CN106006754A - Method for synthesizing highly pure tooeleite through hydrothermal technology - Google Patents
Method for synthesizing highly pure tooeleite through hydrothermal technology Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 17
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 17
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- OGLYSQODVISTQQ-UHFFFAOYSA-N tetrahydroxy-$l^{5}-arsane Chemical compound O[AsH](O)(O)O OGLYSQODVISTQQ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 10
- 239000011707 mineral Substances 0.000 abstract description 10
- 229910052742 iron Inorganic materials 0.000 abstract description 8
- AQLMHYSWFMLWBS-UHFFFAOYSA-N arsenite(1-) Chemical compound O[As](O)[O-] AQLMHYSWFMLWBS-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 229910052935 jarosite Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- GCPXMJHSNVMWNM-UHFFFAOYSA-N arsenous acid Chemical compound O[As](O)O GCPXMJHSNVMWNM-UHFFFAOYSA-N 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000011550 stock solution Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- 241001522296 Erithacus rubecula Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- VETKVGYBAMGARK-UHFFFAOYSA-N arsanylidyneiron Chemical compound [As]#[Fe] VETKVGYBAMGARK-UHFFFAOYSA-N 0.000 description 1
- MJLGNAGLHAQFHV-UHFFFAOYSA-N arsenopyrite Chemical compound [S-2].[Fe+3].[As-] MJLGNAGLHAQFHV-UHFFFAOYSA-N 0.000 description 1
- 229910052964 arsenopyrite Inorganic materials 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical group [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001608 iron mineral Inorganic materials 0.000 description 1
- UYZMAFWCKGTUMA-UHFFFAOYSA-K iron(3+);trioxido(oxo)-$l^{5}-arsane;dihydrate Chemical compound O.O.[Fe+3].[O-][As]([O-])([O-])=O UYZMAFWCKGTUMA-UHFFFAOYSA-K 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing iron, with or without oxygen or hydrogen, and containing two or more other elements
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
本发明公开了一种水热法合成高纯图水羟砷铁矾的方法。此方法利用三价铁和三价砷为原料，在混合溶液中初始As(III)浓度为1.5‑7.5g/L，控制铁、砷摩尔比为0.8‑1.5、pH值为1.4‑1.8、温度为100‑130℃、水热反应时间为3‑10h，得到的矿物为高纯图水羟砷铁矾。所得矿物纯度高于95％，可为研究其相关性质提供原料。The invention discloses a method for synthesizing high-purity hydroxyarsenite by hydrothermal method. This method utilizes ferric iron and trivalent arsenic as raw materials, and the initial As(III) concentration in the mixed solution is 1.5-7.5g/L, and the molar ratio of iron and arsenic is controlled to be 0.8-1.5, pH value is 1.4-1.8, temperature The temperature is 100-130°C, and the hydrothermal reaction time is 3-10h, and the obtained mineral is high-purity arsenite. The purity of the obtained mineral is higher than 95%, which can provide raw materials for researching its related properties.
Description
技术领域technical field
本发明属于环境工程领域，具体涉及一种水热法合成高纯图水羟砷铁矾的方法。The invention belongs to the field of environmental engineering, and in particular relates to a method for synthesizing high-purity hydroxyarsenite by a hydrothermal method.
背景技术Background technique
图水羟砷铁矾是目前发现的自然界中唯一一种以亚砷酸、硫酸盐存在的含铁矿物，其化学成分为Fe6(AsO3)4SO4(OH)4·4H2O，其中三价砷含量高达28％，铁砷比仅为1.5。因其存在环境、高砷含量及低铁砷比，有学者提出将其作为一种高效除砷的潜在矿物应用于废水中三价砷的直接去除。然而，因图水羟砷铁矾在自然界中主要以颗粒状分散在黄铁矿、砷黄铁矿、臭葱石和黄钾铁矾等矿物中，难以大量提取，目前对该天然矿物的报道仅是其基础的物理化学参数，如颜色为镉黄色，硬度为3，密度为4.23，属于三斜晶系，分子式为Fe6(AsO3)4SO4(OH)4·4H2O。因此为了实现该矿物在实际中的应用，必需要在实验室的条件下合成并研究了解其相关性质。Tushuijadite is the only iron-containing mineral found in nature in the form of arsenous acid and sulfate. Its chemical composition is Fe 6 (AsO 3 ) 4 SO 4 (OH) 4 ·4H 2 O, in which the content of trivalent arsenic is as high as 28%, and the ratio of iron to arsenic is only 1.5. Due to its existence in the environment, high arsenic content, and low ratio of iron to arsenic, some scholars have proposed to use it as a potential mineral for efficient arsenic removal in the direct removal of trivalent arsenic in wastewater. However, because hydroxyarsonite is mainly dispersed in minerals such as pyrite, arsenopyrite, scorodite and jarosite in the form of particles in nature, it is difficult to extract in large quantities. Currently, there are only reports on this natural mineral. It is its basic physical and chemical parameters, such as the color is cadmium yellow, the hardness is 3, the density is 4.23, it belongs to the triclinic system, and the molecular formula is Fe 6 (AsO 3 ) 4 SO 4 (OH) 4 ·4H 2 O. Therefore, in order to realize the practical application of this mineral, it is necessary to synthesize and study its related properties under laboratory conditions.
