CN101624211B - Method for preparing lead hydroxide nano-rod based on liquid-phase chemical reaction - Google Patents
Method for preparing lead hydroxide nano-rod based on liquid-phase chemical reaction Download PDFInfo
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- CN101624211B CN101624211B CN2009101360658A CN200910136065A CN101624211B CN 101624211 B CN101624211 B CN 101624211B CN 2009101360658 A CN2009101360658 A CN 2009101360658A CN 200910136065 A CN200910136065 A CN 200910136065A CN 101624211 B CN101624211 B CN 101624211B
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- 229910021514 lead(II) hydroxide Inorganic materials 0.000 title claims abstract description 32
- 239000002073 nanorod Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 title claims description 10
- 239000007791 liquid phase Substances 0.000 title claims description 9
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 3
- 150000001805 chlorine compounds Chemical class 0.000 claims description 2
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims 1
- 229930013930 alkaloid Natural products 0.000 claims 1
- 150000003797 alkaloid derivatives Chemical class 0.000 claims 1
- 238000000151 deposition Methods 0.000 claims 1
- 230000008021 deposition Effects 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 11
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 22
- 239000011780 sodium chloride Substances 0.000 description 11
- 239000007787 solid Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
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Abstract
一种制备氢氧化铅纳米棒的方法，属于纳米材料制备技术领域，其特征是将硝酸铅及可溶性氯化物按物质的量比例为1∶1-1∶10溶解到去离子水中，配成溶液并加热到50-90摄氏度，再向溶液中按硝酸铅与碱物质的量比例为1∶3加入碱，搅拌得到白色沉淀，过滤洗涤，干燥，即得氢氧化铅纳米棒。所得氢氧化铅纳米棒为六方结构，长度约为50微米，直径为20-500纳米。该方法操作简便，产率高，对环境没有污染。
A method for preparing lead hydroxide nanorods, which belongs to the technical field of nanomaterial preparation, is characterized in that lead nitrate and soluble chloride are dissolved in deionized water at a ratio of 1:1-1:10 according to the amount of substances to form a solution And heating to 50-90 degrees Celsius, then adding alkali to the solution according to the ratio of lead nitrate and alkali substance as 1:3, stirring to obtain white precipitate, filtering, washing, and drying to obtain lead hydroxide nanorods. The obtained lead hydroxide nanorod has a hexagonal structure, the length is about 50 micrometers, and the diameter is 20-500 nanometers. The method has the advantages of simple operation, high yield and no pollution to the environment.
Description
技术领域technical field
本发明涉及一种制备纳米棒的方法，特别涉及一种利用液相化学反应制备氢氧化铅纳米棒的方法。The invention relates to a method for preparing nanorods, in particular to a method for preparing lead hydroxide nanorods by using liquid-phase chemical reaction.
背景技术Background technique
准一维纳米材料，如纳米纤维、纳米棒等，在两维方向上为纳米尺度，其长径大。与三维都为宏观尺度的块体材料相比，具有独特的理化性质，如具有小尺寸效应，量子效应，表面效应等，会显示出独特的光学特性，电学特性，催化特性等。Quasi-one-dimensional nanomaterials, such as nanofibers, nanorods, etc., are nanoscale in the two-dimensional direction, and their major diameters are large. Compared with bulk materials that are all three-dimensional on a macro scale, they have unique physical and chemical properties, such as small size effects, quantum effects, surface effects, etc., and will display unique optical, electrical, and catalytic properties.
目前制备准一维纳米材料的方法比较多，如化学气相沉积法，物理蒸发法，模板法，电化学沉积法，固相法，水热法等。At present, there are many methods for preparing quasi-one-dimensional nanomaterials, such as chemical vapor deposition, physical evaporation, template method, electrochemical deposition method, solid phase method, hydrothermal method, etc.
氢氧化铅有着广泛的应用，如为细胞染色，作及吸收剂等。然而关于氢氧化铅纳米棒的制备方法仍未见文献报道。Lead hydroxide has a wide range of applications, such as staining cells, as absorbents, etc. However, there is still no literature report on the preparation method of lead hydroxide nanorods.
