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申请/专利权人：桂林理工大学

申请日：2014-06-25

公开（公告）日：2014-09-10

公开（公告）号：CN104036912A

专利技术分类：.有机材料的或有机磁性材料的（H01F1/44优先）[2006.01]

专利摘要：本发明公开了一种磁性材料HNC2H53·[Ni4Na3heb6N36]及合成方法。磁性材料HNC2H53·[Ni4Na3heb6N36]的分子式为：C60H71N19Na3Ni4O18分子量为：1650.09，Hheb为3-乙氧基-2-羟基苯甲醛。将0.166克分析纯3-乙氧基-2-羟基苯甲醛溶于4-8毫升分析纯甲醇与4-8毫升分析纯乙腈的混合溶液中，依次加入0.36-0.72g分析纯六水合高氯酸镍和0.065-0.13g分析纯叠氮化钠，搅拌10钟，加入分析纯三乙胺调节至pH=5.5，搅拌20分钟后，静置，过滤，用分析纯甲醇洗涤，于空气中晾干后得到产品。HNC2H53·[Ni4Na3heb6N36]的磁学性质：分子内镍离子间存在铁磁交换，其整体表现为铁磁性。本发明具有工艺简单、成本低廉、化学组分易于控制和重复性好并产量高等优点。

专利权项：一种磁性材料HNC2H53·[Ni4Na3heb6N36]，其特征在于HNC2H53·[Ni4Na3heb6N36]分子式为：C60H71N19Na3Ni4O18，分子量为：1650.09，其中Hheb为3‑乙氧基‑2‑羟基苯甲醛，晶体结构数据见表一,键长键角数据见表二；HNC2H53·[Ni4Na3heb6N36]的磁学性质：1分子内镍离子间存在铁磁交换，其整体表现为铁磁性；2HNC2H53·[Ni4Na3heb6N36]在室温下χMT为5.84cm3Kmol‑1，随着温度降低，χMT逐渐升高，至35K达到最大值14.67cm3Kmol‑1，随后急剧降至2K时的5.7cm3Kmol‑1；且χM–1‑T曲线遵从居里‑韦斯定律，对其拟合得到韦斯常数为39.34K，居里常数为5.18cm3Kmol–1；大而正的韦斯常数及χMT‑T曲线趋势均暗示分子内镍离子间存在铁磁交换，其整体表现为铁磁性；所述HNC2H53·[Ni4Na3heb6N36]的合成方法具体步骤为：将0.166克分析纯3‑乙氧基‑2‑羟基苯甲醛溶于4‑8毫升分析纯甲醇与4‑8毫升分析纯乙腈的混合溶液中，再依次加入0.36‑0.72g分析纯六水合高氯酸镍和0.065‑0.13g分析纯叠氮化钠，搅拌10钟使溶液混合均匀后，加入分析纯三乙胺调节至pH＝5.5，继续搅拌20分钟后，将所制得的混合液静置于室温下，30分钟后得到绿色条状晶体，过滤，并用分析纯甲醇洗涤干净，于空气中晾干后得到产品HNC2H53·[Ni4Na3heb6N36]；表一HNC2H53·[Ni4Na3heb6N36]·CH3OH的晶体学参数表二HNC2H53·[Ni4Na3heb6N36]·CH3OH的键长和键角°C1‑O11.2866C46‑C471.4147Ni3‑O162.0083C1‑C21.4037C46‑C511.4287Ni3‑O142.0463C1‑C61.4317C47‑C481.4217Ni3‑O172.0554C2‑C31.4058C47‑C541.4288Ni4‑O101.9993C2‑C91.4388C48‑C491.3538Ni4‑O72.0193C3‑C41.3409C48‑H480.9300Ni4‑O112.0393C3‑H30.9300C49‑C501.3768Ni4‑O82.0624C4‑C51.4069C49‑H490.9300Ni3‑O162.0083C4‑H40.9300C50‑C511.3887Ni2‑O12.0053C5‑C61.3747C50‑H500.9300Ni2‑O42.0203C5‑H50.9300C51‑O181.3756Ni2‑O22.0494C6‑O31.3766C52‑O181.4246Ni2‑O52.0624C7‑O31.4516C52‑C531.4718Ni3‑O131.9923C7‑C81.4798C52‑H52A0.9700Na3‑O72.2324C7‑H7A0.9700C52‑H52B0.9700Na3‑O42.2364C7‑H7B0.9700C53‑H53A0