CN101786673A - Synthesis method for basic cobalt carbonate ferrum nano material - Google Patents
Synthesis method for basic cobalt carbonate ferrum nano material Download PDFInfo
- Publication number
- CN101786673A CN101786673A CN 201010128596 CN201010128596A CN101786673A CN 101786673 A CN101786673 A CN 101786673A CN 201010128596 CN201010128596 CN 201010128596 CN 201010128596 A CN201010128596 A CN 201010128596A CN 101786673 A CN101786673 A CN 101786673A
- Authority
- CN
- China
- Prior art keywords
- sodium hydroxide
- mol
- solution
- mixed solution
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims description 29
- OBWXQDHWLMJOOD-UHFFFAOYSA-H cobalt(2+);dicarbonate;dihydroxide;hydrate Chemical compound O.[OH-].[OH-].[Co+2].[Co+2].[Co+2].[O-]C([O-])=O.[O-]C([O-])=O OBWXQDHWLMJOOD-UHFFFAOYSA-H 0.000 title claims description 6
- 238000001308 synthesis method Methods 0.000 title abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 90
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000011259 mixed solution Substances 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 32
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004472 Lysine Substances 0.000 claims abstract description 27
- DVMRIYBVDNCIOJ-UHFFFAOYSA-J cobalt(2+) iron(2+) dicarbonate Chemical compound [Fe+2].C([O-])([O-])=O.[Co+2].C([O-])([O-])=O DVMRIYBVDNCIOJ-UHFFFAOYSA-J 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010189 synthetic method Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 10
- XUYPXLNMDZIRQH-LURJTMIESA-N N-acetyl-L-methionine Chemical compound CSCC[C@@H](C(O)=O)NC(C)=O XUYPXLNMDZIRQH-LURJTMIESA-N 0.000 claims 6
- 229930182817 methionine Natural products 0.000 claims 6
- 238000005303 weighing Methods 0.000 claims 3
- 238000001035 drying Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 13
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910001981 cobalt nitrate Inorganic materials 0.000 abstract description 7
- 238000003760 magnetic stirring Methods 0.000 description 15
- 238000000034 method Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 229910021094 Co(NO3)2-6H2O Inorganic materials 0.000 description 3
- 239000004809 Teflon Substances 0.000 description 3
- 229920006362 Teflon® Polymers 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 235000013980 iron oxide Nutrition 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- QRXDDLFGCDQOTA-UHFFFAOYSA-N cobalt(2+) iron(2+) oxygen(2-) Chemical class [O-2].[Fe+2].[Co+2].[O-2] QRXDDLFGCDQOTA-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
本发明涉及的合成方法，包括下述步骤：1)将赖氨酸加入乙二醇中，搅拌，得0.04-0.12摩尔/升的赖氨酸溶液；2)按氯化铁与赖氨酸摩尔比为1∶1-1∶3，取氯化铁加入步骤1)的赖氨酸溶液中，搅拌，得混合溶液A；3)按硝酸钴与氯化铁的摩尔比为1∶1，取硝酸钴加入混合溶液A中，搅拌，得混合溶液B；4)按氢氧化钠与氯化铁的摩尔比为9∶1-15∶1取氢氧化钠，加入乙二醇中，搅拌，得0.6-1摩尔/升的氢氧化钠溶液；5)将步骤4)的氢氧化钠溶液滴加到混合溶液B中，搅拌得混合溶液C，其于180℃反应10小时，产物经洗涤、干燥，得碱式碳酸钴铁纳米材料。本发明具有简单、低成本、无污染、可控制产物形貌的特点。The synthesis method involved in the present invention comprises the following steps: 1) adding lysine to ethylene glycol and stirring to obtain a 0.04-0.12 mole/liter lysine solution; Ratio is 1: 1-1: 3, get ferric chloride and add in the lysine solution of step 1), stir, obtain mixed solution A; 3) be 1: 1 by the mol ratio of cobalt nitrate and ferric chloride, take Add cobalt nitrate into mixed solution A, stir to obtain mixed solution B; 4) take sodium hydroxide according to the molar ratio of sodium hydroxide to ferric chloride of 9:1-15:1, add it to ethylene glycol, and stir to obtain 0.6-1 mol/liter sodium hydroxide solution; 5) Add the sodium hydroxide solution in step 4) dropwise to the mixed solution B, and stir to obtain the mixed solution C, which is reacted at 180°C for 10 hours, and the product is washed and dried , to obtain basic cobalt iron carbonate nanomaterials. The invention has the characteristics of simplicity, low cost, no pollution and controllable product morphology.
