CN103922412A - A method for preparing sheet-like SmWO4(OH) by microwave hydrothermal method - Google Patents

A method for preparing sheet-like SmWO4(OH) by microwave hydrothermal method Download PDF

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CN103922412A
CN103922412A CN201410155185.3A CN201410155185A CN103922412A CN 103922412 A CN103922412 A CN 103922412A CN 201410155185 A CN201410155185 A CN 201410155185A CN 103922412 A CN103922412 A CN 103922412A
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microwave hydrothermal
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黄剑锋
李颖慧
李嘉胤
卢靖
曹丽云
李翠艳
吴建鹏
孔新刚
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Yancheng Julonghu Business Cluster Development Co ltd
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Shaanxi University of Science and Technology
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Abstract

本发明提供一种微波水热法制备片状SmWO4(OH)的方法:将Na2WO4溶液滴加至SmCl3溶液中,不断搅拌得到白色悬浊液,调节白色悬浊液的pH=6~9得到微波水热前驱液,在微波水热反应仪中180~220℃下反应60~90min,然后离心分离、洗涤、干燥得到片状SmWO4(OH)微晶,本发明采用湿化学法制备片状SmWO4(OH),微波水热法工艺过程简单,反应温度较低,时间短,工艺参数易控制,无需高温长时间反应或气氛保护,无需后续处理,可快速制备出高纯度的片状SmWO4(OH)。The present invention provides a method for preparing flaky SmWO 4 (OH) by microwave hydrothermal method: drop Na 2 WO 4 solution into SmCl 3 solution, stir continuously to obtain white suspension, and adjust the pH of the white suspension to 6-9 to obtain the microwave hydrothermal precursor solution, react in a microwave hydrothermal reactor at 180-220°C for 60-90min, then centrifuge, wash, and dry to obtain flaky SmWO 4 (OH) microcrystals. The present invention adopts wet chemical SmWO 4 (OH) is prepared by the microwave hydrothermal method, the process of the microwave hydrothermal method is simple, the reaction temperature is low, the time is short, the process parameters are easy to control, no high temperature long-term reaction or atmosphere protection is required, and no follow-up treatment is required, and high-purity flaky SmWO 4 (OH).

Description

一种微波水热法制备片状SmWO4(OH)的方法A method for preparing sheet-like SmWO4(OH) by microwave hydrothermal method

技术领域technical field

本发明涉及一种SmWO4(OH)的制备方法,特别涉及一种采用微波水热法制备片状SmWO4(OH)的方法。The invention relates to a method for preparing SmWO 4 (OH), in particular to a method for preparing flaky SmWO 4 (OH) by using a microwave hydrothermal method.

背景技术Background technique

钨酸钐是钨酸盐系列中的一员,是一种很有潜力却研究相对较少的新型光催化剂,在光催化降解水中有机污染物和光解水制氢等领域都具有良好的应用前景。对钨酸钐的制备方法的开发,在光催化领域的理论及应用方面都具有重要意义。另外,钨酸钐还可能具有顺磁性、铁电、压电、热释电、非线性电极化率、负热膨胀性等特殊性能,具有广泛的应用前景。Samarium tungstate is a member of the tungstate series. It is a new photocatalyst with great potential but relatively little research. It has good application prospects in the fields of photocatalytic degradation of organic pollutants in water and hydrogen production by photolysis of water. . The development of the preparation method of samarium tungstate is of great significance in the theory and application of photocatalysis. In addition, samarium tungstate may also have special properties such as paramagnetism, ferroelectricity, piezoelectricity, pyroelectricity, nonlinear electrical susceptibility, and negative thermal expansion, and has broad application prospects.

目前对钨酸盐的报道主要集中在Bi2WO6、CaWO4、FeWO4、BaWO4等物质,而对钨酸钐及碱式钨酸钐的报道还很少见,现有报道中采用的制备方法多为固相反应法。At present, the reports on tungstate mainly focus on Bi 2 WO 6 , CaWO 4 , FeWO 4 , BaWO 4 and other substances, while the reports on samarium tungstate and basic samarium tungstate are still rare. The preparation method is mostly solid phase reaction method.

