CN106478738B - 铜-铁异核含能配合物的合成方法和催化性能 - Google Patents
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 24
- IYRDVAUFQZOLSB-UHFFFAOYSA-N copper iron Chemical compound [Fe].[Cu] IYRDVAUFQZOLSB-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 230000003197 catalytic effect Effects 0.000 title abstract description 11
- 238000010189 synthetic method Methods 0.000 title description 3
- JUNAPQMUUHSYOV-UHFFFAOYSA-N 2-(2h-tetrazol-5-yl)acetic acid Chemical compound OC(=O)CC=1N=NNN=1 JUNAPQMUUHSYOV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 238000002485 combustion reaction Methods 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 150000003536 tetrazoles Chemical class 0.000 claims description 2
- 239000003380 propellant Substances 0.000 abstract description 20
- 239000000028 HMX Substances 0.000 abstract description 17
- UZGLIIJVICEWHF-UHFFFAOYSA-N octogen Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 UZGLIIJVICEWHF-UHFFFAOYSA-N 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 9
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 8
- DVARTQFDIMZBAA-UHFFFAOYSA-O ammonium nitrate Chemical class [NH4+].[O-][N+]([O-])=O DVARTQFDIMZBAA-UHFFFAOYSA-O 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 229910002651 NO3 Inorganic materials 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract 1
- 229910017827 Cu—Fe Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 6
- 239000003446 ligand Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- -1 iron ion Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000004449 solid propellant Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical group [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- QWUACBDFMJRBGT-UHFFFAOYSA-N N1N=NC(=C1)C(=O)O.[N] Chemical class N1N=NC(=C1)C(=O)O.[N] QWUACBDFMJRBGT-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 150000004905 tetrazines Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/02—Iron compounds
- C07F15/025—Iron compounds without a metal-carbon linkage