Description
技术领域technical field
本发明涉及一种碱式碳酸钴铁纳米材料的合成方法。The invention relates to a synthesis method of basic cobalt iron carbonate nanometer material.
背景技术Background technique
碱式碳酸钴铁是一种重要的碳酸钴铁矿型材料，可用作阴离子交换剂、吸附剂、分子筛和催化剂等领域。碱式碳酸钴铁还可作为前驱物用于制备其他各种钴铁氧化物。Basic cobalt iron carbonate is an important cobalt iron carbonate type material, which can be used as anion exchanger, adsorbent, molecular sieve and catalyst. Basic cobalt iron carbonate can also be used as a precursor to prepare various other cobalt iron oxides.
不同形形貌的碱式碳酸钴铁具有不同的性质和应用。研究新型、可控地制备不同形貌碱式碳酸钴铁的方法，对阐释天然矿物质的转化和地球化学过程、八面体金属氢氧化物层结构的重组机理等具有重要意义。目前，用于制备碱式碳酸钴铁的方法主要是共沉淀法，而溶剂热合成法由于其易于操作、可控制目标产物的形貌等优点而受到广泛关注。Basic cobalt iron carbonate with different shapes and shapes has different properties and applications. The study of new and controllable methods for preparing basic cobalt iron carbonates with different shapes is of great significance for elucidating the transformation and geochemical processes of natural minerals and the recombination mechanism of octahedral metal hydroxide layer structures. At present, the method used to prepare basic cobalt iron carbonate is mainly the co-precipitation method, and the solvothermal synthesis method has attracted extensive attention due to its advantages such as easy operation and controllable morphology of the target product.
发明内容Contents of the invention
本发明的目的在于提供一种简单、低成本、无污染、形貌可控的碱式碳酸钴铁纳米材料的合成方法。The object of the present invention is to provide a simple, low-cost, pollution-free and shape-controllable synthesis method of basic cobalt iron carbonate nanometer material.
本发明所述的形貌可控是指八面体状或花状。The shape controllable in the present invention refers to octahedral shape or flower shape.
为了实现上述目的，本发明的技术方案是：一种碱式碳酸钴铁纳米材料的合成方法，其特征在于它包括如下步骤：In order to achieve the above object, the technical scheme of the present invention is: a kind of synthetic method of basic cobalt iron carbonate nanometer material, it is characterized in that it comprises the steps:
1)将赖氨酸加入乙二醇中，搅拌使赖氨酸溶解，制得浓度为0.04-0.12摩尔/升的赖氨酸溶液；1) adding lysine to ethylene glycol, stirring to dissolve the lysine, and preparing a lysine solution with a concentration of 0.04-0.12 mol/liter;
2)按氯化铁与赖氨酸的摩尔比为1∶1-1∶3的比例，称取氯化铁，加入步骤1)的赖氨酸溶液中，搅拌使其溶解，得混合溶液A；2) According to the ratio of ferric chloride to lysine molar ratio of 1:1-1:3, weigh ferric chloride, add it to the lysine solution in step 1), stir to dissolve it, and obtain mixed solution A ;
3)按硝酸钴与氯化铁的摩尔比为1∶1的比例，称取硝酸钴，加入步骤2)的混合溶液A中，搅拌使其溶解，得混合溶液B；3) According to the molar ratio of cobalt nitrate and ferric chloride being 1:1, weigh cobalt nitrate, add it in the mixed solution A of step 2), stir to dissolve it, and obtain mixed solution B;
4)按氢氧化钠与氯化铁的摩尔比为9∶1-15∶1的比例，称取氢氧化钠，加入乙二醇中，搅拌使其溶解，制得浓度为0.6-1摩尔/升的氢氧化钠溶液；4) According to the molar ratio of sodium hydroxide to ferric chloride of 9:1-15:1, weigh sodium hydroxide, add it to ethylene glycol, stir to dissolve it, and obtain a concentration of 0.6-1 mol/ liters of sodium hydroxide solution;
5)将步骤4)的氢氧化钠溶液滴加到混合溶液B中，搅拌得混合溶液C；混合溶液C于180℃反应10小时，产物经洗涤、干燥，得到碱式碳酸铁钴纳米材料。5) The sodium hydroxide solution in step 4) was added dropwise to the mixed solution B, and stirred to obtain a mixed solution C; the mixed solution C was reacted at 180° C. for 10 hours, and the product was washed and dried to obtain basic iron cobalt carbonate nanomaterials.