发明内容Contents of the invention
本发明的目在于提供一种液相化学反应制备氢氧化铅纳米棒的方法，其包括下列步骤：(1)将硝酸铅溶解到去离子水中，配成溶液；(2)在步骤(1)中的溶液中按硝酸铅与可溶性氯化物物质的量比例为1∶1-1∶10加入可溶性氯化物；(3)将步骤(2)中的溶液加热到50-80摄氏度；(4)在步骤(3)中的溶液中按硝酸铅与碱物质的量比例为1∶3加入碱，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒；进一步，所述的可溶性氯化物包括氯化钠或氯化钾；进一步，所述的碱包括氢氧化钠或氢氧化钾。此外，本发明还提供了由上述方法制备的氢氧化铅纳米棒，氢氧化铅纳米棒的长度为10-100微米，直径为20-500纳米，纯度高达99％，晶体结构为六方结构。该方法操作简便，产率高，反应时间短，而且对环境没有污染。本发明人在研究硝酸铅与碱液相化学反应时发现，当向先体溶液中添加氯化钠时，由于氯离子的抑制水解的作用，所得沉淀物为氢氧化铅纳米棒。本发明制备氢氧化铅纳米棒的方法是将硝酸铅与氯化钠按一定比例溶解到去离子水形成溶液，并加热到一定温度，再向溶液中加入一定量的氢氧化钾，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。The object of the present invention is to provide a kind of method that liquid-phase chemical reaction prepares lead hydroxide nanorod, and it comprises the following steps: (1) lead nitrate is dissolved in deionized water, is made into solution; (2) in step (1) In the solution in the solution by lead nitrate and soluble chloride material ratio is 1: 1-1: 10 to add soluble chloride; (3) the solution in step (2) is heated to 50-80 degree centigrade; (4) in Add alkali to the solution in step (3) according to the amount ratio of lead nitrate and alkali substance as 1:3, stir to obtain white precipitate, filter, wash and dry to obtain lead hydroxide nanorods; further, the Soluble chlorides include sodium chloride or potassium chloride; further, the alkali includes sodium hydroxide or potassium hydroxide. In addition, the present invention also provides lead hydroxide nanorods prepared by the above method, the length of the lead hydroxide nanorods is 10-100 microns, the diameter is 20-500 nanometers, the purity is as high as 99%, and the crystal structure is hexagonal. The method has the advantages of simple operation, high yield, short reaction time and no pollution to the environment. When the present inventor studied the chemical reaction between lead nitrate and alkali solution, he found that when sodium chloride was added to the precursor solution, the resulting precipitate was lead hydroxide nanorods due to the inhibition of hydrolysis by chloride ions. The method for preparing lead hydroxide nanorods in the present invention is to dissolve lead nitrate and sodium chloride in deionized water in a certain proportion to form a solution, and heat it to a certain temperature, then add a certain amount of potassium hydroxide to the solution, and stir to obtain The white precipitate was filtered, washed and dried to obtain lead hydroxide nanorods.
附图说明Description of drawings
图1是本发明所述的液相化学反应方法制备的氢氧化铅纳米棒的XRD谱线。Fig. 1 is the XRD spectrum line of the lead hydroxide nanorod prepared by the liquid phase chemical reaction method of the present invention.
图2是本发明所述的液相化学反应方法制备的氢氧化铅纳米棒的扫描电镜照片。Fig. 2 is a scanning electron micrograph of lead hydroxide nanorods prepared by the liquid-phase chemical reaction method of the present invention.
图3是本发明所述的液相化学反应方法制备的氢氧化铅纳米棒的透射电镜照片。Fig. 3 is a transmission electron micrograph of lead hydroxide nanorods prepared by the liquid-phase chemical reaction method of the present invention.
图4是本发明所述的液相化学反应方法制备的氢氧化铅纳米棒的高分辨透射电镜照片。Fig. 4 is a high-resolution transmission electron micrograph of lead hydroxide nanorods prepared by the liquid-phase chemical reaction method of the present invention.
图5是本发明所述的液相化学反应方法制备的氢氧化铅纳米棒的选区电子衍射谱。Fig. 5 is the selected area electron diffraction spectrum of the lead hydroxide nanorod prepared by the liquid phase chemical reaction method of the present invention.
具体实施方式Detailed ways
将硝酸铅和氯化钠溶解到去离水中，配成溶液，硝酸铅的浓度为0.01mol/l，氯化钠的浓度为0.01-0.10mol/l，加热溶液到50-80摄氏度，再加入氢氧化钾固体，氢氧化钾的浓度为0.03mol/l，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。Dissolve lead nitrate and sodium chloride in deionized water to make a solution, the concentration of lead nitrate is 0.01mol/l, the concentration of sodium chloride is 0.01-0.10mol/l, heat the solution to 50-80 degrees Celsius, and then add Potassium hydroxide solid, the concentration of potassium hydroxide is 0.03mol/l, stirring to obtain a white precipitate, which is filtered, washed and dried to obtain lead hydroxide nanorods.
