CN101850993A - A kind of preparation method of rod-shaped nano magnesium oxide - Google Patents
A kind of preparation method of rod-shaped nano magnesium oxide Download PDFInfo
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- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 43
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 43
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 229920002472 Starch Polymers 0.000 claims abstract description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008107 starch Substances 0.000 claims abstract description 6
- 235000019698 starch Nutrition 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 10
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 10
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims 3
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- -1 polyoxyethylene nonylphenol Polymers 0.000 claims 1
- 229960004418 trolamine Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 14
- 239000002244 precipitate Substances 0.000 abstract description 11
- 238000001354 calcination Methods 0.000 abstract description 7
- 239000002243 precursor Substances 0.000 abstract description 6
- 239000003995 emulsifying agent Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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Abstract
一种棒状纳米氧化镁的制备方法，属于材料技术领域，按以下步骤进行：(1)将可溶性镁盐、沉淀剂氢氧化钠和晶型控制剂作为反应原料溶于水中，制成反应溶液，所述的晶型控制剂为乙二醇、淀粉、乳化剂OP10或三乙醇胺；(2)将制成的反应溶液在20～90℃和搅拌条件下反应20～40min，获得的沉淀为前驱体；(3)将获得的前驱体在550～750℃条件下煅烧2～4h。本发明的方法通过选取晶型控制剂，同时通过控制沉淀条件获得松散的前驱体，控制煅烧条件制成棒状纳米氧化镁；获得的棒状纳米氧化镁粒径和长径比可控。本方法具有原料易得，工艺简单，适用于工业化生产等优点，在红外隐身材料技术领域具有良好的应用前景。
A preparation method of rod-shaped nano magnesium oxide belongs to the field of material technology, and is carried out according to the following steps: (1) dissolving soluble magnesium salt, precipitating agent sodium hydroxide and crystal form control agent in water as reaction raw materials to prepare a reaction solution, The crystal form control agent is ethylene glycol, starch, emulsifier OP10 or triethanolamine; (2) react the prepared reaction solution at 20-90°C under stirring conditions for 20-40min, and the obtained precipitate is a precursor ; (3) calcining the obtained precursor at 550-750° C. for 2-4 hours. In the method of the invention, a crystal form control agent is selected, a loose precursor is obtained by controlling precipitation conditions, and rod-shaped nano-magnesia is produced by controlling calcination conditions; the particle size and aspect ratio of the obtained rod-shaped nano-magnesia are controllable. The method has the advantages of easy-to-obtain raw materials, simple process, suitability for industrialized production, etc., and has good application prospects in the technical field of infrared stealth materials.
Description
技术领域technical field
本发明属于材料技术领域，特别涉及一种棒状纳米氧化镁的制备方法。The invention belongs to the technical field of materials, in particular to a method for preparing rod-shaped nano magnesium oxide.
背景技术Background technique
纳米氧化镁是一种新型高功能精细无机材料，除了具有普通氧化镁的性质和用途外，由于粒子进入纳米尺度，使纳米氧化镁因纳米粒子所共有的表面效应、量子尺寸效应、体积效应、宏观量子隧道效应外，而且还具有一系列普通氧化镁所不具备的性质，从而开辟了一系列新的应用领域。纳米氧化镁具有不同于本体材料的热、光、电、力学、化学等特殊性能，在工业上有重要的应用前景和巨大的经济潜力。红外吸收是隐身技术的一种，红外隐身材料是当前隐身技术研究的一个热点，具有广阔的研究前景。Nano-magnesia is a new type of high-function fine inorganic material. In addition to the properties and uses of ordinary magnesium oxide, because the particles enter the nanometer scale, nano-magnesia has surface effects, quantum size effects, and volume effects shared by nanoparticles. In addition to the macroscopic quantum tunneling effect, it also has a series of properties that ordinary magnesium oxide does not have, thus opening up a series of new application fields. Nano-magnesium oxide has special properties such as heat, light, electricity, mechanics, and chemistry that are different from bulk materials, and has important application prospects and huge economic potential in industry. Infrared absorption is a kind of stealth technology. Infrared stealth materials are a hotspot in the current research of stealth technology and have broad research prospects.