.9600Na3‑O62.4554C8‑H8A0.9600C53‑H53B0.9600Na2‑O132.2383C8‑H8B0.9600C53‑H53C0.9600Na2‑O102.2523C8‑H8C0.9600C54‑O171.2336Na2‑O152.4294C9‑O21.2256C54‑H540.9300Na2‑O122.4514C9‑H90.9300C55‑C561.43115Na1‑O32.4694C10‑O41.2966C55‑H55A0.9600N16‑Ni12.1314C10‑C151.3947C55‑H55B0.9600N16‑Na22.5474C10‑C111.4147C55‑H55C0.9600N17‑N181.1426C11‑C121.4198C56‑N191.45213N19‑H19A0.9104C11‑C181.4168C56‑H56A0.9700Na1‑O12.2444C12‑C131.3179C56‑H56B0.9700Na1‑O162.2524C12‑H120.9300C57‑N191.5208Na1‑O182.4144C13‑C141.40910C57‑C581.92018N14‑N151.1526C13‑H130.9300C57‑H57A0.9700C30‑C311.3548C14‑C151.3758C57‑H57B0.9700N16‑N171.1935C14‑H140.9300C58‑H58A0.9606N16‑Ni32.1203C15‑O61.3666C58‑H58B0.9606N10‑Na12.5654C16‑C171.42910C58‑H58C0.9606N11‑N121.1266C16‑O61.4587C59‑N191.41212N13‑N141.1935C16‑H16A0.9700C59‑C601.46313N13‑Ni12.1063C16‑H16B0.9700C59‑H59A0.9700N13‑Ni42.1094C17‑H17A0.9600C59‑H59B0.9700N13‑Na32.5604C17‑H17B0.9600C60‑H60A0.9600C32‑H32A0.9700C17‑H17C0.9600C60‑H60B0.9600C32‑H32B0.9700C18‑O51.2216C60‑H60C0.9600C34‑H34A0.9700C18‑H180.9300N1‑N21.1805C34‑H34B0.9700C19‑O71.2825N1‑Ni22.0984C29‑C301.4187C19‑C201.4077N1‑Ni12.1264C29‑C361.4258C19‑C241.4117N1‑Na32.5624C43‑H43A0.9700C30‑H300.9300N2‑N31.1317C43‑H43B0.9700C20‑C211.4267N2‑Na33.0525C44‑H44A0.9600C20‑C271.4408N4‑N51.1765C44‑H44B0.9600C21‑C221.3109N4‑Ni12.1313C44‑H44C0.9600C21‑H210.9300N4‑Ni32.1344C45‑O141.2376C22‑C231.3859N4‑Na12.5524C45‑H450.9300C22‑H220.9300N5‑N61.1466C46‑O161.2825C23‑C241.3717C32‑C331.3557C39‑H390.9300C23‑H230.9300N7‑N81.1755C40‑C411.3778C24‑O91.3787N7‑Ni42.1133C40‑H400.9300C25‑O91.4487N7‑Ni12.1394C41‑C421.3677C25‑C261.4729N7‑Na22.5134C41‑H410.9300C25‑H25A0.9700N8‑N91.1436C42‑O151.3836C25‑H25B0.9700N10‑N111.1905C43‑O151.4416C26‑H26A0.9600N10‑Ni22.1094C43‑C441.5058C26‑H26B0.9600N10‑Ni12.1324C36‑H360.9300C26‑H26C0.9600C35‑H35A0.9600C37‑O131.2946C27‑O81.2387C35‑H35B0.9600C37‑C421.4217C27‑H270.9300C35‑H35C0.9600C37‑C381.4317C28‑O101.2935C36‑O111.2346C38‑C451.4147C28‑C331.4157C33‑O121.3836C39‑C401.3488C28‑C291.4277C34‑O121.4196C31‑H310.9300C31‑C321.4108C34‑C351.5178  