E.Tomaszewicz通过固相反应法,以Sm2O3和WO3为原料制备了Sm2WO6晶体[E.Tomaszewicz.Reactivity in the solid state between CoWO4and RE2WO6where RE=Sm,Eu,Gd.Thermochimica Acta,447(2006)69-74]。P.Urbanowicz等人也用类似方法合成了Sm2WO6晶体[P.Urbanowicz,E.Tomaszewicz,et al.Magnetic properties of R2WO6(where R=Nd,Sm,Eu,Gd,Dy and Ho).Physica B,404(2009)2213-2217]。固相反应法制备钨酸钐,需要将原料Sm2O3和WO3按比例均匀混合,然后加热到较高温度(800℃~1200℃),保温较长时间(12~24h),得到产品。这种方法具有高产率、工艺简单等优点,然而反应需在高温下进行、制备周期较长、能耗大,不符合目前追求绿色、环保、节能、高效的趋势。E.Tomaszewicz prepared Sm 2 WO 6 crystals with Sm 2 O 3 and WO 3 as raw materials by solid state reaction [E.Tomaszewicz.Reactivity in the solid state between CoWO 4 and RE 2 WO 6 where RE=Sm,Eu , Gd. Thermochimica Acta, 447 (2006) 69-74]. P.Urbanowicz et al. also used a similar method to synthesize Sm 2 WO 6 crystals [P.Urbanowicz, E.Tomaszewicz, et al.Magnetic properties of R 2 WO 6 (where R=Nd,Sm,Eu,Gd,Dy and Ho ). Physica B, 404 (2009) 2213-2217]. The preparation of samarium tungstate by solid phase reaction method requires the raw materials Sm 2 O 3 and WO 3 to be uniformly mixed in proportion, then heated to a higher temperature (800°C-1200°C) and kept for a long time (12-24h) to obtain the product . This method has the advantages of high yield and simple process. However, the reaction needs to be carried out at high temperature, the preparation cycle is long, and the energy consumption is large, which is not in line with the current trend of pursuing green, environmental protection, energy saving, and high efficiency.

在关于钨酸盐的已有报道中,湿化学法成为主流制备方法,如液相反应法、微乳液法、溶剂热法、水热法等,其中水热法和微波水热法是报道最多的方法。Gao Chunmei等在200℃下将Bi(NO3)3·5H2O和Na2WO4·2H2O制备的前驱液进行水热反应20h,制备了Bi2WO6粉体[Gao C M,Wang Z Y.Effect of pH Valueson Photocatalytic Properties of Bi2WO6Synthesized by Hydrothermal Method.Journal of Wuhan University of Technology-Mater.Sci.Ed,24(2009):533-536];黄毅等用Bi(NO3)3·5H2O和Na2WO4·2H2O制备前驱液,在180℃分别反应2、4、6、12、24、36、48h,得到Bi2WO6粉体[黄毅,申玥.花状Bi2WO6光催化剂的制备及性能研究.功能材料,2010,增I(41):52-56]。In the existing reports on tungstate, wet chemical method has become the mainstream preparation method, such as liquid phase reaction method, microemulsion method, solvothermal method, hydrothermal method, etc., among which hydrothermal method and microwave hydrothermal method are the most reported. Methods. Gao Chunmei et al. prepared Bi 2 WO 6 powder by hydrothermally reacting the precursor solution prepared by Bi(NO 3 ) 3 .5H 2 O and Na 2 WO 4 .2H 2 O at 200°C for 20 hours [Gao C M, Wang Z Y.Effect of pH Value on Photocatalytic Properties of Bi 2 WO 6 Synthesized by Hydrothermal Method.Journal of Wuhan University of Technology-Mater.Sci.Ed, 24(2009):533-536]; Huang Yi et al. used Bi(NO 3 ) 3 ·5H 2 O and Na 2 WO 4 ·2H 2 O to prepare the precursor solution, react at 180°C for 2, 4, 6, 12, 24, 36, 48 hours respectively to obtain Bi 2 WO 6 powder [Huang Yi, Shen Yue. Preparation and properties of flower-like Bi 2 WO 6 photocatalyst. Functional Materials, 2010, Zeng I(41):52-56].