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/2243—At least one oxygen and one nitrogen atom present as complexing atoms in an at least bidentate or bridging ligand
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/10—Complexes comprising metals of Group I (IA or IB) as the central metal
- B01J2531/16—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/842—Iron
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
本发明涉及铜‑铁异核含能配合物的制备与应用领域。用温和的水溶液法制备了铜‑铁异核四氮唑乙酸含能配合物，该配合物的组成为：Cu(II)Fe(III)3(tza)6(OH)3H2O·(H2O)6(NO3)2.配合物属于六方晶系，空间群为P63/m(176)。该配合物具有绿色，钝感且高能的特点，对硝铵类推进剂中主要成分奥克托金(HMX)具有明显的催化热分解作用，可望成为硝铵类推进剂中的潜在的含能燃烧催化剂。本发明制备方法简单环保，原料易得。
Description
技术领域
本发明涉及铜-铁异核含能配合物的制备与应用领域，具体来讲，是指铜、铁离子与四氮唑乙酸形成的铜-铁异核配合物的制备及其应用。
背景技术
推进剂燃烧性能的调节是推进剂应用研究的核心技术之一。燃速压强指数是衡量推进剂燃烧稳定性好坏的重要指标之一，一般要求推进剂具有燃速调节范围宽和压强指数低的燃烧特性。目前，研究人员一般采用添加燃烧催化剂来调节燃速及降低压强指数，其用量少，且效果显著，是固体推进剂中重要的功能材料。由于固体推进剂配方的多样性、成分的复杂性及催化剂的选择性，使得不同的推进剂需要不同的燃烧催化剂。含能的燃烧催化剂由于本身含能，且在推进剂燃烧过程中能原位产生新鲜的微纳米催化剂，所以一方面能避免惰性催化剂使推进剂能量降低的缺点，另一方面可大大提高催化剂的催化性能。为此，含能燃烧催化剂的研究己在国内外受到普遍重视。由于多核的含能配合物可在原位产生多种类微、纳米催化剂，为此，可对推进剂中的不同组分分别起到催化或协同催化作用，因此，相比于单核催化剂，异核催化剂会有较好的催化性能。为此，合成异核的含能燃烧催化剂成为该领域的研究方向之一。
已有研究表明：氧化铜和氧化铁可分别作为推进剂中的燃烧催化剂，所以其形成的异核含能配合物预期会提高推进剂的的燃烧性能。
四唑类化合物由于具有配位能力优良、配位模式多样，结构中含有大量生成焓较高的N＝N、C-N键，具有较高的能量，且燃烧产物大多为N2，不会造成污染。其中四氮唑乙酸含有羧基，可提高推进剂的氧平衡，是一类可合成多种新颖拓扑结构含能配体，因此，本发明用四氮唑乙酸与金属离子铜、铁在室温条件下，水溶液中方便地合成了铜-铁异核含能配合物，该合成方法具有反应过程温和，且易于工业化的特点，预计可作为推进剂中的潜在的含能燃烧催化剂。
发明内容
本发明的目的是提供一种铜-铁异核四氮唑乙酸含能配合物的合成方法及其催化作用。
本发明实现过程如下：
取0.1mmol/mL的Cu(NO3)2 6.00-12.00mL加入到10.00-12.00mL的0.1mmol/mL的Htza(用NaOH调pH＝9)溶液中，搅拌均匀，再向混合溶液中加入6.00-12.00mL 0.1mmol/mL的Fe(NO3)3溶液，混合均匀，溶液为深棕色，静止5天，有深棕色八面体晶体析出。
以上所述例子，仅是氮杂环羧酸类配体中的四氮唑乙酸与硝酸铜，硝酸铁合成铜-铁异核四氮唑乙酸配合物的一个实例，本发明还应包括其它氮杂环羧酸类的类似配体如三氮唑羧酸类，四嗪类及其它四唑羧酸类配体，加入的金属离子应包括相应的硫酸盐，醋酸盐及碳酸盐等，且制备产物的各个反应物浓度范围可分别可增大和减少十倍，配体与各金属离子之比为12∶1-1∶12。
本发明还提供了铜-铁异核四氮唑乙酸含能配合物对高能硝胺类推进剂中主要组分奥克托金(HMX)热分解的催化作用。将合成的含能配合物与HMX按质量比1∶3机械混合，进行热重和差示扫描量热测试，研究配合物的热稳定性及对HMX催化热分解作用，探讨其作为燃烧催化剂的可行性。结果表明：所合成的铜-铁异核四氮唑乙酸含能配合物对HMX有明显的催化作用，可成为硝铵类推进剂中潜在的燃烧催化剂。