按上述方案，步骤1)中所述赖氨酸溶液的浓度为0.04摩尔/升，步骤2)中氯化铁与赖氨酸的摩尔比为1∶1，步骤4)中氢氧化钠与氯化铁的摩尔比为15∶1；氢氧化钠溶液的浓度为1摩尔/升。According to the above scheme, the concentration of the lysine solution described in step 1) is 0.04 mol/liter, and the mol ratio of ferric chloride and lysine in step 2) is 1: 1, and in step 4) sodium hydroxide and chlorine The molar ratio of iron oxide is 15:1; the concentration of sodium hydroxide solution is 1 mol/liter.
按上述方案，步骤1)中所述赖氨酸溶液的浓度为0.04摩尔/升，步骤2)中氯化铁与赖氨酸的摩尔比为1∶1，步骤4)中氢氧化钠与氯化铁的摩尔比为9∶1；氢氧化钠溶液的浓度为0.6摩尔/升。According to the above scheme, the concentration of the lysine solution described in step 1) is 0.04 mol/liter, and the mol ratio of ferric chloride and lysine in step 2) is 1: 1, and in step 4) sodium hydroxide and chlorine The molar ratio of iron oxide is 9:1; the concentration of sodium hydroxide solution is 0.6 mol/liter.
按上述方案，步骤1)中所述赖氨酸溶液的浓度为0.12摩尔/升，步骤2)中氯化铁与赖氨酸的摩尔比为1∶3，步骤4)中氢氧化钠与氯化铁的摩尔比为9∶1；氢氧化钠溶液的浓度为0.6摩尔/升。According to the above scheme, the concentration of the lysine solution described in step 1) is 0.12 mol/liter, and the mol ratio of ferric chloride and lysine in step 2) is 1: 3, and in step 4) sodium hydroxide and chlorine The molar ratio of iron oxide is 9:1; the concentration of sodium hydroxide solution is 0.6 mol/liter.
本发明的有益效果是：在简单的反应体系中，通过改变反应物的比例，实现了不同形貌碱式碳酸钴铁的可控合成。本发明方法所用试剂常用；合成步骤简单；产物形貌可控。所合成的不同形貌的碱式碳酸钴铁可用于阴离子交换剂、吸附剂、分子筛和催化剂等各个领域。The beneficial effect of the invention is: in a simple reaction system, by changing the ratio of reactants, the controllable synthesis of basic cobalt iron carbonate with different shapes is realized. The reagents used in the method of the invention are commonly used; the synthesis steps are simple; and the morphology of the product is controllable. The synthesized basic cobalt iron carbonate with different morphologies can be used in various fields such as anion exchangers, adsorbents, molecular sieves and catalysts.
附图说明Description of drawings
图1(a)是实施例1得到产物的扫描电镜照片。Fig. 1 (a) is the scanning electron micrograph of the product that embodiment 1 obtains.
图1(b)是实施例2得到产物的扫描电镜照片。Fig. 1 (b) is the scanning electron micrograph of the product that embodiment 2 obtains.
图1(c)是实施例3得到产物的扫描电镜照片。Fig. 1 (c) is the scanning electron micrograph of the product that embodiment 3 obtains.
图2(a)是实施例1得到产物的XRD图谱。Fig. 2 (a) is the XRD spectrum of the product obtained in Example 1.
图2(b)是实施例2得到产物的XRD图谱。Fig. 2 (b) is the XRD spectrum of the product obtained in Example 2.
图2(c)是实施例3得到产物的XRD图谱。Fig. 2 (c) is the XRD spectrum of the product obtained in Example 3.