发明内容Contents of the invention

本发明的目的在于提供一种微波水热法制备片状SmWO4(OH)的方法,此方法工艺过程简单,参数易控制,温度低,生产时间短,可以制备高纯度的片状SmWO4(OH)。The object of the present invention is to provide a method for preparing flaky SmWO 4 (OH) by microwave hydrothermal method. The process of this method is simple, the parameters are easy to control, the temperature is low, the production time is short, and high-purity flaky SmWO 4 (OH) can be prepared. OH).

为达到上述目的,本发明采用了以下技术方案:To achieve the above object, the present invention adopts the following technical solutions:

步骤一:将SmCl3·6H2O和Na2WO4·2H2O分别加入去离子水中,然后搅拌5~15min得到SmCl3溶液和Na2WO4溶液;Step 1: Add SmCl 3 6H 2 O and Na 2 WO 4 2H 2 O to deionized water respectively, and then stir for 5-15 minutes to obtain SmCl 3 solution and Na 2 WO 4 solution;

步骤二:将Na2WO4溶液滴加至SmCl3溶液中,不断搅拌(5~10分钟)得到白色悬浊液,控制Sm:W的摩尔比=1.5~2.5:1,且W6+浓度为0.01~0.06mol/L;Step 2: Add the Na 2 WO 4 solution dropwise to the SmCl 3 solution, and keep stirring (5-10 minutes) to obtain a white suspension. Control the molar ratio of Sm:W=1.5-2.5:1, and the concentration of W 6+ 0.01~0.06mol/L;

步骤三:用NaOH水溶液调节白色悬浊液的pH至6~9,并持续搅拌10~30min,得到微波水热前驱液;Step 3: adjust the pH of the white suspension to 6-9 with NaOH aqueous solution, and keep stirring for 10-30 minutes to obtain a microwave hydrothermal precursor;

步骤四:将微波水热前驱液装入聚四氟乙烯反应釜中,然后将聚四氟乙烯反应釜密封后放入微波水热反应仪中,并在180~220℃下反应60~90min,反应结束后自然冷却至室温;Step 4: Put the microwave hydrothermal precursor solution into the polytetrafluoroethylene reactor, then seal the polytetrafluoroethylene reactor and put it into the microwave hydrothermal reactor, and react at 180-220°C for 60-90 minutes, Naturally cool to room temperature after reaction finishes;

步骤五:经过步骤四后,打开聚四氟乙烯反应釜,将反应得到的产物离心分离得到沉淀,将沉淀依次用去离子水和无水乙醇洗涤后放入真空干燥箱并在50~60℃下烘干,即可得到片状SmWO4(OH)微晶。Step 5: After step 4, open the polytetrafluoroethylene reaction kettle, centrifuge the product obtained from the reaction to obtain a precipitate, wash the precipitate with deionized water and absolute ethanol in turn, put it in a vacuum drying oven and store it at 50-60°C Drying at a lower temperature can obtain flaky SmWO 4 (OH) microcrystals.

所述NaOH水溶液的浓度为0.2~1mol/L。The concentration of the NaOH aqueous solution is 0.2˜1 mol/L.

所述微波水热前驱液在聚四氟乙烯反应釜中的填充比为20~50%。The filling ratio of the microwave hydrothermal precursor solution in the polytetrafluoroethylene reactor is 20-50%.

本发明的有益效果体现在:The beneficial effects of the present invention are reflected in:

本发明采用湿化学法制备片状SmWO4(OH),微波水热法工艺过程简单,反应温度较低,时间短,工艺参数易控制,无需高温长时间反应或气氛保护,无需后续处理,可快速制备出高纯度的片状SmWO4(OH),使用本发明方法制得的SmWO4(OH)粉体在光催化降解有机污染物和光解水制氢等领域有广阔的研究和应用价值。The invention adopts a wet chemical method to prepare flake SmWO 4 (OH), and the microwave hydrothermal method has a simple process, a low reaction temperature, a short time, easy control of process parameters, no need for high-temperature long-term reaction or atmosphere protection, and no need for subsequent treatment. High-purity flaky SmWO 4 (OH) can be quickly prepared, and the SmWO 4 (OH) powder prepared by the method of the invention has broad research and application value in the fields of photocatalytic degradation of organic pollutants and photolysis of water to produce hydrogen.