本发明具有以下的优点及效果：
本发明可在常温下，利用温和的水溶液法，合成了含能的铜-铁异核四氮唑乙酸配合物。本发明避免使用了挥发或有毒的有机溶剂，是一种绿色的合成铜-铁异核四氮唑(或Cu-Fe异核四氮唑乙酸含能配合物)乙酸含能配合物的方法。此配合物对高能硝胺类推进剂中的主要成分HMX有明显的催化热分解作用，是高能硝胺类推进剂中潜在的燃烧催化剂。
附图说明
图1 铜-铁异核四氮唑乙酸含能配合物的配位环境图
图2 铜-铁异核四氮唑乙酸含能配合物的三维网状图
图3 铜-铁异核四氮唑乙酸含能配合物的DSC-TG曲线
图4 铜-铁异核四氮唑乙酸含能配合物对HMX的催化热分解的DSC曲线
具体实施方式
本发明是通过以下实施例实现的，但实施中所述条件和结果对发明的内容和权利不构成限制。
典型制备方法：
取0.1mmol/mL的Cu(NO3)2 6.00mL加入到12.00mL的0.1mmol/mL的Htza(用NaOH调PH＝9)溶液中，搅拌均匀，再向混合溶液中加入6.00mL 0.1mmol/mL的Fe(NO3)3溶液，混合均匀，溶液为深棕色，静止5天，有深棕色八面体晶体析出。
结构表征：
单晶结构分析知其为Cu-Fe异核四氮唑乙酸含能配合物，元素及单晶结构分析知其化学式为：Cu(II)Fe(III)3(tza)6(OH)3H2O·(H2O)6(NO3)2.，其晶体结构图见图1。结果表明：配合物属于六方晶系，P 63/m(176)空间群。其不对称单元包括一个Cu(II)原子，三个Fe(III)原子，一个tza-配体，一个配位水，一个OH-，三个晶格水和一个NO3 -。形成如图2的三维网状结构图。
Cu-Fe异核四氮唑乙酸配合物DSC-TG的热分解图
图3是铜-铁异核四氮唑乙酸含能配合物的DSC-TG的热分解图，氮气气氛，升温速率10℃/min，从它的热重曲线可以看出，其热分解分为两个阶段。从40.6到104.4℃为第一阶段，从质量损失来看可以判断为失去晶格水和配位水，实验值为7.53％，理论值为7.56％。在第二阶段，从188-328℃温度区间有一个较强的质量损失过程，可以推断配合物在此温度区间发生了剧烈的分解反应，配合物框架结构垮塌，分解为一些固体小分子和气体产物并放出大量的热。该配合物的分解过程对应在DSC曲线上表现为一个放热峰，相应峰顶温度241℃。配合物热分解最终剩余残渣质量约为25.1％，与形成Fe2O3与CuO的混合物残渣的理论值24.6％基本相当，可以认为分解最终产物为Fe2O3与CuO的混合物。配合物的分解放热量1041J·g-1。由于配合物的分解温度较高而且热分解时能够释放较多的能量，因此配合物为热稳定性较好的含能配合物。
Cu-Fe异核四氮唑乙酸配合物撞击感度测试
感度测试严格按照GJB772A-97方法601.1标准测试，本实验所用仪器为WL-1型立式落锤仪，采用特性落高(50％爆炸概率时的落高)法表征配合物的撞击感度。实验条件：锤重(10.000士0.010)kg，标准撞击装置，试样量测试药量为(30士1)mg，环境温度为290K。配合物在此条件下的特性落高H50为27.4cm。常用的含能材料黑索今(RDX)和奥克托金(HMX)的特性落高H50分别为15.26cm和11.38cm，所合成的Cu-Fe异核四氮唑乙酸配合物与它们相比，显然可看出所合成的配合物是一个较为钝感的含能配合物。
Cu-Fe异核四氮唑乙酸配合物对HMX的催化热分解
将Cu-Fe异核四氮唑乙酸配合物与HMX以1∶3的质量比研麿混合，所做的DSC曲线见图4，可以看出：HMX的放热峰温度由282.6℃提前到279.7℃，总放热量为1255.2Jg-1，比HMX增加了209.7Jg-1，表明含能配合物能有效催化硝铵类推进剂中的主要成分奥克托金(HMX)，这种特性使其有可能成为硝铵类推进剂中潜在的燃速催化剂。
Claims (3)
1.一种铜-铁异核四氮唑乙酸的含能配合物，其特征在于：其化学式为Cu(II)Fe(III)3(tza)6(OH)3H2O·(H2O)6(NO3)2。
2.根据权利要求1所述的含能配合物的制备方法，包括以下步骤：
取0.1mmol/mL的Cu(NO3)26.00-12.00mL加入到10.00-12.00mL的0.1mmol/mL的四氮唑乙酸溶液中，这里四氮唑乙酸溶液用NaOH溶液调节pH＝9，搅拌均匀后，再向混合溶液中加入6.00-12.00mL0.1mmol/mL的Fe(NO3)3溶液，混合均匀，溶液为深棕色，静止5天，有深棕色八面体晶体析出。
3.权利要求1所述配合物作为燃烧催化剂的用途。
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