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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：CN104036910A

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·[Co4Na3heb6N36]及合成方法。磁性材料HNC2H53·[Co4Na3heb6N36]的分子式为：C60H71N19Na3Co4O18分子量为：1651.05。将0.166克分析纯的3-乙氧基-2-羟基苯甲醛溶于4-8毫升分析纯甲醇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钴和0.065-0.13g分析纯叠氮化钠，并搅拌10分钟后加入分析纯三乙胺调节至pH=5.5，搅拌20分钟后，静置于室温下，过滤，用分析纯甲醇洗涤。HNC2H53·[Co4Na3heb6N36]的磁学性质：分子内钴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、重复性好并产量高等优点。

专利权项：一种磁性材料HNC2H53·[Co4Na3heb6N36]，其特征在于HNC2H53·[Co4Na3heb6N36]具有优良的磁学特性，其分子式为：C60H71N19Na3Co4O18，分子量为：1651.05，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·[Co4Na3heb6N36]的磁学性质：1分子内钴离子间存在铁磁交换，其整体表现为铁磁性；2HNC2H53·[Co4Na3heb6N36]在室温下χMT为12.53cm3Kmol‑1，随着温度降低，χMT逐渐升高，至14K达到最大值20.08cm3Kmol‑1，随后急剧降至2K时的8.38cm3Kmol‑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5.00K，居里常数为12.56cm3Kmol–1；大而正的韦斯常数及χMT‑T曲线趋势均暗示分子内钴离子间存在铁磁交换，其整体表现为铁磁性；所述HNC2H53·[Co4Na3heb6N36]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钴和0.065‑0.13g分析纯叠氮化钠，并搅拌10分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分钟后得到红色条状晶体，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·[Co4Na3heb6N36]；表一HNC2H53·[Co4Na3heb6N36]·CH3OH的晶体学参数表二HNC2H53·[Co4Na3heb6N36]·CH3OH的键长和键角°C1‑O11.2867C46‑C471.4128C36‑H360.9300C1‑C21.4109C46‑C511.4248C37‑O131.2937C1‑C61.4179C47‑C541.4279C37‑C381.4048C2‑C31.40110C47‑C481.4319C37‑C421.4378C2‑C91.43110C48‑C491.35110C38‑C451.4149C3‑C41.34912C48‑H480.9300C38‑C391.4169C3‑H30.9300C49‑C501.37010C39‑C401.35311C4‑C51.39911C49‑H490.9300C39‑H390.9300C4‑H40.9300C50‑C511.3888C40‑C411.37510C5‑C61.3639C50‑H500.9300C40‑H400.9300C5‑H50.9300C51‑O181.3637Na2‑O122.4545C6‑O31.3877C52‑O181.4277C30‑C311.37311C7‑O31.4458C52‑C531.49010C57‑H57B0.9700C7‑C81.46211C52‑H52A0.9700C14‑C151.37610C7‑H7A0.9700C52‑H52B0.9700Na3‑O72.2474C7‑H7B0.9700C53‑H53A0.9600Na3‑O42.2664C8‑H8A0.9600C53‑H53B0.9600Na3‑O92.3905C8‑H8B0.9600C53‑H53C0.9600Na3‑O62.4586C8‑H8C0.9600C54‑O171.2318C45‑H450.9300C9‑O21.2229C54‑H540.9300C46‑O161.2856C9‑H90.9300C55‑C561.402C41‑C421.3719C10‑O41.2917C55‑H55A0.9600C41‑H410.9300C10‑C111.4089C55‑H55B0.9600C42‑O151.3817C10‑C151.4179C55‑H55C0.9600C43‑O151.4247C11‑C181.42911C56‑N191.44618C43‑C441.49710