CN104741108B - A low-temperature preparation method of γ-phase bismuth oxide (γ-Bi2O3) photocatalyst - Google Patents
A low-temperature preparation method of γ-phase bismuth oxide (γ-Bi2O3) photocatalyst Download PDFInfo
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Abstract
本发明涉及一种γ‑Bi2O3光催化剂的低温制备方法。（1）配制一定浓度的Bi(NO3)3的硝酸溶液；（2）配制一定浓度强碱性水溶液，将其置于50~95℃水浴条件下恒温加热；（3）将（1）中所得的Bi(NO3)3溶液缓慢加入到强碱性水溶液中，搅拌0.5~24 h；（4）将上述所得样品冷却至室温，经过离心、洗涤、干燥即可得γ‑Bi2O3光催化剂。
The invention relates to a low-temperature preparation method of a gamma - Bi2O3 photocatalyst. (1) Prepare a certain concentration of Bi(NO 3 ) 3 nitric acid solution; (2) Prepare a certain concentration of strong alkaline aqueous solution, and place it in a water bath at 50-95°C for constant temperature heating; (3) Put (1) The obtained Bi(NO 3 ) 3 solution was slowly added into a strong alkaline aqueous solution, and stirred for 0.5~24 h; (4) Cool the above obtained sample to room temperature, centrifuge, wash and dry to obtain γ‑Bi 2 O 3 catalyst of light.
Description
技术领域technical field
本发明是一种γ-Bi2O3光催化剂的低温制备方法，属于材料制备领域。The invention relates to a low-temperature preparation method of a gamma - Bi2O3 photocatalyst, which belongs to the field of material preparation.
背景技术Background technique
Bi2O3作为一种功能性半导体材料已经渗透到人类的生产和生活中，特别是在电子陶瓷工业、有机合成催化等领域已得到广泛应用。同时氧化铋因其独特的光学性能，使其在能源利用与环境保护方面显示出诱人的前景，被认为是一种潜在的光催化剂材料。Bi2O3属于p-型半导体，是一种先进的半导体光催化材料。Bi2O3具有多种晶体结构：面心立方相δ-Bi2O3，体心立方相γ-Bi2O3，四方相β-Bi2O3，单斜相α-Bi2O3。随晶体结构的不同，带隙宽度在2.38~3.96 eV之间变化。由于不同晶型之间禁带宽度差别较大，作为光催化剂时，其光催化活性也表现出较大的差异。As a functional semiconductor material, Bi 2 O 3 has penetrated into human production and life, especially in the fields of electronic ceramics industry and organic synthesis catalysis. At the same time, due to its unique optical properties, bismuth oxide shows attractive prospects in energy utilization and environmental protection, and is considered as a potential photocatalyst material. Bi 2 O 3 belongs to p-type semiconductor and is an advanced semiconductor photocatalytic material. Bi 2 O 3 has a variety of crystal structures: face-centered cubic phase δ-Bi 2 O 3 , body-centered cubic phase γ-Bi 2 O 3 , tetragonal phase β-Bi 2 O 3 , monoclinic phase α-Bi 2 O 3 . With different crystal structures, the bandgap width varies between 2.38 and 3.96 eV. Due to the large difference in the band gap between different crystal forms, when used as a photocatalyst, its photocatalytic activity also shows a large difference.