具体实施方式Detailed ways
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the content of the present invention is not limited to the following examples.
实施例1：Example 1:
0.1462克赖氨酸加入25mL乙二醇中，在磁力搅拌下溶解；将0.2704克氯化铁[FeCl3·6H2O]加入上述赖氨酸溶液中，在磁力搅拌下溶解，得到混合溶液A；将0.2910克硝酸钴[Co(NO3)2·6H2O]加入混合溶液A中，在磁力搅拌下使之溶解，得到混合溶液B；0.6000克氢氧化钠加入15毫升乙二醇中，在磁力搅拌下溶解；将上述氢氧化钠溶液匀速滴加(在1-2分钟内滴完)到混合溶液B中，磁力搅拌20分钟后，得到混合溶液C；混合溶液C转入容积为50毫升的高压釜聚四氟乙烯内衬中，于180℃反应10小时。反应结束后，反应釜自然冷却到室温，用去离子水和乙醇交替离心(10000转/分×5分钟)洗涤；产物在60℃干燥4小时，得到花状碱式碳酸钴铁纳米材料。图1(a)是得到产物的扫描电镜照片，显示所得的产物为纳米片组装成的花状结构；图2(a)是得到产物的XRD图谱，与JCPDS卡片号：50-0235(Co5.84Fe2.16(OH)16(CO3)1.08·0.32H2O))对比，说明所得的产物为碱式碳酸钴铁。Add 0.1462 grams of lysine to 25 mL of ethylene glycol and dissolve under magnetic stirring; add 0.2704 grams of ferric chloride [FeCl 3 6H 2 O] to the above lysine solution and dissolve under magnetic stirring to obtain a mixed solution A 0.2910 gram of cobalt nitrate [Co(NO 3 ) 2 6H 2 O] was added in the mixed solution A, and dissolved under magnetic stirring to obtain the mixed solution B; 0.6000 gram of sodium hydroxide was added in 15 milliliters of ethylene glycol, Dissolve under magnetic stirring; Add the above-mentioned sodium hydroxide solution dropwise at a uniform speed (dropping within 1-2 minutes) into the mixed solution B, and after magnetic stirring for 20 minutes, a mixed solution C is obtained; the mixed solution C is transferred to a volume of 50 ml in an autoclave lined with Teflon and reacted at 180°C for 10 hours. After the reaction, the reactor was naturally cooled to room temperature, washed with deionized water and ethanol by alternating centrifugation (10,000 rpm x 5 minutes); the product was dried at 60°C for 4 hours to obtain flower-shaped basic cobalt iron carbonate nanomaterials. Fig. 1 (a) is a scanning electron micrograph of the obtained product, showing that the obtained product is a flower-like structure assembled by nanosheets; Fig. 2 (a) is the XRD pattern of the obtained product, which is related to the JCPDS card number: 50-0235 (Co 5.84 The comparison of Fe 2.16 (OH) 16 (CO 3 ) 1.08 ·0.32H 2 O)) shows that the obtained product is basic cobalt iron carbonate.