C11‑C121.43811C56‑H56A0.9700C43‑H43A0.9700C12‑C131.32813C56‑H56B0.9700C43‑H43B0.9700C12‑H120.9300C57‑N191.48910C44‑H44A0.9600C13‑C141.39113C57‑C581.56310C44‑H44B0.9600C13‑H130.9300C57‑H57A0.9700C44‑H44C0.9600C14‑H140.9300C58‑H58A0.9600Co2‑O12.0254C15‑O61.3458C58‑H58B0.9600Co2‑O42.0434C16‑C171.35214C58‑H58C0.9600Co2‑O22.0974C16‑O61.44811C59‑C601.36717Co2‑O52.1065C16‑H16A0.9700C59‑N191.41016Co3‑O132.0214C16‑H16B0.9700C59‑H59A0.9700Co3‑O162.0254C17‑H17A0.9600C59‑H59B0.9700Co3‑O142.0784C17‑H17B0.9600C60‑H60A0.9600Co3‑O172.1144C17‑H17C0.9600C60‑H60B0.9600Co4‑O102.0294C18‑O51.2099C60‑H60C0.9600C45‑O141.2428C18‑H180.9300N1‑N21.1797Co4‑O72.0404C19‑O71.2817N1‑Co22.1434Co4‑O112.0814C19‑C201.4129N1‑Co12.1584Co4‑O82.0994C19‑C241.4249N1‑Na32.5485Na2‑O132.2604C30‑H300.9300N2‑N31.1438Na2‑O102.2754C20‑C211.4139C32‑C331.3509Na2‑O152.4275C20‑C271.41210N4‑N51.1706C31‑C321.38611C21‑C221.34712N4‑Co12.1654N16‑N171.1966C21‑H210.9300N4‑Co32.1864N16‑Co32.1554C22‑C231.37512N4‑Na12.5244N16‑Co12.1784C22‑H220.9300N5‑N61.1448N16‑Na22.5254C23‑C241.3899C36‑O111.2338N17‑N181.1327C23‑H230.9300N7‑N81.1826N19‑H19A0.9137C24‑O91.3668N7‑Co42.1584Na1‑O162.2674C25‑O91.4319N7‑Co12.1754Na1‑O12.2774C25‑C261.45212N7‑Na22.4985Na1‑O182.4024C25‑H25A0.9700N8‑N91.1378Na1‑O32.4665C25‑H25B0.9700N10‑N111.1956C32‑H32A0.9700C26‑H26A0.9600N10‑Co22.1454C32‑H32B0.9700C26‑H26B0.9600N10‑Co12.1664C33‑O121.3907C26‑H26C0.9600N10‑Na12.5395C34‑O121.4247C27‑O81.2498N11‑N121.1417C34‑C351.50611C27‑H270.9300N13‑N141.1806C34‑H34A0.9700C28‑O101.2947N13‑Co12.1424C34‑H34B0.9700C28‑C291.4198N13‑Co42.1754C35‑H35A0.9600C28‑C331.4228N13‑Na32.5405C35‑H35B0.9600C29‑C301.4209N14‑N151.1417C35‑H35C0.9600C29‑C361.4219C31‑H310.9300  O1‑C1‑C2123.76O18‑Na1‑N4140.5916H60A‑C60‑H60C109.5O1‑C1‑C6120.45O3‑Na1‑N499.4116H60B‑C60‑H60C109.5C2‑C1‑C6115.96O16‑Na1‑N1091.8815N2‑N1‑Co2123.64C3‑C2‑C1120.97O1‑Na1‑N1074.2915N2‑N1‑Co1131.24C3‑C2‑C9117.17O18‑Na1‑N1097.3116Co2‑N1‑Co199.2717C1‑C2‑C9122.07O3‑Na1‑N10140.5416N2‑N1‑Na3102.74C4‑C3‑C2121.38N4‑Na1‑N1075.0314Co2‑N1‑Na392.0517C4‑C3‑H3119.3O14‑C45‑C38128.86Co1‑N1‑Na397.2617C2‑C3‑H3119.3O18‑C52‑H52B109.9N3‑N2‑N1176.38C3‑C4‑C5119.28O18‑C52‑H52A109.9O10‑Co4‑N787.9015C3‑C4‑H4120.4C53‑C52‑H52A109.9O7‑Co4‑N795.5916C5‑C4‑H4120.4C40‑C39‑H39119.5O11‑Co4‑N7169