附图说明Description of drawings

图1为本发明实施例1制备的SmWO4(OH)微晶的X-射线衍射(XRD)图谱。Fig. 1 is an X-ray diffraction (XRD) pattern of SmWO 4 (OH) microcrystals prepared in Example 1 of the present invention.

图2为本发明实施例1制备的SmWO4(OH)微晶的扫描电镜(SEM)照片。Fig. 2 is a scanning electron microscope (SEM) photo of the SmWO 4 (OH) microcrystal prepared in Example 1 of the present invention.

图3为紫外照射下降解Rh-B的降解速率-时间图,S1-S4分别对应实施例1-实施例4。Fig. 3 is a degradation rate-time diagram of Rh-B degradation under ultraviolet irradiation, and S1-S4 correspond to Example 1-Example 4, respectively.

具体实施方式Detailed ways

下面结合附图及实施例对本发明做详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and embodiments.

实施例1:Example 1:

步骤一:将分析纯SmCl3·6H2O和Na2WO4·2H2O分别加入一定量的去离子水中,在磁力搅拌器上搅拌5min得到透明溶液A(SmCl3溶液)和透明溶液B(Na2WO4溶液);Step 1: Add analytically pure SmCl 3 6H 2 O and Na 2 WO 4 2H 2 O to a certain amount of deionized water, stir on a magnetic stirrer for 5 minutes to obtain transparent solution A (SmCl 3 solution) and transparent solution B ( Na2WO4 solution) ;

步骤二:将透明溶液B缓慢滴加至透明溶液A中,不断搅拌得到白色悬浊液,控制Sm:W=2:1(摩尔比),W6+浓度为0.05mol/L;Step 2: Slowly add the transparent solution B to the transparent solution A, and keep stirring to obtain a white suspension. Control Sm:W=2:1 (molar ratio), and the concentration of W 6+ is 0.05mol/L;

步骤三:用浓度为0.5mol/L的NaOH水溶液调节白色悬浊液的pH=7,并持续搅拌30min,得到微波水热前驱液;Step 3: Adjust the pH of the white suspension to 7 with an aqueous NaOH solution with a concentration of 0.5mol/L, and continue stirring for 30 minutes to obtain a microwave hydrothermal precursor;

步骤四:将微波水热前驱液装入聚四氟乙烯反应釜中,填充比为40%,密封聚四氟乙烯反应釜,放入微波水热反应仪中,在220℃下反应90min,反应结束后自然冷却至室温;Step 4: Put the microwave hydrothermal precursor solution into the polytetrafluoroethylene reactor with a filling ratio of 40%, seal the polytetrafluoroethylene reactor, put it into the microwave hydrothermal reactor, and react at 220°C for 90 minutes. Naturally cool to room temperature after finishing;

步骤五:打开聚四氟乙烯反应釜,将反应得到的产物离心分离得到沉淀,依次用去离子水和无水乙醇洗涤沉淀,将洗涤后的沉淀放入真空干燥箱并在60℃下烘干,即可得到片状SmWO4(OH)微晶。Step 5: Open the polytetrafluoroethylene reactor, centrifuge the product obtained from the reaction to obtain a precipitate, wash the precipitate with deionized water and absolute ethanol in turn, put the washed precipitate into a vacuum drying oven and dry it at 60°C , you can get flaky SmWO 4 (OH) microcrystals.

参见图1,X-射线衍射(XRD)图谱显示本实施例所得产物为纯相SmWO4(OH),结晶性较好。参见图2,从扫描电镜(SEM)照片中可见,本实施例所得产物具有不规则片状的微观形貌。Referring to Fig. 1, the X-ray diffraction (XRD) pattern shows that the product obtained in this example is a pure phase SmWO 4 (OH) with good crystallinity. Referring to Fig. 2, it can be seen from the scanning electron microscope (SEM) photo that the product obtained in this example has an irregular sheet-like microscopic appearance.