实施例2：Example 2:
0.1462克赖氨酸加入25mL乙二醇中，在磁力搅拌下溶解；将0.2704克氯化铁[FeCl3·6H2O]加入上述赖氨酸溶液中，在磁力搅拌下溶解，得到混合溶液A；将0.2910克硝酸钴[Co(NO3)2·6H2O]加入混合溶液A中，在磁力搅拌下使之溶解，得到混合溶液B；0.3600克氢氧化钠加入15毫升乙二醇中，在磁力搅拌下溶解；将上述氢氧化钠溶液匀速滴加(在1-2分钟内滴完)到混合溶液B中，磁力搅拌20分钟后，得到混合溶液C；混合溶液C转入容积为50毫升的高压釜聚四氟乙烯内衬中，于180℃反应10小时。反应结束后，反应釜自然冷却到室温，用去离子水和乙醇交替离心(10000转/分×5分钟)洗涤；产物在60℃干燥4小时，得到八面体状碱式碳酸钴铁纳米材料。图1(b)是得到产物的扫描电镜照片，显示所得的产物为八面体状结构；图2(b)是得到产物的XRD图谱，与JCPDS卡片号：50-0235(Co5.84Fe2.16(OH)16(CO3)1.08·0.32H2O))对比，说明所得的产物为碱式碳酸钴铁。Add 0.1462 grams of lysine to 25 mL of ethylene glycol and dissolve under magnetic stirring; add 0.2704 grams of ferric chloride [FeCl 3 6H 2 O] to the above lysine solution and dissolve under magnetic stirring to obtain a mixed solution A 0.2910 gram of cobalt nitrate [Co(NO 3 ) 2 6H 2 O] was added in the mixed solution A, and dissolved under magnetic stirring to obtain the mixed solution B; 0.3600 gram of sodium hydroxide was added in 15 milliliters of ethylene glycol, Dissolve under magnetic stirring; Add the above-mentioned sodium hydroxide solution dropwise at a uniform speed (dropping within 1-2 minutes) into the mixed solution B, and after magnetic stirring for 20 minutes, a mixed solution C is obtained; the mixed solution C is transferred to a volume of 50 ml in an autoclave lined with Teflon and reacted at 180°C for 10 hours. After the reaction, the reactor was naturally cooled to room temperature, washed with deionized water and ethanol by alternating centrifugation (10,000 rpm x 5 minutes); the product was dried at 60° C. for 4 hours to obtain octahedral basic cobalt iron carbonate nanomaterials. Fig. 1 (b) is the scanning electron micrograph of the obtained product, showing that the obtained product is an octahedral structure; Fig. 2 (b) is the XRD spectrum of the obtained product, and JCPDS card number: 50-0235 (Co 5.84 Fe 2.16 (OH ) 16 (CO 3 ) 1.08 ·0.32H 2 O)) comparison, indicating that the obtained product is basic cobalt iron carbonate.
实施例3：Example 3:
0.4386克赖氨酸加入25mL乙二醇中，在磁力搅拌下溶解；将0.2704克氯化铁[FeCl3·6H2O]加入上述赖氨酸溶液中，在磁力搅拌下溶解，得到混合溶液A；将0.2910克硝酸钴[Co(NO3)2·6H2O]加入混合溶液A中，在磁力搅拌下使之溶解，得到混合溶液B；0.3600克氢氧化钠加入15毫升乙二醇中，在磁力搅拌下溶解；将上述氢氧化钠溶液匀速滴加(在1-2分钟内滴完)到混合溶液B中，磁力搅拌20分钟后，得到混合溶液C；混合溶液C转入容积为50毫升的高压釜聚四氟乙烯内衬中，于180℃反应10小时。反应结束后，反应釜自然冷却到室温，用去离子水和乙醇交替离心(10000转/分×5分钟)洗涤；产物在60℃干燥4小时，得到八面体状和纳米粒子状碱式碳酸钴铁纳米材料。图1(c)是得到产物的扫描电镜照片，显示所得的产物含有八面体状结构和纳米粒子状结构；图2(c)是得到产物的XRD图谱，与JCPDS卡片号：50-0235(Co5.84Fe2.16(OH)16(CO3)1.08·0.32H2O))对比，说明所得的产物为碱式碳酸钴铁。Add 0.4386 g of lysine to 25 mL of ethylene glycol and dissolve under magnetic stirring; add 0.2704 g of ferric chloride [FeCl 3 6H 2 O] to the above lysine solution and dissolve under magnetic stirring to obtain a mixed solution A 0.2910 gram of cobalt nitrate [Co(NO 3 ) 2 6H 2 O] was added in the mixed solution A, and dissolved under magnetic stirring to obtain the mixed solution B; 0.3600 gram of sodium hydroxide was added in 15 milliliters of ethylene glycol, Dissolve under magnetic stirring; Add the above-mentioned sodium hydroxide solution dropwise at a uniform speed (dropping within 1-2 minutes) into the mixed solution B, and after magnetic stirring for 20 minutes, a mixed solution C is obtained; the mixed solution C is transferred to a volume of 50 ml in an autoclave lined with Teflon and reacted at 180°C for 10 hours. After the reaction, the reactor was naturally cooled to room temperature, and washed with deionized water and ethanol by alternating centrifugation (10000 rpm × 5 minutes); the product was dried at 60°C for 4 hours to obtain octahedral and nanoparticle-like basic cobalt carbonate iron nanomaterials. Fig. 1 (c) is the scanning electron micrograph that obtains the product, shows that the product of obtaining contains octahedral structure and nanoparticle-like structure; Fig. 2 (c) is the XRD pattern that obtains the product, and JCPDS card number: 50-0235 (Co 5.84 Fe 2.16 (OH) 16 (CO 3 ) 1.08 ·0.32H 2 O)) comparison, indicating that the obtained product is basic cobalt iron carbonate.
