CN108910843A - 一种推进剂燃料的制备方法 - Google Patents
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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- C01B21/16—Hydrazine; Salts thereof
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- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
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- C07C243/10—Hydrazines
- C07C243/12—Hydrazines having nitrogen atoms of hydrazine groups bound to acyclic carbon atoms
- C07C243/14—Hydrazines having nitrogen atoms of hydrazine groups bound to acyclic carbon atoms of a saturated carbon skeleton
Abstract
本发明公开了一种推进剂燃料的制备方法，包括以下步骤，将肼或其甲基衍生物与硼烷的四氢呋喃溶液均匀混合后进行反应，反应后旋干四氢呋喃溶液，得到第一产物，将所述第一产物加入第一溶剂，然后进行洗涤后，旋干第一溶剂，得到肼基硼烷衍生物。该方法将具有高挥发性的肼类燃料及其肼的加急化衍生物硼氢化，得到的肼类的硼氢化物为无色不挥发液体或白色固体，无挥发性，极大地降低了肼类燃料的危害性，且肼类的硼氢化物点火延迟时间极短，是一种新型的航天推进剂燃料。
Description
技术领域
本发明涉及推进剂技术领域，具体涉及一种推进剂燃料及其制备方法。
背景技术
在航天航空及国防军事领域(如战略、战术导弹)中，推进剂是最核心的关键技术之一。当前，液体推进剂仍是世界上使用最广泛的推进剂。自燃推进剂是液体推进剂中最具代表性的一种,目前世界各国最普遍采用自燃推进剂燃料是肼及肼的甲基化衍生物。但是肼类化合物具有高挥发性、剧毒性和强致癌性，对环境和人体健康十分有害，而且由于其易燃和强挥发性，大大增加了其运输和储存的成本。
发明内容
本发明为了解决上述的技术问题，提供了一种推进剂燃料的制备方法，该方法将具有高挥发性的肼类燃料及其肼的加急化衍生物硼氢化，得到的肼类的硼氢化物为无色不挥发液体或白色固体，无挥发性，极大地降低了肼类燃料的危害性，且肼类的硼氢化物点火延迟时间极短，是一种新型的航天推进剂燃料。
为了达到上述技术效果，本发明提供一种推进剂燃料的制备方法，包括以下步骤：将肼或其甲基衍生物与硼烷的四氢呋喃溶液均匀混合后进行反应，反应后旋干四氢呋喃溶液，得到第一产物，将所述第一产物加入第一溶剂，然后进行洗涤后，旋干第一溶剂，得到肼基硼烷衍生物。
进一步的，所述均匀混合采用磁力搅拌进行混合。
进一步的，所述反应过程具体为先在15～25℃下反应2～3小时，然后升温至65～85℃反应8～10小时，然后降温到15～25℃。
所述硼烷的四氢呋喃溶液的体积及与肼或其甲基衍生物的体积比为1:0.5～1:5，其中所述硼烷的四氢呋喃溶液的浓度为1mol/L。
进一步的，所述第一溶剂为二氯甲烷。
进一步的，所述洗涤具体为使用丙酮进行洗涤。
进一步的，所述肼基硼烷衍生物选自1-硼烷肼衍生物，1,2-二硼烷肼衍生物，1-硼烷偏甲肼衍生物衍生物，1,2-二硼烷偏甲肼衍生物，1-硼烷偏二甲肼衍生物中的任意一种。
进一步的，所述肼或者肼的甲基衍生物反应前溶于无水四氢呋喃溶液中，所述肼或者肼的甲基衍生物与无水四氢呋喃溶液的体积比1：0.5-1:20。