.5617C6‑C5‑C4120.68C38‑C39‑H39119.5O8‑Co4‑N794.8517C6‑C5‑H5119.7O10‑Co4‑O1186.8616O10‑Co4‑N1394.3716C4‑C5‑H5119.7O7‑Co4‑O1189.8817O7‑Co4‑N1387.3915C5‑C6‑O3124.77O10‑Co4‑O892.5117O11‑Co4‑N1390.7117C5‑C6‑C1122.07O7‑Co4‑O886.0216O8‑Co4‑N13171.6518O3‑C6‑C1113.36O11‑Co4‑O894.3918N7‑Co4‑N1380.7015O3‑C7‑C8108.87N19‑C59‑H59B105.8O10‑Co4‑O7176.3115O3‑C7‑H7A109.9H59A‑C59‑H59B106.2O15‑C43‑H43A110.2C8‑C7‑H7A109.9C59‑C60‑H60A109.5C43‑C44‑H44A109.5O3‑C7‑H7B109.9C59‑C60‑H60B109.5N5‑N4‑Co1130.64C8‑C7‑H7B109.9H60A‑C60‑H60B109.5N5‑N4‑Co3123.04H7A‑C7‑H7B108.3C57‑C58‑H58A109.5Co1‑N4‑Co398.6016C7‑C8‑H8A109.5C57‑C58‑H58B109.5N5‑N4‑Na1105.04C7‑C8‑H8B109.5H58A‑C58‑H58B109.5Co1‑N4‑Na197.3316H8A‑C8‑H8B109.5C57‑C58‑H58C109.5Co3‑N4‑Na193.0714C7‑C8‑H8C109.5H58A‑C58‑H58C109.5N6‑N5‑N4176.37H8A‑C8‑H8C109.5H58B‑C58‑H58C109.5O15‑C42‑C37113.45H8B‑C8‑H8C109.5C60‑C59‑N19125.916O14‑Co3‑O1792.1218O2‑C9‑C2130.67C60‑C59‑H59A105.8O13‑Co3‑N1687.0415O2‑C9‑H9114.7N19‑C59‑H59A105.8O16‑Co3‑N1694.3916C2‑C9‑H9114.7C60‑C59‑H59B105.8O14‑Co3‑N16171.2816O4‑C10‑C11123.16C58‑C57‑H57A107.1O17‑Co3‑N1694.7017O4‑C10‑C15118.56N19‑C57‑H57B107.1O13‑Co3‑N493.7916C11‑C10‑C15118.46C58‑C57‑H57B107.1O16‑Co3‑N486.8015C10‑C11‑C18122.57H57A‑C57‑H57B106.8O14‑Co3‑N492.7317C10‑C11‑C12118.78O13‑Na2‑O10165.5617O17‑Co3‑N4171.8017C18‑C11‑C12118.87O13‑Na2‑O1567.3214N16‑Co3‑N481.1515C13‑C12‑C11121.79O10‑Na2‑O15123.9116O15‑C43‑C44107.46C13‑C12‑H12119.2O13‑Na2‑O12120.0816N8‑N7‑Co4124.74C11‑C12‑H12119.2O10‑Na2‑O1267.3114N8‑N7‑Co1126.94C12‑C13‑C14119.69O15‑Na2‑O12108.6917Co4‑N7‑Co198.8817C12‑C13‑H13120.2O13‑Na2‑N794.6716N8‑N7‑Na2109.14C14‑C13‑H13120.2O10‑Na2‑N774.8815Co4‑N7‑Na293.2516C15‑C14‑C13121.89O15‑Na2‑N7101.3816Co1‑N7‑Na295.4815C15‑C14‑H14119.1O12‑Na2‑N7140.5216N9‑N8‑N7179.19C13‑C14‑H14119.1O13‑Na2‑N1673.6915N11‑N10‑Co2122.74O6‑C15‑C14125.38O10‑Na2‑N1694.0315N11‑N10‑Co1131.24O6‑C15‑C10114.96O15‑Na2‑N16140.8016N10‑Co1‑N1694.7316C14‑C15‑C10119.88O12‑Na2‑N1693.9115N7‑Co1‑N1692.4415C17‑C16‑O6112.010N7‑Na2‑N1677.4514C1‑O1‑Co2130.64C17‑C16‑H16A109.2O16‑Co3‑O1491.4516C1‑O1‑Na1122.44O6‑C16‑H16A109.2O13‑Co3‑O1793.0517Co2‑O1‑Na1104.3017C17‑C16‑H16B109.2O16‑Co3‑O1786.4716C9‑O2‑Co2124.95O6‑C16‑H16B109.2O13‑Co3‑O16178.5216C6‑O3‑C7116.86H16A‑C16‑H16B107.9O13‑Co3‑O1487.1815C6‑O3‑Na1115.