparation step, preparation step is relatively simple.
Further, within 5~12h, time and the consumed energy is greatly saved in the reaction time, is had good
Application prospect.
Detailed description of the invention
Fig. 1 is the Sm (OH) of different time of the present invention preparation2The XRD diagram of Cl photochemical catalyst；
Fig. 2 is the Sm (OH) of different time of the present invention preparation2The SEM of Cl photochemical catalyst schemes, wherein (a) reaction time 5h；
(b) reaction time 8h；(c) reaction time 10h；(d) reaction time 12h；
Fig. 3 is Sm (OH) prepared by embodiment 32Cl degrades the degradation rate figure of MO under ultraviolet light conditions.
Specific embodiment
Embodiments of the present invention are described in further detail below:
The present invention prepares hydroxy chloride samarium photochemical catalyst by a step solvent-thermal method.Compare from preparation method, the invention
With six chloride hydrate samarium (SmCl3·6H2O), ethyl alcohol (C2H5OH) it is Material synthesis Sm (OH)2Cl, using solvent-thermal method, one-step method
Directly prepare Sm (OH)2Cl photochemical catalyst, this method reaction is heated evenly, easy to control, and that there is no other is miscellaneous for resulting product
Phase, utilization rate is high, and in addition invention institute is low using cost of material, is easy to get to target product.
Specific step is as follows:
1) a certain amount of SmCl is weighed3·6H2O dissolves in the dehydrated alcohol of 30ml~40ml, obtains institute Sm3+Concentration
In the solution of 7mol/L~8mol/L, 60min is stirred, solution A is obtained.
2) solution A is transferred in homogeneous water heating kettle, is put into homogeneous reactor, packing ratio is controlled 30%~40%, instead
Answering temperature control is 160~180 DEG C, reacts 5~12h.
3) to after reaction, take out reactant, distinguish centrifuge washing 4~6 times, 60 DEG C through deionized water and dehydrated alcohol
Sm (OH) can be obtained in dry 5~7h2Cl photochemical catalyst.
Sm (OH) prepared by the present invention2Cl material has advantageous advantage, material in terms of solving water pollution problems
Chemical energy can be converted into using luminous energy to handle the organic pollutant in water body, while material will not cause secondary dirt to environment
Dye, is a kind of novel environmental friendly materials.
Rare earth element, because having special physicochemical properties, has caused the extensive of scientific worker since being found
Concern.Rare earth element has similar electronic structure and atomic radius, because it is with the miscellaneous track of unfilled 4f electricity, make its
Light, electricity, magnetic and catalytic field are widely applied.Rare earth doped element is the effective way for improving luminescent material performance, be may be implemented
The functionalization of traditional glass and ceramics.By the unremitting effort of scientists, rare earth material is widely used to luminescent material, forever
The fields such as magnetic material, catalysis material, function ceramics, superconductor, hydrogen storage material.
China's rare earth element rich reserves provide advantageous advantage for the research of rare earth material.Sm(OH)2Cl makees
For the important component of lanthanide series compound family, there is huge application prospect in catalytic field, optical field.Solvent-thermal method
Preparing crystal has the characteristics that pollution is small, low energy consumption, easily controllable, in preparation Sm (OH)2Cl crystal has certain advantage.Sm
(OH)2Cl has huge application prospect in field of functional materials as a member in lanthanide series compound family.At present for Sm
(OH)2The research of Cl is also fewer, is concentrated mainly on the determination of its crystal structure.Sm(OH)2There are three types of crystal structures to distinguish by Cl
Are as follows: (a) monoclinic system, space group P121/m1, a=6.16, b=3.8, c=6.74, α=λ=90., β=112.17.(b)
Monoclinic system, space group P1121/m, a=6.18, b=6.75, c=3.82, α=β=90.λ=112.(c) rhombic system,
Space group is Pnma, a=12.6014, b=3.7709, c=6.2740, α=β=λ=90.It is layer structure, two-dimensional layer edge
A axis direction ordered arrangement.At present to Sm (OH)2Cl is concentrated mainly on the research of crystal structure, to its controlledly synthesis and correlation
The report of application is less.The present invention has prepared Sm (OH) using solvent-thermal method2Cl crystal.Currently, Sm (OH)2The research of Cl its
Middle solvent-thermal method is the most universal, is heated evenly, at low cost, simple and easy to control, and the sample topography of synthesis is preferable, in photocatalysis field
With potential application.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
1) SmCl of 0.21mol is weighed3·6H2O dissolves in the dehydrated alcohol of 30ml, obtains Sm3+Concentration is 7mol/L's
Solution stirs 60min, obtains solution A.
2) mixed solution A is transferred in homogeneous water heating kettle, is put into homogeneous reactor, packing ratio control is reacted 30%
Temperature control is 160 DEG C, reacts 5h.
3) to after reaction, take out reactant, distinguish centrifuge washing 6 times through deionized water and dehydrated alcohol, 60 DEG C dry
Sm (OH) can be obtained in dry 7h2Cl photochemical catalyst.
Embodiment 2
1) SmCl of 0.24mol is weighed3·6H2O dissolves in the dehydrated alcohol of 33ml, obtains Sm3+Concentration is 7.3mol/L
Solution, stir 60min, obtain solution A；
2) then mixed solution A is transferred in homogeneous water heating kettle, is put into homogeneous reactor, and packing ratio is controlled 35%, instead
Answering temperature control is 167 DEG C, reacts 8h.
3) to after reaction, take out reactant, distinguish centrifuge washing 5 times through deionized water and dehydrated alcohol, 60 DEG C dry
Sm (OH) can be obtained in dry 6h2Cl photochemical catalyst.