下面对本申请进行进一步的解释和说明，本申请的肼及其甲基衍生物具有如下三种结构式：H2N-NH2 将肼或其甲基衍生物与硼烷的四氢呋喃溶液反应，当硼烷的四氢呋喃溶液的体积及与肼类化合物的体积比例不同时，会得到不同的肼基硼烷衍生物，即化合物1、化合物2、化合物3、化合物4和化合物5，其中化合物1～化合物5的结构式分别为
本发明具有如下有益效果：硼烷基团具有将挥发性燃料固化而不降低其点火延迟时间的功能。本发明利用硼烷的这种功能，将具有高挥发性的肼类燃料及其肼的加急化衍生物硼氢化，得到的肼类的硼氢化物为无色不挥发液体或白色固体，无挥发性，极大地降低了肼类燃料的危害性，且肼类的硼氢化物点火延迟时间极短，得到了一种新型的航天推进剂燃料，且该制备方法具有原料易得、操作简便、安全性高、条件温和、工艺可控，可以大批量制造生产的特点。
附图说明
图1为本发明推进剂燃料的合成路线图；
具体实施方式
下面结合附图和具体实施例对本发明做进一步的说明。
实施例1
将1.6ml肼(32g/mol)溶于30ml无水四氢呋喃溶液，搅拌混合均匀后，常温下缓慢加入75ml浓度为1M的硼烷四氢呋喃溶液，磁力搅拌混合，待硼烷溶液加入完毕后，常温反应2h后，缓慢升温至70℃反应8h。降至室温后旋干四氢呋喃溶液，加入50ml二氯甲烷，丙酮多次洗涤后，旋干二氯甲烷得到无色透明液体1，产物收率89％。1H NMR(600MHz,DMSO-d6):δppm:1.5(s,2H),7.2(s,2H),0.04–0.40(m,3H,BH3).Elemental analysis,calcd(％)forBH7N2(46.07):H:15.38,N:61.06,Found,H:14.99,N:61.43。
实施例2
将1.6ml肼(32g/mol)溶于30ml无水四氢呋喃溶液，搅拌混合均匀后，常温下缓慢加入110ml浓度为1M的硼烷四氢呋喃溶液，磁力搅拌混合，待硼烷溶液加入完毕后，常温反应3h后，缓慢升温至70℃反应4h，再升温至80℃反应10h。降至室温后旋干四氢呋喃溶液，加入70ml二氯甲烷，丙酮多次洗涤后，旋干二氯甲烷得到微白色液体2，产物收率90.5％。1HNMR(600MHz,DMSO-d6):δppm:7.2(s,4H),0.09–0.42(m,6H,BH3).Elemental analysis,calcd(％)for B2H10N2(60.10):H:16.88,N:46.91,Found,H:17.02,N:47.22。
实施例3
将2.3ml一甲肼(46g/mol)溶于30ml无水四氢呋喃溶液，搅拌混合均匀后，常温下缓慢加入60ml浓度为1M的硼烷四氢呋喃溶液，磁力搅拌混合，待硼烷溶液加入完毕后，常温反应2h后，缓慢升温至70℃反应6h。降至室温后旋干四氢呋喃溶液，加入40ml二氯甲烷，丙酮多次洗涤后，旋干二氯甲烷得到无色透明液体3，产物收率87.3％。1H NMR(600MHz,DMSO-d6):δppm:1.5(s,H),2.47(m,3H,CH3),7.2(s,2H),0.04–0.40(m,3H,BH3).13C NMR(150MHz,DMSO-d6):δ:ppm:34.15.Elemental analysis,calcd(％)for CH9BN2(60.09):C:20.05,H:15.14,N:46.76,Found,C:19.70,H:15.39,N:47.13。
实施例4
将2.3ml一甲肼(46g/mol)溶于30ml无水四氢呋喃溶液，搅拌混合均匀后，常温下缓慢加入130ml浓度为1M的硼烷四氢呋喃溶液，磁力搅拌混合，待硼烷溶液加入完毕后，常温反应3h后，缓慢升温至70℃反应5h，再升温至85℃反应8h。降至室温后旋干四氢呋喃溶液，加入70ml二氯甲烷，丙酮多次洗涤后，旋干二氯甲烷得到微白色蜡状固体4，产物收率92.1％。1H NMR(600MHz,DMSO-d6):δppm:2.90(s,H),7.2(s,2H),0.07–0.43(m,6H,BH3).13CNMR(150MHz,DMSO-d6):δ:ppm:31.23.Elemental analysis,calcd(％)for CH12B2N2(74.12):C:16.29,H:16.40,N:37.99,Found,C:15.96,H:17.02,N:37.22。