O1‑C1‑C2125.25O16‑Na1‑N1090.2413C42‑C41‑C40119.76O1‑C1‑C6118.85O18‑Na1‑N1097.1313C42‑C41‑H41120.2C2‑C1‑C6116.05O3‑Na1‑N10139.4414C40‑C41‑H41120.2C1‑C2‑C3121.36N4‑Na1‑N1073.3512C1‑O1‑Na1124.23C1‑C2‑C9121.45N19‑C59‑H59A105.3N16‑Ni1‑N1094.8614C3‑C2‑C9117.36C39‑C40‑H40119.4N4‑Ni1‑N1091.6114C4‑C3‑C2121.46C59‑C60‑H60A109.5N13‑Ni1‑N779.3414C4‑C3‑H3119.3C40‑C39‑H39119.5C41‑C42‑O15125.15C2‑C3‑H3119.3C38‑C39‑H39119.5C41‑C42‑C37122.35C3‑C4‑C5119.26C39‑C40‑C41121.36O15‑C42‑C37112.64C3‑C4‑H4120.4C46‑O16‑Ni3129.43O15‑C43‑C44107.05C5‑C4‑H4120.4C46‑O16‑Na1123.93O15‑C43‑H43A110.3C6‑C5‑C4120.76Ni3‑O16‑Na1106.3913C44‑C43‑H43A110.3C6‑C5‑H5119.6C54‑O17‑Ni3126.04O15‑C43‑H43B110.3C4‑C5‑H5119.6C51‑O18‑C52118.44C44‑C43‑H43B110.3C5‑C6‑O3124.75C51‑O18‑Na1116.53H43A‑C43‑H43B108.6C5‑C6‑C1121.26C52‑O18‑Na1125.04C43‑C44‑H44A109.5O3‑C6‑C1114.05O1‑Na1‑O367.1913C43‑C44‑H44B109.5O3‑C7‑C8107.45O16‑Na1‑O3127.0214H44A‑C44‑H44B109.5O3‑C7‑H7A110.2O18‑Na1‑O3110.7814C43‑C44‑H44C109.5C8‑C7‑H7A110.2O1‑Na1‑N491.8714H44A‑C44‑H44C109.5O3‑C7‑H7B110.2O16‑Na1‑N472.7713H44B‑C44‑H44C109.5C8‑C7‑H7B110.2O18‑Na1‑N4139.0715N1‑Ni1‑N793.4415H7A‑C7‑H7B108.5O3‑Na1‑N4100.4514N16‑Ni1‑N792.9015C7‑C8‑H8A109.5O1‑Na1‑N1072.9313N4‑Ni1‑N794.3714C7‑C8‑H8B109.5Ni3‑O13‑Na2106.9814N10‑Ni1‑N7170.9214H8A‑C8‑H8B109.5C45‑O14‑Ni3127.03C56‑N19‑C57107.39C7‑C8‑H8C109.5C42‑O15‑C43116.34C59‑N19‑H19A104.2H8A‑C8‑H8C109.5C42‑O15‑Na2116.73C56‑N19‑H19A112.7H8B‑C8‑H8C109.5C43‑O15‑Na2126.73Ni3‑N16‑Ni1100.2215O2‑C9‑C2130.06C57‑N19‑H19A97.9N17‑N16‑Na2110.73O2‑C9‑H9115.0O1‑Na1‑O16160.1114Ni3‑N16‑Na293.1714C2‑C9‑H9115.0O1‑Na1‑O18124.0015Ni1‑N16‑Na295.4614O4‑C10‑C15118.65O16‑Na1‑O1867.4713N18‑N17‑N16177.26O4‑C10‑C11123.25O13‑Na2