实施例2:Example 2:

步骤一:将分析纯SmCl3·6H2O和Na2WO4·2H2O分别加入一定量的去离子水中,在磁力搅拌器上搅拌5min得到透明溶液A(SmCl3溶液)和透明溶液B(Na2WO4溶液);Step 1: Add analytically pure SmCl 3 6H 2 O and Na 2 WO 4 2H 2 O to a certain amount of deionized water, stir on a magnetic stirrer for 5 minutes to obtain transparent solution A (SmCl 3 solution) and transparent solution B ( Na2WO4 solution) ;

步骤二:将透明溶液B缓慢滴加至透明溶液A中,不断搅拌得到白色悬浊液,控制Sm:W=1.5:1(摩尔比),W6+浓度为0.06mol/L;Step 2: Slowly add the transparent solution B to the transparent solution A, and keep stirring to obtain a white suspension. Control Sm:W=1.5:1 (molar ratio), and the concentration of W 6+ is 0.06mol/L;

步骤三:用浓度为0.8mol/L的NaOH水溶液调节白色悬浊液的pH=8,并持续搅拌10min,得到微波水热前驱液;Step 3: Adjust the pH of the white suspension to 8 with an aqueous NaOH solution with a concentration of 0.8 mol/L, and keep stirring for 10 minutes to obtain a microwave hydrothermal precursor;

步骤四:将微波水热前驱液装入聚四氟乙烯反应釜中,填充比为50%,密封聚四氟乙烯反应釜,放入微波水热反应仪中,在220℃下反应60min,反应结束后自然冷却至室温;Step 4: Put the microwave hydrothermal precursor liquid into the polytetrafluoroethylene reactor with a filling ratio of 50%, seal the polytetrafluoroethylene reactor, put it into the microwave hydrothermal reactor, and react at 220°C for 60 minutes. Naturally cool to room temperature after finishing;

步骤五:打开聚四氟乙烯反应釜,将反应得到的产物离心分离得到沉淀,依次用去离子水和无水乙醇洗涤沉淀,将洗涤后的沉淀放入真空干燥箱并在50℃下烘干,即可得到片状SmWO4(OH)微晶。Step 5: Open the polytetrafluoroethylene reactor, centrifuge the product obtained from the reaction to obtain a precipitate, wash the precipitate with deionized water and absolute ethanol in turn, put the washed precipitate into a vacuum drying oven and dry it at 50°C , you can get flaky SmWO 4 (OH) microcrystals.

实施例3:Example 3:

步骤一:将分析纯SmCl3·6H2O和Na2WO4·2H2O分别加入一定量的去离子水中,在磁力搅拌器上搅拌15min得到透明溶液A(SmCl3溶液)和透明溶液B(Na2WO4溶液);Step 1: Add analytically pure SmCl 3 6H 2 O and Na 2 WO 4 2H 2 O to a certain amount of deionized water, stir on a magnetic stirrer for 15 minutes to obtain transparent solution A (SmCl 3 solution) and transparent solution B ( Na2WO4 solution) ;

步骤二:将透明溶液B缓慢滴加至透明溶液A中,不断搅拌得到白色悬浊液,控制Sm:W=2.5:1(摩尔比),W6+浓度为0.025mol/L;Step 2: Slowly add the transparent solution B to the transparent solution A, and keep stirring to obtain a white suspension. Control Sm:W=2.5:1 (molar ratio), and the concentration of W 6+ is 0.025mol/L;

步骤三:用浓度为1mol/L的NaOH水溶液调节白色悬浊液的pH=9,并持续搅拌15min,得到微波水热前驱液;Step 3: Adjust the pH of the white suspension to 9 with an aqueous NaOH solution with a concentration of 1mol/L, and keep stirring for 15 minutes to obtain a microwave hydrothermal precursor;

步骤四:将微波水热前驱液装入聚四氟乙烯反应釜中,填充比为20%,密封聚四氟乙烯反应釜,放入微波水热反应仪中,在180℃下反应90min,反应结束后自然冷却至室温;Step 4: Put the microwave hydrothermal precursor liquid into the polytetrafluoroethylene reactor with a filling ratio of 20%, seal the polytetrafluoroethylene reactor, put it into the microwave hydrothermal reactor, and react at 180°C for 90 minutes. Naturally cool to room temperature after finishing;

步骤五:打开聚四氟乙烯反应釜,将反应得到的产物离心分离得到沉淀,依次用去离子水和无水乙醇洗涤沉淀,将洗涤后的沉淀放入真空干燥箱并在60℃下烘干,即可得到片状SmWO4(OH)微晶。Step 5: Open the polytetrafluoroethylene reactor, centrifuge the product obtained from the reaction to obtain a precipitate, wash the precipitate with deionized water and absolute ethanol in turn, put the washed precipitate into a vacuum drying oven and dry it at 60°C , you can get flaky SmWO 4 (OH) microcrystals.

