发明名称 荧光材料[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]及合成方法
摘要 本发明公开了一种荧光材料[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]及合成方法。荧光材料[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]的分子式为:C<sub>21</sub>H<sub>22</sub>CuN<sub>3</sub>NaO<sub>7</sub>,分子量为:514.96,Hehbd为3-乙氧基水杨醛,dca为双氰胺根。(1)取0.125g-0.250g分析纯的3-乙氧基水杨醛,0.134-0.268g分析纯的双氰胺钠和0.278-0.556g分析纯的六水合高氯酸铜混合,溶于10-20ml分析纯甲醇溶液中,搅拌,调节pH为7.0,搅拌,静置。[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]在280nm的入射光照射下产生3952a.u.强度的309nm的荧光。本发明工艺简单、成本低廉、化学组分易于控制、重复性好且产量高。
申请公布号 CN104194772B 申请公布日期 2016.05.18
申请号 CN201410418048.4 申请日期 2014.08.25
申请人 桂林理工大学 发明人 张淑华;赵儒霞;周玉洁;张海洋
分类号 C09K11/06(2006.01)I;C07F1/08(2006.01)I 主分类号 C09K11/06(2006.01)I
代理机构 代理人
主权项 一种荧光材料[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)],其特征在于[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]的分子式为:C<sub>21</sub>H<sub>22</sub>CuN<sub>3</sub>NaO<sub>7</sub>,分子量为:514.96,Hehbd为3‑乙氧基水杨醛,dca为双氰胺根,晶体结构数据见表一,键长键角数据见表二;[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]在280nm的入射光照射下产生3952a.u.强度的309nm的荧光;所述[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]的合成方法具体步骤为:将0.125g‑0.250g分析纯的3‑乙氧基水杨醛、0.134‑0.268g分析纯的双氰胺钠和0.278‑0.556g分析纯的六水合高氯酸铜混合,溶于10‑20mL分析纯甲醇溶液中,搅拌10分钟后加入分析纯三乙胺调节pH为7.0,继续搅拌20分钟后,将得到的溶液于室温下静置3天后,得到黑色的块状晶体即[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)];表一:[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]的晶体学参数<img file="FDA0000868375040000011.GIF" wi="1206" he="1502" />表二:[CuNa(ehbd)<sub>2</sub>(dca)(CH<sub>3</sub>OH)]的键长<img file="FDA0000868375040000012.GIF" wi="38" he="55" />和键角°<tables num="0001" wi="165"><table><tgroup cols="4"><colspec colname="c001" colwidth="25%" /><colspec colname="c002" colwidth="24%" /><colspec colname="c003" colwidth="25%" /><colspec colname="c004" colwidth="24%" /><tbody><row><entry morerows="1">Cu1‑O4</entry><entry morerows="1">1.8996(18)</entry><entry morerows="1">C1‑C2</entry><entry morerows="1">1.417(4)</entry></row><row><entry morerows="1">Cu1‑O1</entry><entry morerows="1">1.9006(17)</entry><entry morerows="1">C10‑C15</entry><entry morerows="1">1.418(4)</entry></row><row><entry morerows="1">Cu1‑O2</entry><entry morerows="1">1.927(2)</entry><entry morerows="1">C10‑C11</entry><entry morerows="1">1.421(4)</entry></row><row><entry morerows="1">Cu1‑O5</entry><entry morerows="1">1.9458(18)</entry><entry morerows="1">C6‑C5</entry><entry morerows="1">1.368(4)</entry></row><row><entry morerows="1">Na1‑O4</entry><entry morerows="1">2.3764(19)</entry><entry morerows="1">C15‑C14</entry><entry morerows="1">1.374(4)</entry></row><row><entry morerows="1">Na1‑O1</entry><entry morerows="1">2.361(2)</entry><entry morerows="1">C3‑C2</entry><entry morerows="1">1.420(4)</entry></row><row><entry morerows="1">Na1‑O3</entry><entry morerows="1">2.695(2)</entry><entry morerows="1">C3‑C4</entry><entry morerows="1">1.349(5)</entry></row><row><entry morerows="1">Na1‑O6</entry><entry morerows="1">2.707(2)</entry><entry morerows="1">C2‑C9</entry><entry morerows="1">1.426(4)</entry></row><row><entry morerows="1">Na1‑O7</entry><entry morerows="1">2.347(3)</entry><entry morerows="1">C4‑C5</entry><entry morerows="1">1.396(5)</entry></row><row><entry morerows="1">Na1‑N1</entry><entry morerows="1">2.451(3)</entry><entry morerows="1">C11‑C12</entry><entry morerows="1">1.417(4)</entry></row></tbody></tgroup></table></tables><tables num="0002" wi="165"><table><tgroup cols="4"><colspec colname="c001" colwidth="25%" /><colspec colname="c002" colwidth="24%" /><colspec colname="c003" colwidth="25%" /><colspec