‑O10162.8316C59‑N19‑C56112.010C15‑C10‑C11118.25O13‑Na2‑O1567.5712C59‑N19‑C57121.910C10‑C11‑C12119.36O10‑Na2‑O15125.6314Ni3‑N16‑Ni1100.2215C10‑C11‑C18122.55O13‑Na2‑O12121.0814O14‑C45‑C38127.95C12‑C11‑C18118.26O10‑Na2‑O1267.8912O14‑C45‑H45116.0C13‑C12‑C11122.27O15‑Na2‑O12109.0615C38‑C45‑H45116.0C13‑C12‑H12118.9O13‑Na2‑N793.7014O16‑C46‑C47124.95C11‑C12‑H12118.9O10‑Na2‑N773.4813O16‑C46‑C51118.15C12‑C13‑C14118.37O15‑Na2‑N7102.6714C47‑C46‑C51117.05C12‑C13‑H13120.9O12‑Na2‑N7139.5813C46‑C47‑C48120.06C14‑C13‑H13120.9O13‑Na2‑N1672.4712Ni1‑N13‑Na398.3415C15‑C14‑C13122.37O10‑Na2‑N1692.8913Ni4‑N13‑Na393.0113C15‑C14‑H14118.8O15‑Na2‑N16139.8213N15‑N14‑N13176.46C13‑C14‑H14118.8O12‑Na2‑N1694.8214C59‑C60‑H60B109.5O6‑C15‑C14125.76N7‑Na2‑N1675.4013C39‑C38‑C37119.15O6‑C15‑C10114.75C28‑O10‑Na2121.53N17‑N16‑Ni3121.43C14‑C15‑C10119.66Ni4‑O10‑Na2105.0214N17‑N16‑Ni1127.93C17‑C16‑O6109.76C36‑O11‑Ni4125.73C46‑C47‑C54121.75C17‑C16‑H16A109.7C33‑O12‑C34116.94C48‑C47‑C54118.35O6‑C16‑H16A109.7C33‑O12‑Na2114.43C49‑C48‑C47121.06C17‑C16‑H16B109.7C34‑O12‑Na2125.03C49‑C48‑H48119.5O6‑C16‑H16B109.7C37‑O13‑Ni3129.63C47‑C48‑H48119.5H16A‑C16‑H16B108.2C37‑O13‑Na2123.33C48‑C49‑C50120.36C16‑C17‑H17A109.5C24‑O9‑C25120.85C48‑C49‑H49119.9C16‑C17‑H17B109.5C24‑O9‑Na3116.03C50‑C49‑H49119.9H17A‑C17‑H17B109.5C25‑O9‑Na3123.14C41‑C40‑H40119.4C16‑C17‑H17C109.5C28‑O10‑Ni4129.03H58A‑C58‑H58C109.4H17A‑C17‑H17C109.5C18‑O5‑Ni2125.64H58B‑C58‑H58C109.4H17B‑C17‑H17C109.5C15‑O6‑C16117.95O1‑Ni2‑O4176.3915O5‑C18‑C11129.96C15‑O6‑Na3115.33O1‑Ni2‑O288.8014O5‑C18‑H18115.0C16‑O6‑Na3125.34O4‑Ni2‑O289.1815C11‑C18‑H18115.0C19‑O7‑Ni4130.94O1‑Ni2‑O589.8715O7‑C19‑C20123.55C19‑O7‑Na3122.64O4‑Ni2‑O587.3215O7‑C19‑C24120.05Ni4‑O7‑Na3106.1314C49‑C50‑C51121.06C20‑C19‑C24116.55C27‑O8‑Ni4126.04C49‑C50‑H50119.5C19‑C20‑C21120.16Ni1‑N10‑Na197.3114C50‑C51‑C46120.76C19‑C20‑C27122.75N12‑N11‑N10176.86O18‑C52‑C53109