CN110845285B - Method for reducing hygroscopicity of ammonium perchlorate - Google Patents
Method for reducing hygroscopicity of ammonium perchlorate Download PDFInfo
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- CN110845285B CN110845285B CN201810949268.8A CN201810949268A CN110845285B CN 110845285 B CN110845285 B CN 110845285B CN 201810949268 A CN201810949268 A CN 201810949268A CN 110845285 B CN110845285 B CN 110845285B
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- ethyl acetate
- fluororubber
- ammonium perchlorate
- polyacrylate rubber
- hygroscopicity
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B29/00—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate
- C06B29/22—Compositions containing an inorganic oxygen-halogen salt, e.g. chlorate, perchlorate the salt being ammonium perchlorate
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
- C06B23/009—Wetting agents, hydrophobing agents, dehydrating agents, antistatic additives, viscosity improvers, antiagglomerating agents, grinding agents and other additives for working up
Abstract
The invention discloses a method for reducing the hygroscopicity of ammonium perchlorate. According to the method, ammonium perchlorate, polyacrylate rubber and fluororubber are added into an ethyl acetate solution of the fluororubber according to the mass ratio of 96:3: 1-98: 1:1, the ethyl acetate solution of the polyacrylate rubber is slowly dripped while grinding, air drying is carried out, ethyl acetate is removed, and the ammonium perchlorate with the surface coated with the polyacrylate rubber and the fluororubber is obtained. The invention adopts a coating method, uses polyacrylate as a coating material and fluororubber as a cross-linking agent to coat AP, has simple, safe and reliable operation method, and obtains composite particles with uniform coating and obviously reduced hygroscopicity.
Description
Technical Field
The invention relates to a method for reducing the hygroscopicity of Ammonium Perchlorate (AP), belonging to the technical field of energetic materials.
Technical Field
Composite particle materials are multiphase materials made from 2 or more than 2 different types of particles through a process that has superior performance to each individual component material, and in some aspects may have unique properties that the component materials do not have.
AP is a strong oxidant, is commonly used in rocket propellants, has the advantages of no heavy metal ions, higher thermal stability, chemical stability and the like, and is a main energy substance and the most common oxidant in composite solid propellants, modified biradical propellants and NEPE propellants for a long time. The modified biradical propellant is widely applied to tactical rockets and missile weapon systems. Because a large amount of ultrafine ammonium perchlorate is introduced into the double-base propellant, the performance of AP has great influence on the overall performance of the propellant. However, AP has strong hygroscopicity, belongs to an energy-containing material which is easy to absorb moisture, and is easy to absorb moisture in the production, transportation and storage processes, and if AP absorbs moisture and is agglomerated, a plurality of potential safety hazards can be caused to the transportation and storage of the propellant, the quality of AP is influenced, and safety accidents such as spontaneous combustion, explosion and the like are easy to occur.
Therefore, the surface modification of AP has important significance in the fields of propellants, energetic materials and the like. The plum bin and the like are used for coating the AP with paraffin and thermoplastic polyurethane, so that a coating layer is formed on the surface of the AP, and the hygroscopicity and the sensitivity of the AP particles are reduced (plum bin and the like)]Energetic material 2014,22(06): 792-797). Wuhao uses graphene oxide to carry out unary coating on AP, uses fluorosilane to carry out binary coating on AP to prepare AP/GO/FAS composite particles, reduces the moisture absorption rate by 50%, advances the thermal decomposition peak by 32.9 ℃, and eliminates the thermal decomposition peak (Wuhao et al, binary coated AP moisture absorption and thermal decomposition performance research [ J]Solid rocket technology, 2014,37(05): 684-687). Preparation of nano Fe by ceramic membrane-antisolvent method for xujuan2O3Coating hydroxyl-terminated polybutadiene (HTPB) on the surface of the/AP composite particle by a solvent evaporation method to prepare nano Fe2O3The result of the/AP/HTPB composite particle shows that Fe2O3Nano Fe in/AP/HTPB composite particle2O3Uniformly dispersed, the HTPB coated on the outer layer prevents the moisture absorption of superfine AP (nanometer Fe such as Zijuan)2O3Preparation and characterization of/AP/HTPB composite particles [ J]The explosive and fire journal, 2012,35(06): 23-27.).
Disclosure of Invention
The invention aims to provide a simple method for reducing the hygroscopicity of AP.
The technical scheme for realizing the purpose of the invention is as follows:
the method for reducing the hygroscopicity of the ammonium perchlorate comprises the following specific steps:
adding ammonium perchlorate into an ethyl acetate solution of fluororubber according to the mass ratio of 96:3: 1-98: 1:1 of the ammonium perchlorate to the polyacrylate rubber to obtain the ammonium perchlorate with the surface coated with the polyacrylate rubber and the fluororubber, slowly dropwise adding the ethyl acetate solution of the polyacrylate rubber while grinding, drying in the air, and removing ethyl acetate.