目前纳米氧化镁的制备有多种方法，近年的研究结果表明，采用可溶性镁盐与沉淀剂混合，再通过表面活性剂控制晶粒形状，在搅拌、超声波或加热条件下制成沉淀，然后经过煅烧获得纳米氧化镁。现有的方法中纳米的形貌控制主要由反应时间、反应温度、搅拌条件及煅烧温度和时间决定，选用的表面活性剂如硬脂酸盐的等成本较高，更重要的是在控制纳米氧化镁的形状方面没有取得突破的效果；不同形状的纳米氧化镁具有不同的红外吸收特征，适用于各种不同的红外吸收范围，如何选择更适宜的表面活性剂等辅助材料，以及根据不同的材料确定其他工艺条件，制备出形状可控的、适合特殊要求的纳米氧化镁材料是目前急需解决的问题。At present, there are many methods for the preparation of nano-magnesium oxide. The research results in recent years have shown that soluble magnesium salts are mixed with precipitants, and then the grain shape is controlled by surfactants, and precipitates are made under stirring, ultrasonic or heating conditions, and then processed Calcination to obtain nano-magnesium oxide. In the existing methods, the morphology control of nanometers is mainly determined by reaction time, reaction temperature, stirring conditions, and calcination temperature and time. There is no breakthrough in the shape of magnesium oxide; different shapes of nano magnesium oxide have different infrared absorption characteristics, which are suitable for various infrared absorption ranges, how to choose more suitable auxiliary materials such as surfactants, and according to different It is an urgent problem to be solved at present to determine other process conditions for materials and to prepare nano-magnesia materials with controllable shape and suitable for special requirements.
发明内容Contents of the invention
针对现有纳米氧化镁制备技术上存在的不足，本发明提供一种棒状纳米氧化镁的制备方法，目的在于通过选择适宜的晶型控制剂，确定优化的工艺路线，采用低成本且工艺简单的方法制备棒状纳米氧化镁。Aiming at the deficiencies in the existing nano-magnesia preparation technology, the present invention provides a method for preparing rod-shaped nano-magnesia. Methods to prepare rod-shaped nano magnesium oxide.
本发明的方法按以下步骤进行：Method of the present invention carries out according to the following steps:
1、将可溶性镁盐、沉淀剂氢氧化钠和晶型控制剂作为反应原料溶于水中，制成反应溶液，反应原料的成分按重量百分比为氢氧化钠27～44％，可溶性镁盐55～72％，晶型控制剂0.1～2％，水的用量以将全部物料溶解为准；所述的晶型控制剂为乙二醇、淀粉、乳化剂OP10或三乙醇胺。1. Dissolve soluble magnesium salt, precipitating agent sodium hydroxide and crystal form control agent in water as reaction raw materials to make reaction solution. The composition of reaction raw materials is 27% to 44% by weight of sodium hydroxide, and 55% to soluble magnesium salt 72%, 0.1-2% crystal form control agent, the amount of water is based on dissolving all materials; the crystal form control agent is ethylene glycol, starch, emulsifier OP10 or triethanolamine.
2、将反应溶液在20～90℃和搅拌条件下反应20～40min，搅拌速度为200～900rpm，获得的沉淀为前驱体。2. The reaction solution is reacted at 20-90° C. under stirring conditions for 20-40 minutes, the stirring speed is 200-900 rpm, and the obtained precipitate is a precursor.
3、将获得的前驱体在550～750℃条件下煅烧2～4h，获得棒状纳米氧化镁。3. Calcining the obtained precursor at 550-750° C. for 2-4 hours to obtain rod-shaped nano magnesium oxide.
上述的可溶性镁盐为氯化镁或硝酸镁。The above-mentioned soluble magnesium salt is magnesium chloride or magnesium nitrate.