.85C21‑C20‑C27117.26N14‑N13‑Ni1128.63O18‑C52‑H52A109.7C22‑C21‑C20121.07N14‑N13‑Ni4124.83O2‑Ni2‑O594.8416C22‑C21‑H21119.5Ni1‑N13‑Ni4100.9815O1‑Ni2‑N193.9715C20‑C21‑H21119.5N14‑N13‑Na3101.03O4‑Ni2‑N189.0914C21‑C22‑C23120.46C1‑O1‑Ni2128.83O2‑Ni2‑N192.1616C21‑C22‑H22119.8O7‑Na3‑O4161.6915O5‑Ni2‑N1172.0915C23‑C22‑H22119.8O7‑Na3‑O967.9114O1‑Ni2‑N1088.4213C24‑C23‑C22120.87O4‑Na3‑O9124.9317O4‑Ni2‑N1093.9814C24‑C23‑H23119.6O7‑Na3‑O6125.5315O2‑Ni2‑N10171.9215C22‑C23‑H23119.6O4‑Na3‑O666.7414C53‑C52‑H52A109.7C23‑C24‑O9125.86O9‑Na3‑O6106.0115O18‑C52‑H52B109.7C23‑C24‑C19121.06O7‑Na3‑N1372.9213C53‑C52‑H52B109.7O9‑C24‑C19113.24O4‑Na3‑N1392.3014H52A‑C52‑H52B108.2O9‑C25‑C26111.66O9‑Na3‑N13140.5416C52‑C53‑H53A109.5O9‑C25‑H25A109.3O6‑Na3‑N13100.2514O5‑Ni2‑N1092.7415C26‑C25‑H25A109.3O7‑Na3‑N191.2213N1‑Ni2‑N1080.4714O9‑C25‑H25B109.3O4‑Na3‑N173.6913N9‑N8‑N7179.18C26‑C25‑H25B109.3O9‑Na3‑N1103.2714N11‑N10‑Ni2122.63H25A‑C25‑H25B108.0O6‑Na3‑N1139.5115N11‑N10‑Ni1130.43C25‑C26‑H26A109.5N13‑Na3‑N172.5213C52‑C53‑H53B109.5C25‑C26‑H26B109.5C6‑O3‑Na1115.13H53A‑C53‑H53B109.5H26A‑C26‑H26B109.5C7‑O3‑Na1126.43C52‑C53‑H53C109.5C25‑C26‑H26C109.5C10‑O4‑Ni2129.93H53A‑C53‑H53C109.5H26A‑C26‑H26C109.5C10‑O4‑Na3123.93H53B‑C53‑H53C109.5H26B‑C26‑H26C109.5Ni2‑O4‑Na3104.7015O17‑C54‑C47129.45O8‑C27‑C20128.96C47‑C54‑H54115.3O17‑C54‑H54115.3O8‑C27‑H27115.5H60A‑C60‑H60B109.5C56‑C55‑H55A109.5C20‑C27‑H27115.5C59‑C60‑H60C109.5Ni2‑O1‑Na1105.8715O10‑C28‑C33120.35H60A‑C60‑H60C109.5C9‑O2‑Ni2125.24O10‑C28‑C29122.75H59A‑C59‑H59B106.0C6‑O3‑C7116.84C33‑C28‑C29117.05N16‑Ni3‑N480.0914N8‑N7‑Ni4124.23N19‑C59‑H59B105.3Ni2‑N1‑Na392.1814N8‑N7‑Ni1125.73C60‑C59‑H59B105.3N13‑Ni1‑N1695.1114Ni4‑N7‑Ni199.8015H60B‑C60‑H60C109.5N1‑Ni1‑N16171.6614N8‑N7‑Na2109.74C36‑C29‑C28122.85N5‑N4‑Ni3123.13Ni4‑N7‑Na293.3314C36‑C29‑C30117.85Ni1‑N4‑Ni399.7815Ni1‑N7‑Na296.2414C28‑C29‑C30119.35N5‑N4‑Na1102.83C56‑C55