64C16‑C17‑H17A109.5C55‑C56‑H56B108.9C7‑O3‑Na1125.44C16‑C17‑H17B109.5N19‑C56‑H56B108.9C10‑O4‑Co2130.64H17A‑C17‑H17B109.5H56A‑C56‑H56B107.7C10‑O4‑Na3122.64C16‑C17‑H17C109.5N19‑C57‑C58121.011Co2‑O4‑Na3103.5218H17A‑C17‑H17C109.5N19‑C57‑H57A107.1Co2‑N10‑Co198.9217H17B‑C17‑H17C109.5C56‑C55‑H55C109.5N11‑N10‑Na1104.74O5‑C18‑C11130.07H55A‑C55‑H55C109.5Co2‑N10‑Na192.7016O5‑C18‑H18115.0H55B‑C55‑H55C109.5Co1‑N10‑Na196.8717C11‑C18‑H18115.0C55‑C56‑N19113.416N12‑N11‑N10177.77O7‑C19‑C20124.36C55‑C56‑H56A108.9N14‑N13‑Co1129.94O7‑C19‑C24118.36N19‑C56‑H56A108.9N14‑N13‑Co4124.04C20‑C19‑C24117.46N13‑Co1‑N1094.2616Co1‑N13‑Co499.3617O15‑C43‑H43B110.2N1‑Co1‑N1080.5017N14‑N13‑Na3103.54C44‑C43‑H43B110.2N4‑Co1‑N1090.7616Co1‑N13‑Na397.9217H43A‑C43‑H43B108.5N13‑Co1‑N781.0616Co4‑N13‑Na392.4115C19‑C20‑C21120.77N1‑Co1‑N792.7316N15‑N14‑N13176.07C19‑C20‑C27122.26O7‑Na3‑O4164.9117C18‑O5‑Co2125.75C21‑C20‑C27117.27O7‑Na3‑O968.1216C15‑O6‑C16116.67C22‑C21‑C20120.58O4‑Na3‑O9122.4418C15‑O6‑Na3115.74C22‑C21‑H21119.8O7‑Na3‑O6123.418C16‑O6‑Na3125.85C20‑C21‑H21119.8O4‑Na3‑O666.6517C19‑O7‑Co4131.14C21‑C22‑C23120.17O9‑Na3‑O6105.1819C19‑O7‑Na3122.44C21‑C22‑H22119.9O7‑Na3‑N1374.7214Co4‑O7‑Na3105.4216C23‑C22‑H22119.9O4‑Na3‑N1393.2615C27‑O8‑Co4126.15C22‑C23‑C24122.08O9‑Na3‑N13142.5118C24‑O9‑C25119.46C22‑C23‑H23119.0O6‑Na3‑N1399.0318C24‑O9‑Na3116.04C24‑C23‑H23119.0O7‑Na3‑N192.5816O14‑C45‑H45115.6O9‑C24‑C23126.37O4‑Na3‑N175.0616C38‑C45‑H45115.6O9‑C24‑C19114.45O9‑Na3‑N1102.4518N17‑N16‑Co3121.64C23‑C24‑C19119.37O6‑Na3‑N1140.6917N17‑N16‑Co1127.54O9‑C25‑C26110.07N13‑Na3‑N174.0015Co3‑N16‑Co199.1617O9‑C25‑H25A109.7C42‑C41‑C40120.57N17‑N16‑Na2112.63C26‑C25‑H25A109.7C42‑C41‑H41119.7Co3‑N16‑Na293.4616O9‑C25‑H25B109.7C40‑C41‑H41119.7Co1‑N16‑Na294.6315C26‑C25‑H25B109.7C59‑C60‑H60C109.5N18‑N17‑N16176.57H25A‑C25‑H25B108.2O16‑C46‑C47124.75C59‑N19‑C56111.412C25‑C26‑H26A109.5O16‑C46‑C51118.25C25‑O9‑Na3124.55C25‑C26‑H26B109.5C44‑C43‑H43A110.2C28‑O10‑Co4129.04H26A‑C26‑H26B109.5C53‑C52‑H52B109.9C28‑O10‑Na2121.43C25‑C26‑H26C109.5C41‑C42‑O15125.76Co4‑O10‑Na2103.9217H26A‑C26‑H26C109.5C41‑C42‑C37120.96C36‑O11‑Co4126.44H26B‑C26‑H26C109.5C39‑C40‑C41120.68C33‑O12‑C34117.35O8‑C27‑C20129.66C39‑C40‑H40119.7C33‑O12‑Na2115.33O8‑C27‑H27115.2C41‑C40‑H40119.7C34‑O12‑Na2124.14C20‑C27‑H27