实施例4:Example 4:

步骤一:将分析纯SmCl3·6H2O和Na2WO4·2H2O分别加入一定量的去离子水中,在磁力搅拌器上搅拌10min得到透明溶液A(SmCl3溶液)和透明溶液B(Na2WO4溶液);Step 1: Add analytically pure SmCl 3 6H 2 O and Na 2 WO 4 2H 2 O to a certain amount of deionized water respectively, and stir on a magnetic stirrer for 10 minutes to obtain transparent solution A (SmCl 3 solution) and transparent solution B ( Na2WO4 solution) ;

步骤二:将透明溶液B缓慢滴加至透明溶液A中,不断搅拌得到白色悬浊液,控制Sm:W=1.5:1(摩尔比),W6+浓度为0.03mol/L;Step 2: Slowly add the transparent solution B to the transparent solution A, and keep stirring to obtain a white suspension. Control Sm:W=1.5:1 (molar ratio), and the concentration of W 6+ is 0.03mol/L;

步骤三:用浓度为0.2mol/L的NaOH水溶液调节白色悬浊液的pH=6,并持续搅拌10min,得到微波水热前驱液;Step 3: Adjust the pH of the white suspension to 6 with an aqueous NaOH solution with a concentration of 0.2mol/L, and keep stirring for 10 minutes to obtain a microwave hydrothermal precursor;

步骤四:将微波水热前驱液装入聚四氟乙烯反应釜中,填充比为30%,密封聚四氟乙烯反应釜,放入微波水热反应仪中,在180℃下反应60min,反应结束后自然冷却至室温;Step 4: Put the microwave hydrothermal precursor liquid into the polytetrafluoroethylene reactor with a filling ratio of 30%, seal the polytetrafluoroethylene reactor, put it into the microwave hydrothermal reactor, and react at 180°C for 60 minutes. Naturally cool to room temperature after finishing;

步骤五:打开聚四氟乙烯反应釜,将反应得到的产物离心分离得到沉淀,依次用去离子水和无水乙醇洗涤沉淀,将洗涤后的沉淀放入真空干燥箱并在60℃下烘干,即可得到片状SmWO4(OH)微晶。Step 5: Open the polytetrafluoroethylene reactor, centrifuge the product obtained from the reaction to obtain a precipitate, wash the precipitate with deionized water and absolute ethanol in turn, put the washed precipitate into a vacuum drying oven and dry it at 60°C , you can get flaky SmWO 4 (OH) microcrystals.

本发明创新性地采用微波水热方法,在较低温度下合成片状SmWO4(OH),设备简单,容易控制,周期短,可以快速合成SmWO4(OH)。经检测实施例1-实施例4所制备的片状SmWO4(OH)具有明显的光催化活性。图3为紫外光照射下降解Rh-B的降解速率-时间图,从图3中可看出,与空白对比测试相比,实施例1-实施例4制备出的片状SmWO4(OH)对Rh-B具有明显的光催化降解活性。The present invention innovatively adopts a microwave hydrothermal method to synthesize sheet-like SmWO 4 (OH) at relatively low temperature, has simple equipment, is easy to control, and has a short cycle, and can quickly synthesize SmWO 4 (OH). It is tested that the sheet-like SmWO 4 (OH) prepared in Examples 1-4 has obvious photocatalytic activity. Fig. 3 is the degradation rate-time diagram of degrading Rh-B under ultraviolet light irradiation, as can be seen from Fig. 3, compared with the blank comparative test, the flaky SmWO 4 (OH) prepared in embodiment 1-embodiment 4 It has obvious photocatalytic degradation activity on Rh-B.