γ-Bi2O3因其理想的禁带宽度和高效的电子和空穴分离效率，在Bi2O3的三种晶型中，被认为是光催化效果最好的氧化铋晶型。但是γ-Bi2O3为高温亚稳晶相，难以在低温条件下合成与制备。γ-Bi2O3的生产大多采用高温煅烧和其它一些高温处理，例如：专利CN102491417A中公开了一种花球形γ-Bi2O3制备方法，但是该发明采用的是水热合成方法，需要在同时具备高温高压条件下才能进行，对实验设备的耐压性及耐热性都有很高的要求，而且所制备产品的纯度较低。文献Weichang Hao等(J. Mater. Sci. Technol.,2014,30(2),192-196)通过沉淀法生产出前驱体，在353℃条件下干燥12 h，然后再经过773℃条件下焙烧2 h，反应过程中需要长时间高温干燥及焙烧，而且制备路线较为复杂，使催化剂的制备成本增高，限制了其实际应用。Among the three crystal forms of Bi 2 O 3 , γ-Bi 2 O 3 is considered to be the bismuth oxide crystal form with the best photocatalytic effect because of its ideal band gap and high electron and hole separation efficiency. But γ-Bi 2 O 3 is a high-temperature metastable crystal phase, which is difficult to synthesize and prepare at low temperature. The production of γ-Bi 2 O 3 mostly adopts high-temperature calcination and other high-temperature treatments. For example, the patent CN102491417A discloses a preparation method of flower-shaped γ-Bi 2 O 3 , but this invention uses a hydrothermal synthesis method, which requires At the same time, it can only be carried out under high temperature and high pressure conditions, which has high requirements on the pressure resistance and heat resistance of the experimental equipment, and the purity of the prepared product is low. The literature Weichang Hao et al. (J. Mater. Sci. Technol., 2014, 30(2), 192-196) produced the precursor by precipitation method, dried at 353°C for 12 h, and then roasted at 773°C 2 h, the reaction process requires a long time of high-temperature drying and roasting, and the preparation route is relatively complicated, which increases the preparation cost of the catalyst and limits its practical application.
发明内容Contents of the invention
本发明就是针对上述问题，提供一种γ-Bi2O3的低温制备方法。本发明操作简单、安全性好，并且制备的产品具有产品纯度高、稳定、光催化活性高的特点。The present invention aims at the above problems and provides a low-temperature preparation method of γ-Bi 2 O 3 . The invention has simple operation and good safety, and the prepared product has the characteristics of high product purity, stability and high photocatalytic activity.
一种γ-Bi2O3光催化剂的低温制备方法，包括如下步骤：A low-temperature preparation method of γ-Bi 2 O 3 photocatalysts, comprising the steps of:
（1）将Bi(NO3)3·5H2O溶于稀硝酸中配制一定浓度的Bi(NO3)3的硝酸溶液；(1) Dissolve Bi(NO 3 ) 3 ·5H 2 O in dilute nitric acid to prepare a certain concentration of Bi(NO 3 ) 3 nitric acid solution;
（2）配制一定浓度的强碱性水溶液，并将其置于特定温度的水浴条件，恒温加热；(2) Prepare a strong alkaline aqueous solution with a certain concentration, place it in a water bath at a specific temperature, and heat it at a constant temperature;
（3）将步骤（1）中Bi(NO3)3的硝酸溶液缓慢滴加入强碱性水溶液中，并在恒温水浴条件下反应一定时间；(3) Slowly drop the nitric acid solution of Bi(NO 3 ) 3 into the strong alkaline aqueous solution in step (1), and react for a certain period of time under the condition of constant temperature water bath;
（4）将步骤（3）得到的产物冷却至室温，经过过滤、洗涤、干燥即可得 (4) Cool the product obtained in step (3) to room temperature, filter, wash and dry to obtain
到γ-Bi2O3。to γ-Bi 2 O 3 .
步骤(1)中所述的Bi(NO3)3的浓度为0.1~9 mol/L。The concentration of Bi(NO 3 ) 3 described in step (1) is 0.1-9 mol/L.
步骤(1)中所述的稀硝酸的浓度为0.02~5 mol/L。The concentration of the dilute nitric acid described in step (1) is 0.02～5 mol/L.
步骤(2)中所述的碱性溶液为NaOH或KOH的水溶液。The alkaline solution described in step (2) is an aqueous solution of NaOH or KOH.
步骤(2)中所述的碱性溶液NaOH或KOH的浓度为0.5~20 mol/L。The concentration of the alkaline solution NaOH or KOH described in step (2) is 0.5-20 mol/L.
步骤(3)中所述的水浴温度范围为50~95℃。The water bath temperature range described in step (3) is 50～95 ℃.
步骤(3)中所述的反应时间为0.5~24 h。The reaction time described in step (3) is 0.5～24 h.