‑H55B109.5C31‑C30‑C29121.46Ni1‑N4‑Na197.7314H55A‑C55‑H55B109.5C31‑C30‑H30119.3Ni3‑N4‑Na193.1113C56‑C55‑H55C109.5C29‑C30‑H30119.3N6‑N5‑N4176.36H55A‑C55‑H55C109.5C30‑C31‑C32119.46N6‑N5‑Na1121.45H55B‑C55‑H55C109.5C30‑C31‑H31120.3N4‑N5‑Na155.03C55‑C56‑N19114.612C32‑C31‑H31120.3N3‑N2‑N1177.48C55‑C56‑H56A108.6C33‑C32‑C31120.76C60‑C59‑H59A105.3N19‑C56‑H56A108.6C33‑C32‑H32A107.2C40‑C39‑C38121.16N19‑C59‑C60128.011C31‑C32‑H32A107.2N5‑N4‑Ni1130.53O13‑Ni3‑O16179.2213C33‑C32‑H32B107.2O11‑Ni4‑N7170.6814O13‑Ni3‑O1488.6513C31‑C32‑H32B107.2O8‑Ni4‑N794.8014O16‑Ni3‑O1490.7113H32A‑C32‑H32B106.8N13‑Ni4‑N779.8814O13‑Ni3‑O1791.3015C32‑C33‑O12124.15O8‑Ni4‑N13172.6415O16‑Ni3‑O1788.2714C32‑C33‑C28122.05O10‑Ni4‑N788.0314O14‑Ni3‑O1791.8215O12‑C33‑C28113.95O7‑Ni4‑N794.5614O13‑Ni3‑N1687.3013O12‑C34‑C35107.75N2‑N1‑Ni2123.14C55‑C56‑H56B108.6O12‑C34‑H34A110.2N2‑N1‑Ni1130.34N19‑C56‑H56B108.6C35‑C34‑H34A110.2Ni2‑N1‑Ni1100.3815H56A‑C56‑H56B107.6O12‑C34‑H34B110.2N2‑N1‑Na3103.03N19‑C57‑C5899.58C35‑C34‑H34B110.2O7‑Ni4‑O1189.2414N19‑C57‑H57A111.9H34A‑C34‑H34B108.5O10‑Ni4‑O890.9415O16‑Ni3‑N1693.3914C34‑C35‑H35A109.5O7‑Ni4‑O887.6814O14‑Ni3‑N16171.8315C34‑C35‑H35B109.5O11‑Ni4‑O893.8615O17‑Ni3‑N1695.3614H35A‑C35‑H35B109.5O10‑Ni4‑N1393.9315O13‑Ni3‑N493.1915C34‑C35‑H35C109.5O7‑Ni4‑N1387.6814O16‑Ni3‑N487.3013H35A‑C35‑H35C109.5O11‑Ni4‑N1391.7915C58‑C57‑H57A111.9H35B‑C35‑H35C109.5O10‑Ni4‑O7177.1612N19‑C57‑H57B111.9O11‑C36‑C29128.65O10‑Ni4‑O1188.3814C58‑C57‑H57B111.9O11‑C36‑H36115.7N13‑Ni1‑N4171.8516H57A‑C57‑H57B109.6C29‑C36‑H36115.7N1‑Ni1‑N494.1915C57‑C58‑H58A109.5O13‑C37‑C42119.84N16‑Ni1‑N479.9114C57‑C58‑H58B109.5O13‑C37‑C38123.85N13‑Ni1‑N1095.2614H58A‑C58‑H58B109.4C42‑C37‑C38116.45N1‑Ni1‑N1079.3015C57‑C58‑H58C109.5C45‑C38‑C39118.05Ni1‑N1‑Na397.7415O14‑Ni3‑N493.0614C45‑C38‑C37122.95N13‑Ni1‑N191.3815O17‑Ni3‑N4173.4415

百度查询： 桂林理工大学 磁性材料HN(C₂H₅)₃·[Ni₄Na₃(heb)₆(N₃)₆]及合成方法