Embodiment 3
1) SmCl of 0.273mol is weighed3·6H2O dissolves in the dehydrated alcohol of 36ml, obtains Sm3+Concentration is 7.6mol/
The solution of L stirs 60min, obtains solution A；
2) then mixed solution A is transferred in homogeneous water heating kettle, is put into homogeneous reactor, and packing ratio is controlled 40%, instead
Answering temperature control is 174 DEG C, reacts 10h.
3) to after reaction, take out reactant, distinguish centrifuge washing 4 times through deionized water and dehydrated alcohol, 60 DEG C dry
Sm (OH) can be obtained in dry 5h2Cl photochemical catalyst.
Embodiment 4
1) SmCl of 0.32mol is weighed3·6H2O dissolves in the dehydrated alcohol of 40ml, obtains Sm3+Concentration is 8mol/L's
Solution stirs 60min, obtains solution A；
2) then mixed solution A is transferred in homogeneous water heating kettle, is put into homogeneous reactor, and packing ratio is controlled 40%, instead
Answering temperature control is 180 DEG C, reacts 12h.
3) to after reaction, take out reactant, distinguish centrifuge washing 4 times through deionized water and dehydrated alcohol, 60 DEG C dry
Sm (OH) can be obtained in dry 5h2Cl photochemical catalyst.
Fig. 1 is Sm (OH) of the present invention prepared by differential responses2The XRD diagram of Cl photochemical catalyst, as can be seen from the figure
Prepared sample and standard card PFD72-2212 (Sm (OH)2Cl peak) corresponds and object is compared pure, and Fig. 2 is to react not
Sm (OH) is prepared with the time2The SEM of Cl schemes, and is that the SEM of reaction time sample in 5h, 8h, 10h and 12h schemes.As seen from the figure when
When reaction time is 5h as shown in (a), sample is largely tiny graininess, in local growth at small sheet.Work as reaction
When time proceeds to 8h as shown in (b), it is about 200-400nm's that sample microstructure, which is changed into small sheet to be piled into thickness,
Bulk, and self assembly is together, the formation of this structure may be in order to reduce the surface energy of sample caused by.Reaction continue into
Row, when reacted between when reaching 10h as shown in (c), the laminated structure of sample is more obvious, and being increased by the strip of 8h is length and width
About 1 μm of big sheet, and be packed together, but wherein still have sub-fraction sample that graininess and strip is presented,
Show that the structural development of sample at this time is imperfect.When reaching 12h with the reaction time as shown in figure (d), sample is showed by straight
Diameter is about 0.8-1.5 μm, and thickness is about the cube structure that the piece of 50nm is piled into.Fig. 3 is (Sm (OH)2Cl) ultraviolet
The degradation rate figure of degradation MO under striation part, from figure 3, it can be seen that degradation efficiency reaches 75% after ultraviolet lighting 30min,
With good degradation efficiency.
Claims (6)
1. a kind of method that solvent-thermal method prepares hydroxy chloride samarium photochemical catalyst, which comprises the following steps:
1) SmCl is weighed3·6H2O dissolves in dehydrated alcohol, obtains solution A；
2) solution A is subjected to homogeneous hydro-thermal reaction；
3) after to homogeneous hydro-thermal reaction, product is washed and is dried to obtain Sm (OH)2Cl photochemical catalyst.
2. the method that a kind of solvent-thermal method according to claim 1 prepares hydroxy chloride samarium photochemical catalyst, which is characterized in that
Sm in solution A3+Concentration be 7mol/L~8mol/L.
3. the method that a kind of solvent-thermal method according to claim 1 prepares hydroxy chloride samarium photochemical catalyst, which is characterized in that
Solution A is transferred in homogeneous water heating kettle in step 2), is put into homogeneous reactor, packing ratio is controlled 30%~40%.
4. the method that a kind of solvent-thermal method according to claim 1 prepares hydroxy chloride samarium photochemical catalyst, which is characterized in that
Reaction temperature is 160~180 DEG C in step 3), and the reaction time is 5~12h.
5. the method that a kind of solvent-thermal method according to claim 1 prepares hydroxy chloride samarium photochemical catalyst, which is characterized in that
Washing in step 3) specifically: distinguish product centrifuge washing 4~6 times through deionized water and dehydrated alcohol.
6. the method that a kind of solvent-thermal method according to claim 1 prepares hydroxy chloride samarium photochemical catalyst, which is characterized in that
It is dry in step 3) specifically: in 60 DEG C of at a temperature of dry 5~7h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974130A (en) * | 2022-12-02 | 2023-04-18 | 吉林大学 | Hydroxyl samarium chloride nano material and preparation method thereof |
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| CN102432056A (en) * | 2011-10-13 | 2012-05-02 | 陕西科技大学 | Method for preparing Sm2O3 nano crystals by solvent thermal method |
| CN102897822A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Method for preparing monoclinic Sm2O3 nanocrystal through solvothermal method |
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2018
- 2018-07-24 CN CN201810821987.1A patent/CN108993551A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432056A (en) * | 2011-10-13 | 2012-05-02 | 陕西科技大学 | Method for preparing Sm2O3 nano crystals by solvent thermal method |
| CN102897822A (en) * | 2012-10-19 | 2013-01-30 | 陕西科技大学 | Method for preparing monoclinic Sm2O3 nanocrystal through solvothermal method |
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| LIXIONG YIN ET AL: "Red AgCl/SmOCl Z-scheme composites: Enhanced photocatalytic performance under sunlight", 《MATERIALS LETTERS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115974130A (en) * | 2022-12-02 | 2023-04-18 | 吉林大学 | Hydroxyl samarium chloride nano material and preparation method thereof |
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Application publication date: 20181214 |