步骤(4)中所述的产物在30~90℃条件下烘干2~24 h。The product described in step (4) is dried at 30-90°C for 2-24 h.
附图说明Description of drawings
图1为实施例1中γ-Bi2O3样品的X射线衍射(XRD)图；Fig. 1 is the X-ray diffraction (XRD) pattern of γ-Bi 2 O 3 samples in embodiment 1;
图2为对比例1中α-Bi2O3样品的X射线衍射(XRD)图；Fig. 2 is the X-ray diffraction (XRD) figure of α-Bi 2 O 3 samples in Comparative Example 1;
图3为光照180 min时，对比例1中α-Bi2O3、实施例1中γ-Bi2O3样品对罗丹明B的光催化降解率图；Figure 3 is a photocatalytic degradation rate diagram of rhodamine B by α-Bi 2 O 3 in Comparative Example 1 and γ-Bi 2 O 3 samples in Example 1 when the light was 180 min;
图4为对比例2中α/γ-Bi2O3、实施例2中γ-Bi2O3样品的X射线衍射(XRD)图；Fig. 4 is the X-ray diffraction (XRD) pattern of α/γ-Bi 2 O 3 in Comparative Example 2 and γ-Bi 2 O 3 samples in Example 2;
图5为实施例2中γ-Bi2O3样品对罗丹明B的光催化降解率图；Fig. 5 is the graph of the photocatalytic degradation rate of rhodamine B to γ-Bi 2 O 3 samples in embodiment 2;
图6为对比例2中α和γ混合晶相氧化铋(α/γ-Bi2O3)的扫描电镜图；6 is a scanning electron microscope image of α and γ mixed crystal phase bismuth oxide (α/γ-Bi 2 O 3 ) in Comparative Example 2;
图7为实施例3中γ-Bi2O3样品的扫描电镜图；Fig. 7 is the scanning electron micrograph of γ-Bi 2 O 3 samples in embodiment 3;
图8为实施例3中γ-Bi2O3样品对罗丹明B的光催化降解率图。Fig. 8 is a diagram of the photocatalytic degradation rate of Rhodamine B by the γ-Bi 2 O 3 sample in Example 3.
具体实施方式detailed description
为了进一步说明本发明，列举以下实施例，但它并不限制各附加权利要求所定义的发明范围。In order to further illustrate the present invention, the following examples are given without limiting the scope of the invention defined by the appended claims.
实施例1Example 1
γ-Bi2O3光催化材料的低温制备及光催化活性Low Temperature Preparation and Photocatalytic Activity of γ-Bi 2 O 3 Photocatalytic Material
1.1 γ-Bi2O3光催化材料的低温制备方法包括如下步骤：1.1 The low-temperature preparation method of γ-Bi 2 O 3 photocatalytic material includes the following steps:
（1）将Bi(NO3)3·5H2O溶于1 mol/L的硝酸中，配制成浓度为0.5 mol/L的Bi(NO3)3的硝酸溶液；(1) Dissolve Bi(NO 3 ) 3 5H 2 O in 1 mol/L nitric acid to prepare a Bi(NO 3 ) 3 nitric acid solution with a concentration of 0.5 mol/L;
（2）配置浓度为2 mol/L的NaOH溶液，将NaOH溶液放入水浴锅中加热到75℃，恒温；(2) Prepare a NaOH solution with a concentration of 2 mol/L, put the NaOH solution in a water bath and heat it to 75°C, and keep the temperature constant;
（3）将步骤(1)中Bi(NO3)3的硝酸溶液缓慢滴加入步骤(2)中的NaOH溶液，温度保持在75℃；(3) Slowly add the nitric acid solution of Bi(NO 3 ) 3 in step (1) dropwise to the NaOH solution in step (2), keeping the temperature at 75°C;
（4）当滴加结束后，继续保持75℃恒温反应3 h；(4) After the dropwise addition, continue to maintain a constant temperature of 75°C for 3 h;
（5）停止反应后将得到的产物冷却至室温，用去离子水和无水乙醇洗涤，在60℃干燥12 h，即可得的γ-Bi2O3。(5) After stopping the reaction, the obtained product was cooled to room temperature, washed with deionized water and absolute ethanol, and dried at 60°C for 12 h to obtain γ-Bi 2 O 3 .