colname="c004" colwidth="24%" /><tbody><row><entry morerows="1">O4‑C10</entry><entry morerows="1">1.306(3)</entry><entry morerows="1">C11‑C18</entry><entry morerows="1">1.405(4)</entry></row><row><entry morerows="1">O1‑C1</entry><entry morerows="1">1.302(3)</entry><entry morerows="1">N2‑C20</entry><entry morerows="1">1.273(5)</entry></row><row><entry morerows="1">O2‑C9</entry><entry morerows="1">1.239(3)</entry><entry morerows="1">N2‑C19</entry><entry morerows="1">1.279(5)</entry></row><row><entry morerows="1">O5‑C18</entry><entry morerows="1">1.244(4)</entry><entry morerows="1">C14‑C13</entry><entry morerows="1">1.401(4)</entry></row><row><entry morerows="1">O3‑C6</entry><entry morerows="1">1.369(3)</entry><entry morerows="1">C12‑C13</entry><entry morerows="1">1.343(5)</entry></row><row><entry morerows="1">O3‑C7</entry><entry morerows="1">1.432(3)</entry><entry morerows="1">N3‑C20</entry><entry morerows="1">1.131(4)</entry></row><row><entry morerows="1">O6‑C15</entry><entry morerows="1">1.377(3)</entry><entry morerows="1">C7‑C8</entry><entry morerows="1">1.485(5)</entry></row><row><entry morerows="1">O6‑C16</entry><entry morerows="1">1.438(4)</entry><entry morerows="1">C16‑C17</entry><entry morerows="1">1.480(5)</entry></row><row><entry morerows="1">O7‑C21</entry><entry morerows="1">1.429(4)</entry><entry morerows="1">N1‑C19</entry><entry morerows="1">1.126(4)</entry></row><row><entry morerows="1">C1‑C6</entry><entry morerows="1">1.427(4)</entry><entry morerows="1"> </entry><entry morerows="1"> </entry></row><row><entry morerows="1">O4‑Cu1‑O1</entry><entry morerows="1">86.23(8)</entry><entry morerows="1">C6‑O3‑C7</entry><entry morerows="1">118.0(2)</entry></row><row><entry morerows="1">O4‑Cu1‑O2</entry><entry morerows="1">172.16(8)</entry><entry morerows="1">C7‑O3‑Na1</entry><entry morerows="1">125.18(19)</entry></row><row><entry morerows="1">O4‑Cu1‑O5</entry><entry morerows="1">93.92(8)</entry><entry morerows="1">C15‑O6‑Na1</entry><entry morerows="1">116.43(16)</entry></row><row><entry morerows="1">C6‑O3‑Na1</entry><entry morerows="1">116.60(15)</entry><entry morerows="1">C15‑O6‑C16</entry><entry morerows="1">116.5(2)</entry></row><row><entry morerows="1">O1‑Cu1‑O2</entry><entry morerows="1">94.03(8)</entry><entry morerows="1">C16‑O6‑Na1</entry><entry morerows="1">127.07(17)</entry></row><row><entry morerows="1">O1‑Cu1‑O5</entry><entry morerows="1">176.13(9)</entry><entry morerows="1">C21‑O7‑Na1</entry><entry morerows="1">116.9(2)</entry></row><row><entry morerows="1">C18‑O5‑Cu1</entry><entry morerows="1">124.20(19)</entry><entry morerows="1">O1‑C1‑C6</entry><entry morerows="1">117.8(2)</entry></row><row><entry morerows="1">O2‑Cu1‑O5</entry><entry morerows="1">85.30(8)</entry><entry morerows="1">O1‑C1‑C2</entry><entry morerows="1">124.8(2)</entry></row><row><entry morerows="1">C1‑O1‑Na1</entry><entry morerows="1">129.69(16)</entry><entry morerows="1">C2‑C1‑C6</entry><entry morerows="1">117.4(3)</entry></row><row><entry morerows="1">C9‑O2‑Cu1</entry><entry morerows="1">125.50(19)</entry><entry morerows="1">O4‑C10‑C15</entry><entry morerows="1">118.6(2)</entry></row><row><entry morerows="1">O4‑Na1‑O3</entry><entry morerows="1">127.60(8)</entry><entry morerows="1">O4‑C10‑C11</entry><entry morerows="1">124.0(2)</entry></row><row><entry morerows="1">O4‑Na1‑O6</entry><entry morerows="1">61.33(6)</entry><entry morerows="1">C15‑C10‑C11</entry><entry morerows="1">117.4(2)</entry></row><row><entry morerows="1">O4‑Na1‑N1</entry><entry morerows="1">121.76(9)</entry><entry