实施例1Example 1
取0.166g硝酸铅和0.06g氯化钠溶于50ml去离子水中，将溶液加热到80摄氏度，然后，取0.084g氢氧化钾固体加到溶液中，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。如图1所示，产物经X射线粉末衍射鉴定为氢氧化铅；用扫描电子显微镜对产物进行形貌分析，从图2中可以看出其形貌为棒，棒的长度约为50微米，棒的直径在100-500纳米之间，长径比高达100以上；图3显示在透射电子显微镜下看到的形貌也为棒状；图4显示在高分辨透射电子显微镜下看清晰的(002)晶面的晶格条纹，(002)晶面的面间距约为6.43
实施例2Example 2
取0.662g硝酸铅和0.117g氯化钠溶于200ml去离子水中，将溶液加热到90摄氏度，然后，取0.336g氢氧化钾固体加到溶液中，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。Take 0.662g lead nitrate and 0.117g sodium chloride and dissolve in 200ml deionized water, heat the solution to 90 degrees Celsius, then add 0.336g potassium hydroxide solid to the solution, stir to obtain a white precipitate, filter, wash, After drying, lead hydroxide nanorods are obtained.
实施例3Example 3
取0.662g硝酸铅和0.234g氯化钠溶于200ml去离子水中，将溶液加热到90摄氏度，然后，取0.084g氢氧化钾固体加到溶液中，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。Take 0.662g lead nitrate and 0.234g sodium chloride and dissolve in 200ml deionized water, heat the solution to 90 degrees Celsius, then add 0.084g potassium hydroxide solid to the solution, stir to obtain a white precipitate, filter, wash, After drying, lead hydroxide nanorods are obtained.
实施例4Example 4
取0.662g硝酸铅和0.351g氯化钠溶于200ml去离子水中，将溶液加热到90摄氏度，然后，取0.084g氢氧化钾固体加到溶液中，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。Take 0.662g lead nitrate and 0.351g sodium chloride and dissolve in 200ml deionized water, heat the solution to 90 degrees Celsius, then add 0.084g potassium hydroxide solid to the solution, stir to obtain a white precipitate, filter, wash, After drying, lead hydroxide nanorods are obtained.
实施例5Example 5
取0.662g硝酸铅和0.468g氯化钠溶于200ml去离子水中，将溶液加热到90摄氏度，然后，取0.084g氢氧化钾固体加到溶液中，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。Take 0.662g lead nitrate and 0.468g sodium chloride and dissolve in 200ml deionized water, heat the solution to 90 degrees Celsius, then add 0.084g potassium hydroxide solid to the solution, stir to obtain a white precipitate, filter, wash, After drying, lead hydroxide nanorods are obtained.
实施例3Example 3
取0.662g硝酸铅和0.585g氯化钠溶于200ml去离子水中，将溶液加热到90摄氏度，然后，取0.084g氢氧化钾固体加到溶液中，搅拌，得到白色沉淀物，过滤、洗涤、干燥，即得氢氧化铅纳米棒。Take 0.662g lead nitrate and 0.585g sodium chloride and dissolve in 200ml deionized water, heat the solution to 90 degrees Celsius, then add 0.084g potassium hydroxide solid to the solution, stir to obtain a white precipitate, filter, wash, After drying, lead hydroxide nanorods are obtained.
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| CN1491896A (en) * | 2002-10-23 | 2004-04-28 | 新疆大学 | A method for preparing lead oxide nanorods by solid-phase chemical reaction |
| CN101348277A (en) * | 2007-07-18 | 2009-01-21 | 北京化工大学 | A kind of synthetic method of nano lead hydroxide |
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| CN1491896A (en) * | 2002-10-23 | 2004-04-28 | 新疆大学 | A method for preparing lead oxide nanorods by solid-phase chemical reaction |
| CN101348277A (en) * | 2007-07-18 | 2009-01-21 | 北京化工大学 | A kind of synthetic method of nano lead hydroxide |
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| Title |
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| 杜江燕等.铅(II)化合物与NaOH室温条件下的固相化学反应研究.《无机化学学报》.1999,第15卷(第3期),383-387. * |
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