图1为γ-Bi2O3样品的XRD谱图，在2θ=24.7°、27.7°、30.4°、32.9°、41.7°、52.5°、54.2°、55.6°处观察到属于γ-Bi2O3的特征衍射峰，这些衍射峰与JCPDF(#74-1375)中γ-Bi2O3标准衍射峰一致，说明实施例1中得到的产物为γ-Bi2O3。另外，XRD衍射图谱中无杂质峰且衍射峰尖锐，说明所生产的γ-Bi2O3的纯度与结晶度都较高。Figure 1 is the XRD spectrum of the γ-Bi 2 O 3 sample. It is observed at 2θ=24.7°, 27.7°, 30.4°, 32.9°, 41.7°, 52.5°, 54.2°, 55.6° that belong to γ-Bi 2 O 3 , these diffraction peaks are consistent with the standard diffraction peaks of γ-Bi 2 O 3 in JCPDF (#74-1375), indicating that the product obtained in Example 1 is γ-Bi 2 O 3 . In addition, there are no impurity peaks and sharp diffraction peaks in the XRD diffraction pattern, indicating that the produced γ-Bi 2 O 3 has high purity and crystallinity.
1.2 γ-Bi2O3光催化材料的光催化活性1.2 Photocatalytic activity of γ-Bi 2 O 3 photocatalytic materials
利用光催化降解罗丹明B为模型反应，考察了γ-Bi2O3样品的光催化活性。容积为60 mL的反应器上方悬有125 W 高压汞灯光源。在反应器中加入初始浓度为10 mg/L的罗丹明B水溶液60 mL和0.06 g的催化剂(γ-Bi2O3)，搅拌以构成悬浮体系。在汞灯光源的照射下进行光降解反应。在开灯之前，反应溶液在黑暗条件下搅拌30 min以达到吸附平衡。光照之后，每隔一定时间取相同体积的上层清夜，离心后取上层清液在罗丹明B的553 nm吸收波长处测定其吸光度值，根据标准曲线确定亚罗丹明B的浓度。Using the photocatalytic degradation of rhodamine B as a model reaction, the photocatalytic activity of γ-Bi 2 O 3 samples was investigated. A 125 W high-pressure mercury lamp light source is suspended above the reactor with a volume of 60 mL. Add 60 mL of rhodamine B aqueous solution with an initial concentration of 10 mg/L and 0.06 g of catalyst (γ-Bi 2 O 3 ) into the reactor, and stir to form a suspension system. The photodegradation reaction was carried out under the irradiation of a mercury lamp light source. Before turning on the light, the reaction solution was stirred for 30 min in the dark to reach adsorption equilibrium. After illumination, the same volume of supernatant was taken at regular intervals, and after centrifugation, the supernatant was taken to measure the absorbance value at the 553 nm absorption wavelength of rhodamine B, and the concentration of rhodamine B was determined according to the standard curve.
分析方法：在罗丹明B的最大吸收波长处分析滤液中罗丹明B的浓度，因为浓度与吸光度成正比，罗丹明B的光致降解率D可由下式求出：Analysis method: Analyze the concentration of Rhodamine B in the filtrate at the maximum absorption wavelength of Rhodamine B, because the concentration is proportional to the absorbance, the photodegradation rate D of Rhodamine B can be obtained by the following formula:
D＝(Ao-A )/ Ao´ 100%D＝(A o -A )/ A o ´ 100%
其中，Ao为光照理论罗丹明B的吸光度，A为光照时间为t时罗丹明B的吸光度。Among them, A o is the absorbance of rhodamine B according to the light theory, and A is the absorbance of rhodamine B when the light time is t.