上述的棒状纳米氧化镁的长径比为1.26～1.42，长度为38～75nm，直径为27～53nm。The aspect ratio of the rod-shaped nano magnesium oxide is 1.26-1.42, the length is 38-75nm, and the diameter is 27-53nm.
本发明的方法通过选取乙二醇、淀粉、乳化剂OP10或三乙醇胺作为晶型控制剂，同时通过控制沉淀条件获得松散的前驱体，再通过控制煅烧条件制成棒状纳米氧化镁；获得的棒状纳米氧化镁粒径和长径比可控。本发明的方法具有原料易得，工艺简单，适用于工业化生产等优点，在红外隐身材料技术领域具有良好的应用前景。In the method of the present invention, ethylene glycol, starch, emulsifier OP10 or triethanolamine are selected as the crystal form control agent, and at the same time, a loose precursor is obtained by controlling the precipitation conditions, and then rod-shaped nano-magnesia is made by controlling the calcination conditions; the obtained rod-shaped The particle size and aspect ratio of nano magnesium oxide are controllable. The method of the invention has the advantages of easy-to-obtain raw materials, simple process, and suitability for industrialized production, and has good application prospects in the technical field of infrared stealth materials.
附图说明Description of drawings
图1为本发明实施例1的棒状纳米氧化镁的TEM图。FIG. 1 is a TEM image of the rod-shaped nano-magnesia of Example 1 of the present invention.
图2为本发明实施例2的棒状纳米氧化镁的TEM图。Fig. 2 is a TEM image of the rod-shaped nano-magnesia of Example 2 of the present invention.
图3为本发明实施例1的棒状纳米氧化镁的XRD图。Fig. 3 is an XRD pattern of the rod-shaped nano-magnesia of Example 1 of the present invention.
图4为本发明实施例1的棒状纳米氧化镁的红外吸收特征图。Fig. 4 is an infrared absorption characteristic diagram of the rod-shaped nano-magnesia of Example 1 of the present invention.
具体实施方式Detailed ways
本发明实施例中采用的氯化镁和硝酸镁为工业级产品。The magnesium chloride and magnesium nitrate adopted in the embodiment of the present invention are industrial grade products.
本发明实施例中采用的乙二醇、淀粉、乳化剂OP10和三乙醇胺为工业级产品。The ethylene glycol, starch, emulsifier OP10 and triethanolamine used in the examples of the present invention are industrial grade products.
本发明实施例中采用的煅烧设备为马弗炉。The calcining equipment used in the embodiment of the present invention is a muffle furnace.
实施例1Example 1
将氯化镁、氢氧化钠和晶型控制剂乙二醇作为反应原料溶于水中，制成反应溶液，反应原料中氢氧化钠的重量百分比为27％，镁盐的重量百分比为72％，晶型控制剂的重量百分比为1％，水的用量以将全部物料溶解为准。Magnesium chloride, sodium hydroxide and crystal form control agent ethylene glycol are dissolved in water as reaction raw materials to make a reaction solution. The weight percentage of sodium hydroxide in the reaction raw materials is 27%, and the weight percentage of magnesium salt is 72%. Crystal form The weight percentage of the control agent is 1%, and the consumption of water is based on dissolving all the materials.
将反应溶液在20℃条件下搅拌反应40min，搅拌速度为900rpm，然后过滤将沉淀物与水相分离。The reaction solution was stirred and reacted at 20° C. for 40 min at a stirring speed of 900 rpm, and then filtered to separate the precipitate from the water phase.
将获得的沉淀物在550℃条件下煅烧4h，获得棒状纳米氧化镁。The obtained precipitate was calcined at 550° C. for 4 hours to obtain rod-shaped nano magnesium oxide.
棒状纳米氧化镁的长径比为1.26，长度为48nm，直径为38nm。The rod-shaped nano magnesium oxide has an aspect ratio of 1.26, a length of 48nm and a diameter of 38nm.
棒状纳米氧化镁的TEM图如图1所示。The TEM image of rod-shaped nano-magnesia is shown in Figure 1.