目前，国内外有学者尝试在实验室的条件下合成图水羟砷铁矾。Nishimura和Robin(Minerals Engineering.(2008)21:246-251)分别在25℃、60℃、90℃不同的pH下合成tooeleite，推测了其在室温下的稳定存在pH值为2-3.5。刘璟等人(ActaPetrologica et Mineralogica.(2012)31:901-906和SpectrochimicaActa Part A:Molecular and Biomolecular Spectroscopy.(2015)134:428-433)通过95℃恒温水浴合成tooeleite，指出pH在2-9范围内均可成矿，并研究了合成物的溶度积常数、标准反应吉布斯自由能、浸出毒性等相关参数。但我们研究发现此类条件下合成的图水羟砷铁矾纯度较低，其中夹杂着大量的无定形铁的矿物，并使得一部分的砷以吸附态的形式存在，加重了其不稳定性，因此其研究所得的相关参数缺乏严谨性且会产生很大偏差。则合成高纯图水羟砷铁矾对了解其相关性质并实现其实际应用十分必要。At present, some scholars at home and abroad are trying to synthesize Tushui hydroxyarsenite under laboratory conditions. Nishimura and Robin (Minerals Engineering. (2008) 21:246-251) synthesized tooeleite at different pHs of 25°C, 60°C, and 90°C respectively, and speculated that its stable existence at room temperature had a pH value of 2-3.5. Liu Jing et al. (ActaPetrologica et Mineralogica.(2012) 31:901-906 and SpectrochimicaActa Part A: Molecular and Biomolecular Spectroscopy.(2015) 134:428-433) synthesized tooeleite through a 95°C constant temperature water bath, pointing out that the pH is between 2-9 Mineralization can be carried out within the range, and related parameters such as solubility product constant, standard reaction Gibbs free energy, and leaching toxicity of the compound have been studied. However, our research found that the purity of the arsenite synthesized under such conditions is low, and a large amount of amorphous iron minerals are mixed in it, and part of the arsenic exists in the form of adsorption, which aggravates its instability. Therefore, the relevant parameters obtained in its research lack rigor and will produce large deviations. Therefore, it is necessary to synthesize high-purity ferroxasite to understand its related properties and realize its practical application.
本发明用水热法合成高纯图水羟砷铁矾，所得矿物纯度高于95％，可为研究其相关性质提供原料，并为其能否作为一种稳定化固砷矿物提供参考。The invention synthesizes high-purity arsenite with a hydrothermal method, and the obtained mineral has a purity higher than 95%, which can provide raw materials for studying its related properties and provide reference for whether it can be used as a stabilized arsenic-fixing mineral.
发明内容Contents of the invention
本发明提供了一种利用水热法合成高纯图水羟砷铁矾的方法，该方法操作简单，所得样品晶型好、纯度高，为研究其相关性质提供了原料。The invention provides a method for synthesizing high-purity arsonite by using a hydrothermal method. The method is simple to operate, and the obtained sample has good crystal form and high purity, and provides raw materials for studying its related properties.
本发明的目的是通过以下方式实现的：The purpose of the present invention is achieved in the following manner:
一种水热法合成高纯图水羟砷铁矾的方法，包括以下步骤：A method for hydrothermally synthesizing high-purity japonite, comprising the following steps:
(1)Fe(III)、As(III)摩尔比为0.8-1.5的三价砷和三价铁溶液混合，调整溶液pH值1.4-1.8；(1) Fe(III), As(III) molar ratio is 0.8-1.5 trivalent arsenic and ferric iron solution are mixed, adjust solution pH value 1.4-1.8;
(2)将混合液倒入反应釜，100-130℃水热反应一段时间；(2) Pour the mixed solution into a reaction kettle, and conduct a hydrothermal reaction at 100-130°C for a period of time;
(3)反应结束后，溶液冷却静置，而后抽滤，真空烘干，所得产物即为图水羟砷铁矾晶体化合物Fe6(AsO3)4SO4(OH)4·4H2O。(3) After the reaction, the solution was cooled and allowed to stand, then suction filtered and vacuum dried, and the obtained product was the crystalline compound Fe 6 (AsO 3 ) 4 SO 4 (OH) 4 ·4H 2 O.
