CN103641777A - 柠嗪酸铅锆双金属盐及其制备方法和应用 - Google Patents
柠嗪酸铅锆双金属盐及其制备方法和应用 Download PDFInfo
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- CSGQJHQYWJLPKY-UHFFFAOYSA-N CITRAZINIC ACID Chemical compound OC(=O)C=1C=C(O)NC(=O)C=1 CSGQJHQYWJLPKY-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 150000003839 salts Chemical class 0.000 title claims description 35
- 229910052751 metal Inorganic materials 0.000 title claims description 30
- 239000002184 metal Substances 0.000 title claims description 30
- 238000002360 preparation method Methods 0.000 title claims description 14
- QNZFKUWECYSYPS-UHFFFAOYSA-N lead zirconium Chemical compound [Zr].[Pb] QNZFKUWECYSYPS-UHFFFAOYSA-N 0.000 title abstract 3
- 238000002485 combustion reaction Methods 0.000 claims abstract description 24
- 239000003381 stabilizer Substances 0.000 claims abstract description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 30
- 229910052726 zirconium Inorganic materials 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 239000002585 base Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical group [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 4
- 150000003754 zirconium Chemical class 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 2
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- JEHCHYAKAXDFKV-UHFFFAOYSA-J lead tetraacetate Chemical compound CC(=O)O[Pb](OC(C)=O)(OC(C)=O)OC(C)=O JEHCHYAKAXDFKV-UHFFFAOYSA-J 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 abstract description 2
- 150000002736 metal compounds Chemical class 0.000 abstract 2
- 230000008018 melting Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 description 12
- 239000013078 crystal Substances 0.000 description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000003380 propellant Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229960003711 glyceryl trinitrate Drugs 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000004449 solid propellant Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- CNVULGHYDPMIHD-UHFFFAOYSA-L bis[(2-hydroxybenzoyl)oxy]lead Chemical compound [Pb+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O CNVULGHYDPMIHD-UHFFFAOYSA-L 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- UQLDLKMNUJERMK-UHFFFAOYSA-L di(octadecanoyloxy)lead Chemical compound [Pb+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O UQLDLKMNUJERMK-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D213/79—Acids; Esters