图3为实施例1中γ-Bi2O样品对罗丹明B的光催化降解率图，从图中可以看出，在光催化剂加入量为0.06 g、罗丹明B的体积为60 mL(10 mg/L)、光照180 min的条件下，γ-Bi2O3对罗丹明B的降解率可达到72 %，说明γ-Bi2O3具有优异的光催化活性。Fig. 3 is the graph of the photocatalytic degradation rate of Rhodamine B by γ-Bi 2 O samples in Example 1. It can be seen from the figure that when the amount of photocatalyst added is 0.06 g and the volume of Rhodamine B is 60 mL (10 mg/L) and 180 min of light, the degradation rate of γ-Bi 2 O 3 to rhodamine B can reach 72%, indicating that γ-Bi 2 O 3 has excellent photocatalytic activity.
对比例1Comparative example 1
α-Bi2O3光催化材料的低温制备及光催化活性Low Temperature Preparation and Photocatalytic Activity of α-Bi 2 O 3 Photocatalytic Material
按照实施例1相同的操作过程，与实施例1不同之处在于，实施例1步骤(4)中的75℃恒温反应时间为10 min。图2为对比例1中样品的XRD谱图，在2θ=25.8°、26.9°、27.4°、28.0°、33.0°、33.3°、46.4°、52.4°、54.8°处观察到属于α-Bi2O3的特征衍射峰，说明对比例1中所得到的样品为α-Bi2O3。According to the same operation process as in Example 1, the difference from Example 1 is that the reaction time at 75° C. in step (4) of Example 1 is 10 min. Fig. 2 is the XRD pattern of the sample in Comparative Example 1, at 2θ=25.8°, 26.9°, 27.4°, 28.0°, 33.0°, 33.3°, 46.4°, 52.4°, 54.8°, it is observed that it belongs to α-Bi 2 The characteristic diffraction peak of O 3 indicates that the sample obtained in Comparative Example 1 is α-Bi 2 O 3 .
上述结果说明实验过程中加热时间的长短对是否形成γ-Bi2O3有很大的影响。对比例1中α-Bi2O3样品对罗丹明B的降解率为48 %（图3）,低于实施例1中γ-Bi2O3 样品的光催化活性，这也进一步说明了本发明方法所制备的γ-Bi2O3 具有优异的光催化性能。The above results show that the length of heating time during the experiment has a great influence on whether γ-Bi 2 O 3 is formed. The degradation rate of the α-Bi 2 O 3 sample in Comparative Example 1 to Rhodamine B was 48% (Figure 3), which was lower than the photocatalytic activity of the γ-Bi 2 O 3 sample in Example 1, which further illustrated the The γ-Bi 2 O 3 prepared by the inventive method has excellent photocatalytic performance.
实施例2Example 2
γ-Bi2O3光催化材料的低温制备及光催化活性Low Temperature Preparation and Photocatalytic Activity of γ-Bi 2 O 3 Photocatalytic Material
2.1 γ-Bi2O3光催化材料的低温制备2.1 Low temperature preparation of γ-Bi 2 O 3 photocatalytic materials
γ-Bi2O3光催化材料的低温制备方法参照实施例1(1.1),不同之处在于步骤(2)中，将碱性试剂改为KOH溶液。在图4中可以看到实施例2样品的XRD谱图与JCPDF(#74-1375)的γ-Bi2O3标准衍射峰相一致，说明实施例2中所得到的样品为γ-Bi2O3。The low-temperature preparation method of γ-Bi 2 O 3 photocatalytic material refers to Example 1 (1.1), the difference is that in step (2), the alkaline reagent is changed to KOH solution. It can be seen in Figure 4 that the XRD spectrum of the sample in Example 2 is consistent with the γ-Bi 2 O 3 standard diffraction peak of JCPDF (#74-1375), indicating that the sample obtained in Example 2 is γ-Bi 2 O 3 .