本发明方法中所用的赖氨酸，英文名称为lysine，分子量为146.2，其结构式如下：H2NCH2CH2CH2CH2CH(NH2)COOH。The lysine used in the method of the present invention has an English name of lysine, a molecular weight of 146.2, and its structural formula is as follows: H 2 NCH 2 CH 2 CH 2 CH 2 CH(NH 2 )COOH.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101285965A CN101786673B (en) | 2010-03-18 | 2010-03-18 | Synthesis method for basic cobalt carbonate ferrum nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101285965A CN101786673B (en) | 2010-03-18 | 2010-03-18 | Synthesis method for basic cobalt carbonate ferrum nano material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101786673A true CN101786673A (en) | 2010-07-28 |
| CN101786673B CN101786673B (en) | 2011-11-02 |
Family
ID=42530074
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101285965A Expired - Fee Related CN101786673B (en) | 2010-03-18 | 2010-03-18 | Synthesis method for basic cobalt carbonate ferrum nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101786673B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560656A (en) * | 2010-12-22 | 2012-07-11 | 中国科学院大连化学物理研究所 | Preparation method of micron flower-like composite metal basic carbonate |
| CN102731078A (en) * | 2012-06-26 | 2012-10-17 | 武汉理工大学 | Octahedral porous cobalt ferrite material and its preparation method |
| CN103887500A (en) * | 2014-04-15 | 2014-06-25 | 山东大学 | Rod-like cobalt carbonate iron composite material and application thereof |
| CN105047421A (en) * | 2015-06-15 | 2015-11-11 | 昆明理工大学 | Method for preparing graphene/basic carbonate nanocomposite material |
| CN105185606A (en) * | 2015-09-14 | 2015-12-23 | 南京大学 | Preparation method of novel cobaltous dihydroxycarbonate-nitrogen-doped graphene combined electrode material |
| CN110475752A (en) * | 2017-03-08 | 2019-11-19 | 尤米科尔公司 | The precursor of cathode material for rechargable lithium ion cell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1185143A (en) * | 1995-05-26 | 1998-06-17 | H·C·施塔克公司 | Basic cobalt carbonates, production methods and uses thereof |
| CN1736882A (en) * | 2005-08-05 | 2006-02-22 | 北京化工大学 | A kind of preparation method of mesoporous structure Co3O4 nanocrystal |
| CN101486494A (en) * | 2009-02-20 | 2009-07-22 | 武汉理工大学 | Method for synthesizing cobalt carbonate hydroxide nano material |
-
2010
- 2010-03-18 CN CN2010101285965A patent/CN101786673B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1185143A (en) * | 1995-05-26 | 1998-06-17 | H·C·施塔克公司 | Basic cobalt carbonates, production methods and uses thereof |
| CN1736882A (en) * | 2005-08-05 | 2006-02-22 | 北京化工大学 | A kind of preparation method of mesoporous structure Co3O4 nanocrystal |
| CN101486494A (en) * | 2009-02-20 | 2009-07-22 | 武汉理工大学 | Method for synthesizing cobalt carbonate hydroxide nano material |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560656A (en) * | 2010-12-22 | 2012-07-11 | 中国科学院大连化学物理研究所 | Preparation method of micron flower-like composite metal basic carbonate |
| CN102560656B (en) * | 2010-12-22 | 2015-10-28 | 中国科学院大连化学物理研究所 | The preparation method of micron flower-like composite metal basic carbonate |
| CN102731078A (en) * | 2012-06-26 | 2012-10-17 | 武汉理工大学 | Octahedral porous cobalt ferrite material and its preparation method |
| CN103887500A (en) * | 2014-04-15 | 2014-06-25 | 山东大学 | Rod-like cobalt carbonate iron composite material and application thereof |
| CN105047421A (en) * | 2015-06-15 | 2015-11-11 | 昆明理工大学 | Method for preparing graphene/basic carbonate nanocomposite material |
| CN105047421B (en) * | 2015-06-15 | 2017-11-10 | 昆明理工大学 | A kind of preparation method of graphene/subcarbonate nano composite material |