采用X-射线衍射法(XRD)计算纳米氧化镁颗粒粒径。试验所得样品通过荷兰帕纳科公司的X′Pert Pro型X-射线衍射仪检测，XRD可以很方便地提供纳米材料晶粒尺寸的数据。用XRD测量纳米材料晶粒尺寸大小的原理是基于衍射峰的宽度与晶粒尺寸有关这一现象。当晶粒尺寸小于100nm时，其衍射峰宽随晶粒大小变化显著，晶粒大小可采用Scherrer公式进行计算：The particle size of nano-magnesia particles was calculated by X-ray diffraction (XRD). The samples obtained in the test were detected by the X′Pert Pro X-ray diffractometer of PANalytical Company in the Netherlands. XRD can easily provide data on the grain size of nanomaterials. The principle of measuring the grain size of nanomaterials by XRD is based on the phenomenon that the width of the diffraction peak is related to the grain size. When the grain size is less than 100nm, the diffraction peak width varies significantly with the grain size, and the grain size can be calculated using the Scherrer formula:
D＝Kλ/B1/2cosθD＝Kλ/B 1/2 cosθ
式中，D为沿晶面垂直方向的厚度也可以认为是晶粒尺寸大小，K为衍射峰形的Scherrer常数，一般取0.89，λ为射线的波长，B1/2为衍射峰的半高宽，θ为布拉格衍射角度。In the formula, D is the thickness along the vertical direction of the crystal plane, which can also be considered as the grain size, K is the Scherrer constant of the diffraction peak shape, generally 0.89, λ is the wavelength of the ray, and B 1/2 is the half-height of the diffraction peak width, θ is the Bragg diffraction angle.
棒状纳米氧化镁的XRD图如图3所示；红外吸收特征如图4所示。The XRD pattern of rod-shaped nano-magnesia is shown in Figure 3; the infrared absorption characteristics are shown in Figure 4.
实施例2Example 2
将硝酸镁、氢氧化钠和晶型控制剂淀粉作为反应原料溶于水中，制成反应溶液，反应原料中氢氧化钠的重量百分比为44％，镁盐的重量百分比为55％，晶型控制剂的重量百分比为1％，水的用量以将全部物料溶解为准。Magnesium nitrate, sodium hydroxide and crystal form control agent starch are dissolved in water as reaction raw materials to make a reaction solution. The weight percentage of sodium hydroxide in the reaction raw materials is 44%, and the weight percentage of magnesium salt is 55%. Crystal form control The weight percent of agent is 1%, and the consumption of water is based on dissolving all materials.
将反应溶液在90℃条件下搅拌反应20min，搅拌速度为200rpm，然后过滤将沉淀物与水相分离。The reaction solution was stirred and reacted at 90° C. for 20 min at a stirring speed of 200 rpm, and then filtered to separate the precipitate from the water phase.
将获得的沉淀物在600℃条件下煅烧3h，获得棒状纳米氧化镁。The obtained precipitate was calcined at 600° C. for 3 hours to obtain rod-shaped nano magnesium oxide.
棒状纳米氧化镁的长径比为1.42，长度为75nm，直径为53nm。The rod-shaped nano magnesium oxide has an aspect ratio of 1.42, a length of 75nm and a diameter of 53nm.
棒状纳米氧化镁的TEM图如图2所示。The TEM image of rod-shaped nano-magnesia is shown in Figure 2.
实施例3Example 3
将氯化镁、氢氧化钠和晶型控制剂乳化剂OP10作为反应原料溶于水中，制成反应溶液，反应原料中氢氧化钠的重量百分比为39.5％，镁盐的重量百分比为60.4％，晶型控制剂的重量百分比为0.1％，水的用量以将全部物料溶解为准。Magnesium chloride, sodium hydroxide and crystal form control agent emulsifier OP10 are dissolved in water as reaction raw materials to make a reaction solution. In the reaction raw materials, the weight percentage of sodium hydroxide is 39.5%, and the weight percentage of magnesium salt is 60.4%, and the crystal form The weight percentage of the control agent is 0.1%, and the consumption of water is based on dissolving all the materials.