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/14—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of germanium, tin or lead
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- 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
- C06D5/10—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by reaction of solids with liquids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
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Abstract
本发明公开了结构式(I)所示的柠嗪酸铅锆双金属化合物,其作为燃烧催化剂和燃烧稳定剂应用时分解产生均匀的、新生态的铅及其氧化物可作为主要催化活性组分,分解产生的高熔点的二氧化锆作为助催化剂,可进一步提高催化效果。
Description
技术领域
本发明涉及一种柠嗪酸铅锆双金属盐及其制备方法和应用,该双金属盐可作为固体推进剂的双功能弹道改良剂,即燃烧催化剂和燃烧稳定剂(又称不稳定燃烧抑制剂)。
技术背景
在改善双基推进剂或改性双基推进剂配方燃烧性能方面,当前常用的方法是通过加入一些金属盐作为燃烧催化剂,来调节推进剂的燃速和压力指数,添加量一般为质量分数的1%-5%。
铅化合物如雷索酸铅、水杨酸铅、硬脂酸铅等是现今双基系推进剂实际应用最主要的催化剂,然而随着导弹技术的不断发展,目前的燃烧催化剂已不能满足新型固体推进发展的需求。
另外,目前使用的最多的不稳定燃烧抑制剂为铝粉和Al2O3,虽然铝粉的加入解决了推进剂能量低、高频振荡不稳定燃烧等问题,但是铝粉在推进剂燃烧时参与了燃烧反应,使发动机弹道性能受到不利影响,更为重要的是在喷管尾部产生很浓的羽烟,这与现代武器要求推进剂具有低特征信号不符。而Al2O3由于其熔点较低,燃烧时易与催化剂PbO、CuO等凝聚成大粒子,既影响了催化剂的催化效率,也影响了不稳定燃烧的抑制效率。
发明内容
本发明的目的是提供一种柠嗪酸铅锆双金属盐;
本发明的另一目的是提供上述柠嗪酸铅锆双金属盐的合成方法;
本发明还有一个目的是提供上述柠嗪酸铅锆双金属盐作为燃烧催化剂和不稳定燃烧抑制剂的应用,该双金属盐在双基系推进剂中具有催化作用和不稳定燃烧抑制作用。
本发明的实现过程如下:
结构式(I)所示的柠嗪酸铅锆双金属盐,
上述柠嗪酸铅锆双金属盐的制备方法,包括以下步骤:
(1)将可溶性铅盐和可溶性锆盐分别溶于去离子水中配成溶液;
(2)将柠嗪酸用碱溶液溶解,控制溶液pH值在6~8,然后加入可溶性铅盐溶液,在50℃~70℃反应2h~4h;
(3)向步骤(2)溶液中加入强碱溶液,控制溶液pH值在8~10,再加入可溶性锆盐溶液,在70℃~90℃反应3h~5h,冷却、静置;
(4)将沉淀洗涤、过滤、干燥得到柠嗪酸铅锆双金属盐。
上述步骤(1)中,所述的可溶性铅盐为硝酸铅或醋酸铅,可溶性锆盐为硝酸氧锆或氯化氧锆。
上述步骤(2)中,所述的碱为Na2CO3、NaHCO3、吡啶或三乙胺。
上述步骤(3)中,所述的强碱为NaOH、KOH或甲醇钠。
本发明柠嗪酸铅锆双金属盐在双基系推进剂中可作为燃烧催化剂和燃烧稳定剂。
本发明优点与积极效果:本发明合成工艺简单,合成得到的柠嗪酸铅锆双金属盐作为燃烧催化剂和燃烧稳定剂时分解产生均匀的、新生态的铅及其氧化物可作为主要催化活性组分,分解产生的高熔点的二氧化锆作为助催化剂,可进一步提高催化效果。
附图说明
图1 为含柠嗪酸铅锆双基推进剂的燃速-压力曲线;
图2 为含柠嗪酸铅锆双基推进剂的催化效率-压力曲线。
具体实施方式
实施例1 柠嗪酸铅锆双金属盐的制备
(1)称取2.7g(0.01mol)的硝酸氧锆溶于30mL去离子水中配置成硝酸氧锆水溶液;称取3.1g(0.02mol)的柠嗪酸分散于200mL去离子水中,加入1.7g(0.02mol)碳酸氢钠溶解成澄清溶液;
(2)称取3.31g(0. 01mol)硝酸铅用50mL去离子水溶解配置成溶液,加入到柠嗪酸钠溶液中,搅拌混合均匀,升温至50℃,反应2h;
(3)称取1.6g(0.04mol)的氢氧化钠溶解于20mL去离子水中,加至步骤(2)的柠嗪酸铅钠溶液中,反应0.5h,加入步骤(1)配制的硝酸氧锆水溶液,升温至70℃反应3h,然后冷却、静置,将沉淀用去离子水多次洗涤、过滤、干燥可制得黑色柠嗪酸铅锆双金属盐5.91g,产率98.2%。
柠嗪酸铅锆双金属盐的表征
1、热重分析
该化合物在108℃~120℃,有失重现象,且质量损失为6.22%,经计算为失去两个结晶水,说明该化合物含有两个结晶水。
2、元素分析