| CN105185606A (en) * | 2015-09-14 | 2015-12-23 | 南京大学 | Preparation method of novel cobaltous dihydroxycarbonate-nitrogen-doped graphene combined electrode material |
| CN110475752A (en) * | 2017-03-08 | 2019-11-19 | 尤米科尔公司 | The precursor of cathode material for rechargable lithium ion cell |
| CN110475752B (en) * | 2017-03-08 | 2022-08-09 | 尤米科尔公司 | Precursor for cathode material for rechargeable lithium ion batteries |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101786673B (en) | 2011-11-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101786673A (en) | Synthesis method for basic cobalt carbonate ferrum nano material | |
| CN105214664B (en) | A kind of Copper-cladding Aluminum Bar Fe3O4Magnetic composite nano material and its preparation method and application | |
| CN101481107B (en) | Preparation method of nickel zinc ferrite (Ni1-xZnxFe2O4) coated carbon nanotube magnetic nanocomposite material | |
| Wang et al. | Facile and large-scale syntheses of nanocrystal rare earth metal–organic frameworks at room temperature and their photoluminescence properties | |
| CN101499341A (en) | Preparation of carbon nano-tube(MWCNTs)/manganese-zinc ferrite(Mn1-xZnxFe2O4) magnetic nano material by alcohol-thermal method | |
| CN103936796B (en) | A kind of based on flexible double Pyridine bisamide parts and the cobalt complex of benzene dicarboxylic acid and synthetic method thereof with application | |
| CN102040203A (en) | Preparation method and application of nano nickel phosphide | |
| CN101486494A (en) | Method for synthesizing cobalt carbonate hydroxide nano material | |
| CN106542560B (en) | A kind of preparation method of rare earth oxysulfate | |
| CN103170336A (en) | Preparation method of graphene/ferrite composite micron spherical photocatalyst | |
| CN105457662B (en) | A kind of 3D bouquets structure BiOCl-ZnFe2O4Composite photocatalyst material and preparation method thereof | |
| CN114873611A (en) | Method for preparing 3D hollow macroporous Co/Fe PBA nano cage structure material in situ by one-pot method and application thereof | |
| CN103303980B (en) | The method of sulfonated lignin template synthesis nano-sized iron oxide | |
| CN101560101A (en) | Method for preparing cobalt zinc ferrite (CoxZn1-xFe2O4) magnetic nano powder by using alcohol thermal method | |
| CN108996557B (en) | A kind of hollow spherical structure nickel oxide/copper oxide composite nanomaterial and preparation method thereof | |
| Xing et al. | High-valence-state nickel-iron phosphonates with urchin-like hierarchical architecture for highly efficient oxygen evolution reaction | |
| CN102773119A (en) | Tantalum-tungsten mixed polyoxometallate photocatalyst for generating hydrogen activity and preparation method thereof | |
| CN108461764A (en) | Air cell oxygen cathode bifunctional catalyst spherical metal phthalocyanine and preparation method thereof | |
| CN106732396A (en) | Magnetic Fe3O4@plant phenols/polyamines nano-complex adsorbent and preparation method and application | |
| CN110684533A (en) | SiO (silicon dioxide)2Preparation method of europium cuprate nano fluorescent and electrocatalytic powder | |
| CN101298102A (en) | Preparation of nano cobalt granule | |
| CN103145535A (en) | Diethylene glycol ferrous alkoxide with three-dimensional pattern multi-stage structure and preparation method thereof | |
| CN114849716A (en) | 1D/2D composite material based on NiZn-LDH and preparation method and application thereof | |
| CN103112896A (en) | Method for preparing octahedral nano bismuth vanadate photocatalyst by microwave process | |
| CN100486901C (en) | Synthesis method of cobaltosic oxide nano-tube |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111102 Termination date: 20140318 |