步骤(1)的三价砷溶液浓度为1.5-7.5g/L。The concentration of the trivalent arsenic solution in step (1) is 1.5-7.5g/L.
步骤(1)的三价铁为硫酸铁。The ferric iron of step (1) is ferric sulfate.
步骤(1)所述Fe(III)、As(III)摩尔比优选为1.5。The molar ratio of Fe(III) and As(III) in step (1) is preferably 1.5.
步骤(1)所述混合溶液的pH值优选调整为1.6。The pH value of the mixed solution in step (1) is preferably adjusted to 1.6.
步骤(2)所述水热反应温度优选控制在120℃。The hydrothermal reaction temperature in step (2) is preferably controlled at 120°C.
步骤(2)所述水热反应时间控制为3-10h。The hydrothermal reaction time of step (2) is controlled to be 3-10h.
附图说明Description of drawings
图1为不同温度下所得样品XRD图(pH 1.8，Fe/As＝1.5)；Fig. 1 is the sample XRD pattern obtained under different temperatures (pH 1.8, Fe/As=1.5);
图2为不同pH下所得样品XRD图(Fe/As＝1.5，120℃)；Figure 2 is the XRD pattern of samples obtained at different pHs (Fe/As=1.5, 120°C);
图3为不同铁砷比下所得样品XRD图(pH 1.6,120℃)；Figure 3 is the XRD patterns of samples obtained under different iron-arsenic ratios (pH 1.6, 120°C);
图4为pH 1.6、Fe/As＝1.5、120℃下样品SEM图。Figure 4 is the SEM image of the sample at pH 1.6, Fe/As=1.5, and 120°C.
具体实施方式detailed description
以下实施例旨在进一步说明本发明，而不是对本发明的限定。The following examples are intended to further illustrate the present invention, but not limit the present invention.
实施例1Example 1
配制0.2M As(III)和0.3M Fe(III)溶液作为储备原液，分别取20ml充分混合后，调节溶液pH为1.8。将此溶液倒入容量为100ml的反应釜中，放入烘箱，分别设定温度为105-150℃，温度升至设定温度开始计时，在此温度下反应6h，而后让其自然冷却。0.45μm的滤膜抽滤后，于60℃下真空烘干。Prepare 0.2M As(III) and 0.3M Fe(III) solutions as stock solutions, take 20ml respectively and mix thoroughly, then adjust the pH of the solutions to 1.8. Pour this solution into a reaction kettle with a capacity of 100ml, put it into an oven, set the temperature at 105-150°C respectively, start timing when the temperature rises to the set temperature, react at this temperature for 6h, and then let it cool naturally. After suction filtration through a 0.45 μm filter membrane, vacuum-dry at 60°C.
图1为不同温度下所得样品的XRD图。由图1可以看出，135℃以下所有峰均为图水羟砷铁矾的特征峰，且温度越高，峰宽度越窄、强度越高，显示所得样品重图水羟砷铁矾晶型更好、纯度更高。而高于135℃，黄钠铁矾特征峰开始出现，且温度越高其特征峰越明显。因此认为合成高纯图水羟砷铁矾的温度应为135℃以下。Figure 1 is the XRD patterns of samples obtained at different temperatures. It can be seen from Figure 1 that all the peaks below 135°C are the characteristic peaks of japonite, and the higher the temperature, the narrower the peak width and the higher the intensity, indicating that the obtained sample re-crystal form of jajasite Better and more pure. But above 135°C, the characteristic peaks of jarosite began to appear, and the higher the temperature, the more obvious the characteristic peaks. Therefore, it is considered that the temperature for synthesizing high-purity arsenite should be below 135°C.