2.2 γ-Bi2O3光催化剂的光催化活性2.2 Photocatalytic activity of γ - Bi2O3 photocatalyst
对于实施例2中γ-Bi2O3样品，我们仍然采用光催化降解罗丹明B的实验来考察其光催化活性。光催化降解实验按照实施例1中1.2的方法。图5为实施例2中γ-Bi2O3样品的光催化降解率的谱图，从图中可以看出，在光催化剂加入量为0.06 g、罗丹明B的体积为60 mL(10 mg/L)、光照180 min的条件下，γ-Bi2O3样品对罗丹明B的降解率为74 %，具有较高的光催化活性。For the γ-Bi 2 O 3 sample in Example 2, we still use the experiment of photocatalytic degradation of Rhodamine B to investigate its photocatalytic activity. The photocatalytic degradation experiment followed the method of 1.2 in Example 1. Figure 5 is the spectrogram of the photocatalytic degradation rate of the γ- Bi2O3 sample in Example 2. It can be seen from the figure that when the photocatalyst addition is 0.06 g and the volume of rhodamine B is 60 mL (10 mg /L) and 180 min of light, the degradation rate of γ-Bi 2 O 3 sample to Rhodamine B was 74 %, showing a high photocatalytic activity.
对比例2Comparative example 2
α和γ混合晶相氧化铋(α/γ-Bi2O3)材料的低温制备Low Temperature Preparation of α and γ Mixed Phase Bismuth Oxide (α/γ-Bi 2 O 3 ) Materials
按照实施例2的操作过程，与实施2中的不同之处在于，实施例2中步骤(3)中的温度保持在40℃。在图4对比了实施例2和对比例2所生产样品的XRD谱图。可以看出，对比例2中制备的氧化铋为α和γ混合晶相氧化铋(α/γ-Bi2O3)，同时也表明本发明专利中反应温度的高低对能否形成γ-Bi2O3有很大的影响。According to the operation process of Example 2, the difference from Example 2 is that the temperature in step (3) in Example 2 is maintained at 40°C. The XRD spectra of the samples produced in Example 2 and Comparative Example 2 are compared in FIG. 4 . It can be seen that the bismuth oxide prepared in Comparative Example 2 is α and γ mixed crystal phase bismuth oxide (α/γ-Bi 2 O 3 ), and it also shows that the reaction temperature in the patent of the present invention has a great influence on whether γ-Bi can be formed 2 O 3 has a big effect.
图6为α和γ混合晶相氧化铋(α/γ-Bi2O3)样品的扫描电镜（SEM）图，在图中我们可以清楚的看到呈长条棒状的α-Bi2O3和四面体及呈现四面体堆积结构的γ-Bi2O3。Figure 6 is the scanning electron microscope (SEM) image of the α and γ mixed crystal phase bismuth oxide (α/γ-Bi 2 O 3 ) sample, in which we can clearly see the long rod-shaped α-Bi 2 O 3 And tetrahedron and γ-Bi 2 O 3 with tetrahedral packing structure.
实施例3Example 3
γ-Bi2O3光催化材料的低温制备及光催化活性Low Temperature Preparation and Photocatalytic Activity of γ-Bi 2 O 3 Photocatalytic Material
γ-Bi2O3光催化材料的低温制备方法参照实施例1(1.1),不同之处在于步骤(2)中，将碱性试剂NaOH的浓度改为10 mol/L。在此条件下得到的样品为γ-Bi2O3（XRD谱图未给出）。图7为γ-Bi2O3样品的SEM图，从图中可清楚的看到γ-Bi2O3呈现四面体结构。The low-temperature preparation method of the γ-Bi 2 O 3 photocatalytic material refers to Example 1 (1.1), the difference is that in step (2), the concentration of the alkaline reagent NaOH is changed to 10 mol/L. The sample obtained under this condition is γ-Bi 2 O 3 (XRD spectrum not shown). Figure 7 is the SEM image of the γ-Bi 2 O 3 sample, from which it can be clearly seen that the γ-Bi 2 O 3 presents a tetrahedral structure.
光催化降解实验按照实施例1中1.2的方法。图8为相应样品的光催化降解罗丹明B的活性图，从图中可以看出，在光催化剂加入量为0.06 g、罗丹明B的体积为60 mL(10 mg/L)、光照180 min的条件下，实施例3中γ-Bi2O3光催化剂对罗丹明B的降解率为67 %。The photocatalytic degradation experiment followed the method of 1.2 in Example 1. Figure 8 is the activity diagram of photocatalytic degradation of Rhodamine B for the corresponding samples. It can be seen from the figure that when the photocatalyst addition is 0.06 g, the volume of Rhodamine B is 60 mL (10 mg/L), and the light is 180 min Under the conditions of γ-Bi 2 O 3 photocatalyst in Example 3, the degradation rate of Rhodamine B was 67%.