将反应溶液在50℃条件下搅拌反应30min，搅拌速度为600rpm，然后过滤将沉淀物与水相分离。The reaction solution was stirred and reacted at 50° C. for 30 min at a stirring speed of 600 rpm, and then filtered to separate the precipitate from the water phase.
将获得的沉淀物在700℃条件下煅烧3h，获得棒状纳米氧化镁。The obtained precipitate was calcined at 700° C. for 3 hours to obtain rod-shaped nano magnesium oxide.
棒状纳米氧化镁的长径比为1.41，长度为38nm，直径为27nm。The rod-shaped nano magnesium oxide has an aspect ratio of 1.41, a length of 38nm and a diameter of 27nm.
实施例4Example 4
将硝酸镁、氢氧化钠和晶型控制剂三乙醇胺作为反应原料溶于水中，制成反应溶液，反应原料中氢氧化钠的重量百分比为35％，镁盐的重量百分比为63％，晶型控制剂的重量百分比为2％，水的用量以将全部物料溶解为准。Magnesium nitrate, sodium hydroxide and crystal form control agent triethanolamine are dissolved in water as reaction raw materials to make a reaction solution. The weight percentage of sodium hydroxide in the reaction raw materials is 35%, and the weight percentage of magnesium salt is 63%. The crystal form The weight percent of the control agent is 2%, and the consumption of water is based on dissolving all the materials.
将反应溶液在60℃条件下搅拌反应30min，搅拌速度为400rpm，然后过滤将沉淀物与水相分离。The reaction solution was stirred and reacted at 60° C. for 30 min at a stirring speed of 400 rpm, and then filtered to separate the precipitate from the water phase.
将获得的沉淀物在750℃条件下煅烧2h，获得棒状纳米氧化镁。The obtained precipitate was calcined at 750° C. for 2 hours to obtain rod-shaped nano magnesium oxide.
棒状纳米氧化镁的长径比为1.38，长度为58nm，直径为42nm。The rod-shaped nano magnesium oxide has an aspect ratio of 1.38, a length of 58nm and a diameter of 42nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366696A (en) * | 2015-12-14 | 2016-03-02 | 苏州市泽镁新材料科技有限公司 | Method for preparing high-purity nanometer magnesia |
| CN106673590A (en) * | 2016-09-13 | 2017-05-17 | 内蒙古博大新型墙体材料研究所 | Novel heat preservation and isolation wall body material and preparation method thereof |
| CN112897559A (en) * | 2021-02-26 | 2021-06-04 | 绵阳远达电子材料有限公司 | Production process of magnesium hydroxide |
| CN113416592A (en) * | 2021-05-24 | 2021-09-21 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
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Non-Patent Citations (2)
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| 《中国粉体技术》 20090331 王小宇等 菱镁矿为原料制备纳米氧化镁粉体的工艺研究 第49页，1.2 试验方法，第52页2.3 纳米氧化镁的制备 1-3 第15卷, 2 * |
| 《科技资讯》 20071231 李宪平 均匀沉淀法制备纳米氧化镁的研究 第28页，2.4.2表面活性剂的选择和加入量的影响 1-3 , 第8期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105366696A (en) * | 2015-12-14 | 2016-03-02 | 苏州市泽镁新材料科技有限公司 | Method for preparing high-purity nanometer magnesia |
| CN106673590A (en) * | 2016-09-13 | 2017-05-17 | 内蒙古博大新型墙体材料研究所 | Novel heat preservation and isolation wall body material and preparation method thereof |
| CN112897559A (en) * | 2021-02-26 | 2021-06-04 | 绵阳远达电子材料有限公司 | Production process of magnesium hydroxide |
| CN113416592A (en) * | 2021-05-24 | 2021-09-21 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
| CN113416592B (en) * | 2021-05-24 | 2022-07-29 | 广西大学 | Preparation method of hydrophilic corn insulating oil modified by nano magnesium oxide |
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| CN101850993B (en) | 2012-02-22 |
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