115.2N4‑Co1‑N794.3716C37‑O13‑Co3130.04O10‑C28‑C29123.05N10‑Co1‑N7171.7516C37‑O13‑Na2123.93O10‑C28‑C33120.15N13‑Co1‑N1694.9216O1‑Na1‑N493.0115C29‑C28‑C33116.96N1‑Co1‑N16172.8316C59‑N19‑C57121.512C28‑C29‑C30119.76N4‑Co1‑N1681.1015C56‑N19‑C57106.112C28‑C29‑C36123.66O2‑Co2‑O597.2619C59‑N19‑H19A104.8C30‑C29‑C36116.77O1‑Co2‑N195.3117C56‑N19‑H19A114.3C31‑C30‑C29120.58O4‑Co2‑N189.2616C57‑N19‑H19A98.4C31‑C30‑H30119.8O2‑Co2‑N190.6318O16‑Na1‑O1163.3616C29‑C30‑H30119.8O5‑Co2‑N1170.6319O16‑Na1‑O1867.4414C30‑C31‑C32119.88O1‑Co2‑N1088.6616O1‑Na1‑O18122.6217C30‑C31‑H31120.1O4‑Co2‑N1095.1317O16‑Na1‑O3124.7717C32‑C31‑H31120.1O2‑Co2‑N10170.4419O1‑Na1‑O366.9416C33‑C32‑C31121.17O5‑Co2‑N1091.2417Co3‑O13‑Na2105.8017C33‑C32‑H32A107.1N1‑Co2‑N1081.3217C45‑O14‑Co3126.64C31‑C32‑H32A107.1O1‑Co2‑O4174.4716C42‑O15‑C43115.85C33‑C32‑H32B107.1O1‑Co2‑O286.9718C42‑O15‑Na2117.03C31‑C32‑H32B107.1O4‑Co2‑O289.8718C43‑O15‑Na2126.74H32A‑C32‑H32B106.8O1‑Co2‑O590.1719C46‑O16‑Co3130.64C32‑C33‑O12124.76O4‑Co2‑O585.7318C46‑O16‑Na1123.04C32‑C33‑C28122.07O1‑Co2‑O4174.4716Co3‑O16‑Na1105.8015O12‑C33‑C28113.25N13‑Co1‑N190.8017C54‑O17‑Co3126.64O12‑C34‑C35108.47N13‑Co1‑N4173.8416C51‑O18‑C52117.95O12‑C34‑H34A110.0N1‑Co1‑N493.5416C51‑O18‑Na1117.03C35‑C34‑H34A110.0C56‑C55‑H55A109.5C52‑O18‑Na1125.14O12‑C34‑H34B110.0C56‑C55‑H55B109.5O18‑Na1‑O3109.2717C35‑C34‑H34B110.0H55A‑C55‑H55B109.5O16‑Na1‑N474.1514H34A‑C34‑H34B108.4H52A‑C52‑H52B108.3C47‑C46‑C51117.25C34‑C35‑H35A109.5C52‑C53‑H53A109.5C46‑C47‑C54122.66C34‑C35‑H35B109.5C52‑C53‑H53B109.5C46‑C47‑C48120.06H35A‑C35‑H35B109.5H53A‑C53‑H53B109.5C54‑C47‑C48117.46C34‑C35‑H35C109.5C52‑C53‑H53C109.5C49‑C48‑C47120.67H35A‑C35‑H35C109.5H53A‑C53‑H53C109.5C49‑C48‑H48119.7H35B‑C35‑H35C109.5H53B‑C53‑H53C109.5C47‑C48‑H48119.7O11‑C36‑C29128.07O17‑C54‑C47128.56C48‑C49‑C50120.46O11‑C36‑H36116.0O17‑C54‑H54115.8C48‑C49‑H49119.8C29‑C36‑H36116.0C47‑C54‑H54115.8C50‑C49‑H49119.8O13‑C37‑C38124.75C49‑C50‑H50119.3C49‑C50‑C51121.47O13‑C37‑C42118.25C51‑C50‑H50119.3C43‑C44‑H44B109.5C38‑C37‑C42117.16O18‑C51‑C50125.26H44A‑C44‑H44B109.5C37‑C38‑C45122.66O18‑C51‑C46114.35C43‑C44‑H44C109.5C37‑C38‑C39119.66C50‑C51‑C46120.46H44A‑C44‑H44C109.5C45‑C38‑C39117.76O18‑C52‑C53109.06H44B‑C44‑H44C109.5。

百度查询： 桂林理工大学 磁性材料HN(C₂H₅)₃·[Co₄Na₃(heb)₆(N₃)₆]及合成方法