各元素的测量值为(%):C 22.38, H 1.261,含有两个结晶水的目标化合物中各元素理论计算含量为(%):C 22.57, H 1.254,不含结晶水的化合物中各元素理论计算含量为(%):C 23.92, H 0.664。所测的C和H的含量更接近于含两个结晶水的化合物。
3、X射线荧光光谱分析
X射线荧光光谱分析金属的测量值为(%):Zr 13.95, Pb 31.89, 含有两个结晶水的目标化合物中金属含量的理论计算含量为(%):Zr 14.26, Pb 32.45, 而不含结晶水的化合物中金属含量的理论计算含量为(%):Zr 15.12, Pb 34.38。所测的Zr和Pb的含量更接近于含两个结晶水的化合物。
4、红外分析
在原料柠嗪酸红外光谱中,C=O的峰出现在1662cm-1, 柠嗪酸环上的-OH峰出现在3211 cm-1, 3065 cm-1, 2978 cm-1, 2642 cm-1, 而在目标化合物柠嗪酸铅锆化合物的红外光谱中可以看出,由于-OH形成了金属盐,因此,C=O的峰向低波数移动,出现在1599 cm-1,而代表蒽醌环上的-OH峰出现在3211 cm-1, 3065 cm-1, 2978 cm-1, 2642 cm-1出的吸收峰均消失,在3445 cm-1出现一宽峰,为目标化合物中的结晶水峰。
实施例2 柠嗪酸铅锆双金属盐的制备
(1)称取2.7g(0.01mol)的硝酸氧锆溶于30mL去离子水中配置成硝酸氧锆水溶液;称取3.1g(0.02mol)的柠嗪酸分散于200mL去离子水中,加入1.1g(0.01mol)碳酸钠溶解成澄清溶液;
(2)称取3.31g(0. 01mol)硝酸铅用50mL去离子水溶解配置成溶液,加入到柠嗪酸钠溶液中,搅拌混合均匀,升温至60℃,反应2h;
(3)称取2.3g(0.04mol)的氢氧化钾溶解于20mL去离子水中,加至步骤(2)的柠嗪酸铅钠溶液中,反应0.5h,加入步骤(1)配制的硝酸氧锆水溶液,升温至80℃反应4h,然后冷却、静置,将沉淀用去离子水多次洗涤、过滤、干燥可制得黑色柠嗪酸铅锆双金属盐5.82g,产率96.8%。
实施例3 柠嗪酸铅锆双金属盐的制备
(1)称取2.7g(0.01mol)的硝酸氧锆溶于30mL去离子水中配置成硝酸氧锆水溶液;称取3.1g(0.02mol)的柠嗪酸分散于200mL去离子水中,加入1.1g(0.01mol)碳酸钠溶解成澄清溶液;
(2)称取3.32g(0. 01mol)硝酸铅用50mL去离子水溶解配置成溶液,加入到柠嗪酸钠溶液中,搅拌混合均匀,升温至70℃,反应2h;
(3)称取2.3g(0.04mol)的氢氧化钾溶解于20mL去离子水中,加至步骤(2)的柠嗪酸铅钠溶液中,反应0.5h,加入步骤(1)配制的硝酸氧锆水溶液,升温至70℃反应3h,然后冷却、静置,将沉淀用去离子水多次洗涤、过滤、干燥可制得黑色柠嗪酸铅锆双金属盐5.75g,产率95.5%。
实施例4 柠嗪酸铅锆双金属盐应用
实验中所采用双基推进剂样品的基础配方为:硝化棉 (NC) 59%,硝化甘油(NG)30%,功能助剂11%。
固体推进剂样品采用吸收-驱水-放熟-压伸-切成药条的常规无溶剂压伸成型工艺制备。药量按500g配料,催化剂外加,加入量2.5%,对照空白推进剂样品不加催化剂。
燃速测定所用设备为燃速仪,采用靶线法测试样品燃速,将已处理过的5mm×15mm小药柱侧面用聚乙烯醇溶液包覆6次并晾干,然后在燃速仪中测试燃速,实验温度为20℃,压力范围2MPa~22MPa。
在图1、2中,u为燃速,P为压力,n为压力指数,ηr为催化效率(它是指相同压力下含催化剂的推进剂燃速与空白推进剂燃速之比),a为双基空白配方,b是含柠嗪酸铅锆的双基推进剂配方。从图中可以看出,在双基推进剂中,加入3%的柠嗪酸铅锆可明显提高双基推进剂的燃速,使燃速呈倍数提高,在4MPa~20MPa压力范围内,催化效率均在1.5以上,特别是在4MPa~8MPa压力范围内,催化效率达到2.0以上,并且在中高压段可明显降低压力指数,在12MPa~22MPa压力范围内,燃速压力指数n=0.25。
可见,本发明柠嗪酸铅锆双金属盐在双基推进剂中显示了强烈的提高燃速的能力,并在中高压下显著降低压力指数,说明该化合物是一种高效宽平台燃烧催化剂。
Claims (6)
2.权利要求1所述柠嗪酸铅锆双金属盐的制备方法,其特征在于包括以下步骤:
(1)将可溶性铅盐和可溶性锆盐分别溶于去离子水中配成溶液;
(2)将柠嗪酸用碱溶液溶解,控制溶液pH值在6~8,然后加入可溶性铅盐溶液,在50℃~70℃反应2h~4h;
(3)向步骤(2)溶液中加入强碱溶液,控制溶液pH值在8~10,再加入可溶性锆盐溶液,在70℃~90℃反应3h~5h,冷却、静置;
(4)将沉淀洗涤、过滤、干燥得到柠嗪酸铅锆双金属盐。
3.根据权利要求2所述的柠嗪酸铅锆双金属盐的制备方法,其特征在于:步骤(1)中,所述的可溶性铅盐为硝酸铅或醋酸铅,可溶性锆盐为硝酸氧锆或氯化氧锆。
4.根据权利要求2所述的柠嗪酸铅锆双金属盐的制备方法,其特征在于:步骤(2)中,所述的碱为Na2CO3、NaHCO3、吡啶或三乙胺。
5.根据权利要求2所述的柠嗪酸铅锆双金属盐的制备方法,其特征在于:步骤(3)中,所述的强碱为NaOH、KOH或甲醇钠。
6.权利要求1所述的柠嗪酸铅锆双金属盐在双基系推进剂中作为燃烧催化剂和燃烧稳定剂的应用。
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