Claims (3)

1.一种微波水热法制备片状SmWO4(OH)的方法,其特征在于:包括以下步骤:1. A method for preparing sheet-like SmWO 4 (OH) by microwave hydrothermal method, is characterized in that: comprise the following steps: 步骤一:将SmCl3·6H2O和Na2WO4·2H2O分别加入去离子水中得到SmCl3溶液和Na2WO4溶液;Step 1: adding SmCl 3 6H 2 O and Na 2 WO 4 2H 2 O to deionized water respectively to obtain SmCl 3 solution and Na 2 WO 4 solution; 步骤二:将Na2WO4溶液滴加至SmCl3溶液中,不断搅拌得到白色悬浊液,控制Sm:W的摩尔比=1.5~2.5:1,且W6+浓度为0.01~0.06mol/L;Step 2: Add the Na 2 WO 4 solution dropwise to the SmCl 3 solution, and keep stirring to obtain a white suspension. Control the molar ratio of Sm:W=1.5~2.5:1, and the concentration of W 6+ is 0.01~0.06mol/ L; 步骤三:用NaOH水溶液调节白色悬浊液的pH至6~9,并持续搅拌10~30min,得到微波水热前驱液;Step 3: adjust the pH of the white suspension to 6-9 with NaOH aqueous solution, and keep stirring for 10-30 minutes to obtain a microwave hydrothermal precursor; 步骤四:将微波水热前驱液装入聚四氟乙烯反应釜中,然后将聚四氟乙烯反应釜密封后放入微波水热反应仪中,并在180~220℃下反应60~90min,反应结束后自然冷却至室温;Step 4: Put the microwave hydrothermal precursor solution into the polytetrafluoroethylene reactor, then seal the polytetrafluoroethylene reactor and put it into the microwave hydrothermal reactor, and react at 180-220°C for 60-90 minutes, Naturally cool to room temperature after reaction finishes; 步骤五:打开聚四氟乙烯反应釜,将反应得到的产物离心分离得到沉淀,将沉淀依次用去离子水和无水乙醇洗涤后放入真空干燥箱并在50~60℃下烘干,即可得到片状SmWO4(OH)微晶。Step 5: Open the polytetrafluoroethylene reaction kettle, centrifuge the product obtained from the reaction to obtain a precipitate, wash the precipitate with deionized water and absolute ethanol in turn, put it into a vacuum drying oven and dry it at 50-60°C, that is The flaky SmWO 4 (OH) microcrystals can be obtained. 2.根据权利要求1所述一种微波水热法制备片状SmWO4(OH)的方法,其特征在于:所述NaOH水溶液的浓度为0.2~1mol/L。2. A method for preparing flaky SmWO 4 (OH) by microwave hydrothermal method according to claim 1, characterized in that: the concentration of the NaOH aqueous solution is 0.2-1 mol/L. 3.根据权利要求1所述一种微波水热法制备片状SmWO4(OH)的方法,其特征在于:所述微波水热前驱液在聚四氟乙烯反应釜中的填充比为20~50%。3. A method for preparing flaky SmWO 4 (OH) by microwave hydrothermal method according to claim 1, characterized in that: the filling ratio of the microwave hydrothermal precursor solution in the polytetrafluoroethylene reactor is 20- 50%.
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CN111874959A (en) * 2020-08-18 2020-11-03 王星星 SmMoO4(OH)-Ni(OH)2Preparation method of nanosheet

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CN105016372A (en) * 2015-07-27 2015-11-04 陕西科技大学 A preparation method of self-assembled wheat spike-shaped Sm2CO3(OH) nanomaterials
CN106587152A (en) * 2016-12-12 2017-04-26 南京工业大学 Rare earth two-dimensional material EuMoO 4 (OH) nanosheet and preparation method and application thereof
CN106735166A (en) * 2016-12-12 2017-05-31 南京工业大学 EuWO4(OH) nanobelt and preparation method of composite material thereof
CN111874959A (en) * 2020-08-18 2020-11-03 王星星 SmMoO4(OH)-Ni(OH)2Preparation method of nanosheet
CN111874959B (en) * 2020-08-18 2024-01-30 王星星 SmMoO 4 (OH)-Ni(OH) 2 Preparation method of nano-sheet

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