实施例4Example 4
步骤(1)中所述的Bi(NO3)3的浓度为0.1 mol/L；稀硝酸的浓度为0.02mol/L。The concentration of Bi(NO 3 ) 3 described in step (1) is 0.1 mol/L; the concentration of dilute nitric acid is 0.02 mol/L.
步骤(2)中所述的碱性溶液NaOH的浓度为0.5 mol/L，水浴温度为50℃。步骤(3)中所述的水浴温度为50℃；反应时间为24 h。步骤(4)中所述的产物在30℃条件下烘干24 h。其它步骤同实施例1。The concentration of the alkaline solution NaOH described in step (2) is 0.5 mol/L, and the temperature of the water bath is 50°C. The temperature of the water bath described in step (3) is 50° C.; the reaction time is 24 h. The product described in step (4) was dried at 30°C for 24 h. Other steps are the same as in Example 1.
实施例5Example 5
步骤(1)中所述的Bi(NO3)3的浓度为9 mol/L；所述的稀硝酸的浓度为5 mol/L。步骤(2)中所述的碱性溶液KOH的浓度为20 mol/L，水浴温度为95℃。步骤(3)中所述的水浴温度范围为95℃，反应时间为0.5 h。步骤(4)中所述的产物在90℃条件下烘干2h。其它步骤同实施例1。The concentration of Bi(NO 3 ) 3 in step (1) is 9 mol/L; the concentration of dilute nitric acid is 5 mol/L. The concentration of the alkaline solution KOH described in step (2) is 20 mol/L, and the temperature of the water bath is 95°C. The temperature range of the water bath described in step (3) is 95° C., and the reaction time is 0.5 h. The product described in step (4) was dried at 90° C. for 2 hours. Other steps are the same as in Example 1.
实施例6Example 6
步骤(1)中所述的Bi(NO3)3的浓度为4 mol/L，稀硝酸的浓度为5 mol/L。步骤(2)中所述的碱性溶液NaOH 0.5 mol/L，水浴温度为95℃。步骤(3)中所述的水浴温度为95℃，反应时间为10 h。步骤(4)中所述的产物在30℃条件下烘干13 h。其它步骤同实施例1。The concentration of Bi(NO 3 ) 3 in step (1) is 4 mol/L, and the concentration of dilute nitric acid is 5 mol/L. The alkaline solution NaOH described in step (2) is 0.5 mol/L, and the temperature of the water bath is 95°C. The temperature of the water bath described in step (3) was 95° C., and the reaction time was 10 h. The product described in step (4) was dried at 30°C for 13 h. Other steps are the same as in Example 1.
该专利的研发受到国家自然科学基金项目(20903054)，辽宁省自然科学基金项目（2014020107），辽宁省高等学校优秀人才支持计划（LJQ2014041）和***留学回国人员科研启动基金（教外司留[2013]1792号）的资助。The research and development of this patent is supported by the National Natural Science Foundation of China (20903054), the Liaoning Provincial Natural Science Foundation of China (2014020107), the Outstanding Talents Support Program of Liaoning Higher Education Institutions (LJQ2014041) and the Ministry of Education's Research Startup Fund for Returned Overseas Students 2013] No. 1792).
当然，本发明的上述实施例仅为说明本发明所作的举例，而并非是对本发明的具体实施方式的限定。对于所属领域的普通技术人员来说，在上述举例的基础上还可以做其他不同形式的变化或变动。这里无法对所有的实施方式予以详细举例。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。Of course, the above-mentioned embodiments of the present invention are only examples for illustrating the present invention, rather than limiting the specific implementation of the present invention. For those of ordinary skill in the art, on the basis of the above examples, other changes or changes in different forms can also be made. It is not possible to give detailed examples for all implementation manners here. All obvious changes or changes derived from the technical solutions of the present invention are still within the protection scope of the present invention.
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