实施例5
将3.1ml偏二甲肼(60.1g/mol)溶于30ml无水四氢呋喃溶液，搅拌混合均匀后，常温下缓慢加入60ml浓度为1M的硼烷四氢呋喃溶液，磁力搅拌混合，待硼烷溶液加入完毕后，常温反应3h后，缓慢升温至70℃反应12h。降至室温后旋干四氢呋喃溶液，加入50ml二氯甲烷，丙酮多次洗涤后，旋干二氯甲烷得到无色透明液体5，产物收率88.4％。1H NMR(600MHz,DMSO-d6):δppm:2.47(m,6H,CH3),7.2(s,2H),0.04–0.40(m,3H,BH3).13C NMR(150MHz,DMSO-d6):δ:ppm:43.27.Elemental analysis,calcd(％)for C2H11BN2(74.10):C:32.49,H:15.00,N:37.89,Found,C:31.70,H:15.59,N:37.53。
在本说明书中所谈到的“一个实施例”、“另一个实施例”、“实施例”等，指的是结合该实施例描述的具体特征、结构或者特点包括在本申请概括性描述的至少一个实施例中。在说明书中多个地方出现同种表述不是一定指的是同一个实施例。进一步来说，结合任一个实施例描述一个具体特征、结构或者特点时，所要主张的是结合其他实施例来实现这种特征、结构或者特点也落在本发明的范围内。
尽管这里参照发明的多个解释性实施例对本发明进行了描述，但是，应该理解，本领域技术人员可以设计出很多其他的修改和实施方式，这些修改和实施方式将落在本申请公开的原则范围和精神之内。更具体地说，在本申请公开权利要求的范围内，可以对主题组合布局的组成部件和/或布局进行多种变型和改进。除了对组成部件和/或布局进行的变型和改进外，对于本领域技术人员来说，其他的用途也将是明显的。
Claims (8)
1.一种推进剂燃料的制备方法，其特征在于，包括以下步骤：将肼或其甲基衍生物与硼烷的四氢呋喃溶液均匀混合后进行反应，反应后旋干四氢呋喃溶液，得到第一产物，将所述第一产物加入第一溶剂，然后进行洗涤后，旋干第一溶剂，得到肼基硼烷衍生物。
2.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述均匀混合采用磁力搅拌进行混合。
3.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述反应过程具体为先在15～25℃下反应2～3小时，然后升温至65～85℃反应8～10小时，然后降温到15～25℃。
4.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述硼烷的四氢呋喃溶液的体积及与肼或其甲基衍生物的体积比为1:0.5～1:5，其中所述硼烷的四氢呋喃溶液的浓度为1mol/L。
5.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述第一溶剂为二氯甲烷。
6.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述洗涤具体为使用丙酮进行洗涤。
7.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述肼基硼烷衍生物选自1-硼烷肼衍生物，1,2-二硼烷肼衍生物，1-硼烷偏甲肼衍生物衍生物，1,2-二硼烷偏甲肼衍生物，1-硼烷偏二甲肼衍生物中的任意一种。
8.根据权利要求1所述的推进剂燃料的制备方法，其特征在于，所述肼或者肼的甲基衍生物反应前溶于无水四氢呋喃溶液中，所述肼或者肼的甲基衍生物与无水四氢呋喃溶液的体积比1：0.5～1:20。
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Application publication date: 20181130 |