实施例2Example 2
配制0.2M As(III)和0.3M Fe(III)溶液作为储备原液，分别取20ml充分混合后，调节溶液pH为1.2-1.8。将此溶液倒入容量为100ml的反应釜中，放入烘箱，分别设定温度为120℃，温度升至设定温度开始计时，在此温度下反应6h，而后让其自然冷却。0.45μm的滤膜抽滤后，于60℃下真空烘干。Prepare 0.2M As(III) and 0.3M Fe(III) solutions as stock solutions, take 20ml respectively and mix thoroughly, then adjust the pH of the solutions to 1.2-1.8. Pour this solution into a reaction kettle with a capacity of 100ml, put it into an oven, set the temperature at 120°C respectively, start timing when the temperature rises to the set temperature, react at this temperature for 6h, and then let it cool naturally. After suction filtration through a 0.45 μm filter membrane, vacuum-dry at 60°C.
图2为不同pH下所得样品的XRD图。由图2可以看出，除pH1.2条件下生成样为黄钠铁矾，其余实验pH条件下所得产物均为图水羟砷铁矾，且pH1.6条件下所得样品晶型最好。Figure 2 is the XRD patterns of samples obtained at different pHs. It can be seen from Figure 2 that, except for the jarosite produced under the condition of pH 1.2, the products obtained under the other experimental pH conditions are all hydroxyarsonite, and the crystal form of the sample obtained under the condition of pH 1.6 is the best.
实施例3Example 3
配制0.2M As(III)和0.2M、0.3M、0.4MFe(III)溶液作为储备原液，分别取20mlAs(III)与不同浓度等体积Fe(III)充分混合后，调节溶液pH为1.6。将此溶液倒入容量为100ml的反应釜中，放入烘箱，分别设定温度为120℃，温度升至设定温度开始计时，在此温度下反应6h，而后让其自然冷却。0.45μm的滤膜抽滤后，于60℃下真空烘干。Prepare 0.2M As(III) and 0.2M, 0.3M, 0.4M Fe(III) solutions as stock solutions, take 20ml of As(III) and different concentrations of Fe(III) and mix them thoroughly, and then adjust the pH of the solution to 1.6. Pour this solution into a reaction kettle with a capacity of 100ml, put it into an oven, set the temperature at 120°C respectively, start timing when the temperature rises to the set temperature, react at this temperature for 6h, and then let it cool naturally. After suction filtration through a 0.45 μm filter membrane, vacuum-dry at 60°C.
图3为不同铁砷比下所得样品的XRD图。由图3可以看出，铁砷比大于2即有黄钠铁矾特征峰出现，而铁砷比小于2时，铁砷比越大，所得样品晶型越好。Figure 3 is the XRD patterns of the samples obtained under different ratios of iron to arsenic. It can be seen from Figure 3 that if the ratio of iron to arsenic is greater than 2, there will be characteristic peaks of jarosite, and when the ratio of iron to arsenic is less than 2, the larger the ratio of iron to arsenic, the better the crystal form of the obtained sample.
实施例4Example 4
图4为优选条件pH 1.6、Fe/As＝1.5、120℃下所得样品SEM图。由SEM图可知，其形貌为片状堆积的花瓣状结构，无其他形貌的出现，证明其为高纯图水羟砷铁矾。Figure 4 is the SEM image of the sample obtained under the optimal conditions of pH 1.6, Fe/As=1.5, and 120°C. It can be seen from the SEM image that its appearance is a petal-like structure of sheet-like accumulation, and no other appearances appear, which proves that it is a high-purity hydroxyarsenite.
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Cited By (7)
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| CN107010704A (en) * | 2017-05-02 | 2017-08-04 | 中南大学 | A kind of method for handling the waste water containing trivalent arsenic |
| CN107500362A (en) * | 2017-09-15 | 2017-12-22 | 中南大学 | A kind of new figure water hydroxyl sarmientite and its preparation method and application |
| CN107794372A (en) * | 2017-10-25 | 2018-03-13 | 湖南水口山有色金属集团有限公司 | A kind of dearsenification selective from lead anode slurry and the method for zero emission of wastewater treatment |
| CN108101115A (en) * | 2018-01-04 | 2018-06-01 | 中南大学 | A kind of hydro-thermal method prepares the method without sulphur figure water hydroxyl sarmientite |
| CN108483690A (en) * | 2018-02-12 | 2018-09-04 | 中南大学 | A method of processing High-arsenic wastewater |
| CN110436527A (en) * | 2019-08-18 | 2019-11-12 | 桂林理工大学 | A kind of method of hydrothermal synthesis alkalinity arsenic acid-ferric sulfate solid solution |
| CN113135632A (en) * | 2020-01-19 | 2021-07-20 | 大唐环境产业集团股份有限公司 | Method for removing arsenic from arsenic-containing wastewater |
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