morerows="1">O3‑C6‑C1</entry><entry morerows="1">113.8(2)</entry></row><row><entry morerows="1">C1‑O1‑Cu1</entry><entry morerows="1">126.16(17)</entry><entry morerows="1">C5‑C6‑O3</entry><entry morerows="1">125.6(3)</entry></row><row><entry morerows="1">O1‑Na1‑O4</entry><entry morerows="1">66.49(7)</entry><entry morerows="1">C5‑C6‑C1</entry><entry morerows="1">120.5(3)</entry></row><row><entry morerows="1">O1‑Na1‑O3</entry><entry morerows="1">61.21(6)</entry><entry morerows="1">O6‑C15‑C10</entry><entry morerows="1">114.1(2)</entry></row><row><entry morerows="1">O1‑Na1‑O6</entry><entry morerows="1">127.70(7)</entry><entry morerows="1">C14‑C15‑O6</entry><entry morerows="1">124.7(3)</entry></row><row><entry morerows="1">O1‑Na1‑N1</entry><entry morerows="1">115.75(10)</entry><entry morerows="1">C14‑C15‑C10</entry><entry morerows="1">121.2(3)</entry></row><row><entry morerows="1">O5‑C18‑C11</entry><entry morerows="1">128.6(3)</entry><entry morerows="1">C4‑C3‑C2</entry><entry morerows="1">120.9(3)</entry></row><row><entry morerows="1">O3‑Na1‑O6</entry><entry morerows="1">171.08(7)</entry><entry morerows="1">C1‑C2‑C3</entry><entry morerows="1">119.9(3)</entry></row><row><entry morerows="1">C12‑C13‑C14</entry><entry morerows="1">120.5(3)</entry><entry morerows="1">C1‑C2‑C9</entry><entry morerows="1">122.0(3)</entry></row><row><entry morerows="1">C19‑N1‑Na1</entry><entry morerows="1">158.4(3)</entry><entry morerows="1">C3‑C2‑C9</entry><entry morerows="1">118.0(3)</entry></row><row><entry morerows="1">O7‑Na1‑O4</entry><entry morerows="1">100.48(8)</entry><entry morerows="1">C3‑C4—C5</entry><entry morerows="1">119.9(3)</entry></row><row><entry morerows="1">O7‑Na1‑O1</entry><entry morerows="1">109.42(10)</entry><entry morerows="1">C12‑C11‑C10</entry><entry morerows="1">119.6(3)</entry></row><row><entry morerows="1">O7‑Na1‑O3</entry><entry morerows="1">93.80(9)</entry><entry morerows="1">C18‑C11‑C10</entry><entry morerows="1">122.5(2)</entry></row><row><entry morerows="1">O7‑Na1‑O6</entry><entry morerows="1">83.73(9)</entry><entry morerows="1">C18‑C11‑C12</entry><entry morerows="1">118.0(3)</entry></row><row><entry morerows="1">O7‑Na1‑N1</entry><entry morerows="1">126.98(10)</entry><entry morerows="1">C20‑N2‑C19</entry><entry morerows="1">127.6(4)</entry></row><row><entry morerows="1">N1‑C19‑N2</entry><entry morerows="1">172.1(4)</entry><entry morerows="1">O2‑C9‑C2</entry><entry morerows="1">127.4(3)</entry></row><row><entry morerows="1">N1‑Na1‑O3</entry><entry morerows="1">85.01(9)</entry><entry morerows="1">C6‑C5‑C4</entry><entry morerows="1">121.4(3)</entry></row><row><entry morerows="1">N1‑Na1‑O6</entry><entry morerows="1">89.63(9)</entry><entry morerows="1">C15‑C14‑C13</entry><entry morerows="1">120.2(3)</entry></row><row><entry morerows="1">Cu1‑O4‑Na1</entry><entry morerows="1">103.38(8)</entry><entry morerows="1">C13‑C12‑C11</entry><entry morerows="1">121.1(3)</entry></row><row><entry morerows="1">C10‑O4‑Cu1</entry><entry morerows="1">126.62(16)</entry><entry morerows="1">N3‑C20‑N2</entry><entry morerows="1">171.6(4)</entry></row><row><entry morerows="1">C10‑O4‑Na1</entry><entry morerows="1">129.23(16)</entry><entry morerows="1">O3‑C7‑C8</entry><entry morerows="1">108.3(3)</entry></row><row><entry morerows="1">Cu1‑O1‑Na1</entry><entry morerows="1">103.90(8)</entry><entry morerows="1">O6‑C16‑C17</entry><entry morerows="1">107.9(3)</entry></row></tbody></tgroup></table></tables>                                                                     。
地址 541004 广西壮族自治区桂林市建干路12号