Preferably, the mass ratio of the ammonium perchlorate to the polyacrylate rubber to the fluororubber is 97:2: 1.
Preferably, ethanol or water is added during the grinding process to increase the surface energy of the ammonium perchlorate, thereby facilitating coating.
Preferably, the average particle size of the ammonium perchlorate is more than or equal to 155 μm, and more preferably 150 to 200 μm.
Compared with the prior art, the invention has the following advantages:
the invention adopts a coating method, uses polyacrylate as a coating material and fluororubber as a cross-linking agent to coat AP, has simple, safe and reliable operation method, and obtains composite particles with uniform coating and obviously reduced hygroscopicity.
Drawings
FIG. 1 is an SEM image of coated AP of example 2 and raw AP.
Detailed Description
The present invention will be described in more detail with reference to the following examples and the accompanying drawings.
Comparative example 1
Weighing raw materials AP and polyacrylate rubber according to the mass ratio of 97.5:2.5 for later use. 25ml of ethyl acetate is measured, the polyacrylate rubber is added into the ethyl acetate to be soaked for 24 hours, and the mixture is magnetically stirred for 1 hour to be completely dissolved. Adding the raw material AP into the polyacrylate rubber ethyl acetate solution, and stirring in a mortar lightly until the ethyl acetate is completely volatilized. And pouring the treated AP particles into a watch glass, and putting the watch glass into a constant-temperature constant-humidity box. Air-dried at 25 ℃ and 20% humidity. Thus obtaining the treated AP particles.
Example 1
Raw materials AP, polyacrylate rubber: weighing the fluororubber according to the mass ratio of 97:2:1 for later use. 25ml of ethyl acetate is measured, the polyacrylate rubber is added into the ethyl acetate to be soaked for 24 hours, and the mixture is magnetically stirred for 1 hour to be completely dissolved. 5ml of ethyl acetate was weighed, and the fluororubber was added to the ethyl acetate and soaked for 24 hours, followed by magnetic stirring for 1 hour. So that it is completely dissolved. Adding the raw material AP into an ethyl acetate solution of polyacrylate rubber and fluororubber, and stirring in a mortar lightly until the ethyl acetate is completely volatilized. And pouring the treated AP particles into a watch glass, and putting the watch glass into a constant-temperature constant-humidity box. Air-dried at 25 ℃ and 20% humidity. Thus obtaining the treated AP particles.
Example 2
Raw materials AP, polyacrylate rubber: weighing the fluororubber according to the mass ratio of 97:2:1 for later use. 25ml of ethyl acetate is measured, the polyacrylate rubber is added into the ethyl acetate to be soaked for 24 hours, and the mixture is magnetically stirred for 1 hour to be completely dissolved. 5ml of ethyl acetate was weighed, and the fluororubber was added to the ethyl acetate and soaked for 24 hours, followed by magnetic stirring for 1 hour. So that it is completely dissolved. Adding the raw material AP into an ethyl acetate solution of polyacrylate rubber and fluororubber, adding 1ml of ethanol, and stirring in a mortar until the ethyl acetate is completely volatilized. And pouring the treated AP particles into a watch glass, and putting the watch glass into a constant-temperature constant-humidity box. Air-drying at 25 deg.C and 20% humidity. Thus obtaining the treated AP particles.
Example 3
Raw materials AP, polyacrylate rubber: weighing the fluororubber according to the mass ratio of 97:2:1 for later use. 25ml of ethyl acetate is measured, the polyacrylate rubber is added into the ethyl acetate to be soaked for 24 hours, and the mixture is magnetically stirred for 1 hour to be completely dissolved. 5ml of ethyl acetate was weighed, and the fluororubber was added to the ethyl acetate and soaked for 24 hours, followed by magnetic stirring for 1 hour. So that it is completely dissolved. Adding the raw material AP into an ethyl acetate solution of polyacrylate rubber and fluororubber, adding 1ml of deionized water, and stirring in a mortar until the ethyl acetate is completely volatilized. And pouring the treated AP particles into a watch glass, and putting the watch glass into a constant-temperature constant-humidity box. Air-drying at 25 deg.C and 20% humidity. Thus obtaining the treated AP particles.
Example 4
Raw materials AP, polyacrylate rubber: weighing the fluororubber according to the mass ratio of 96:3:1 for later use. 25ml of ethyl acetate is measured, the polyacrylate rubber is added into the ethyl acetate to be soaked for 24 hours, and the mixture is magnetically stirred for 1 hour to be completely dissolved. 5ml of ethyl acetate was weighed, and the fluororubber was added to the ethyl acetate and soaked for 24 hours, followed by magnetic stirring for 1 hour. So that it is completely dissolved. Adding the raw material AP into an ethyl acetate solution of polyacrylate rubber and fluororubber, and stirring in a mortar lightly until the ethyl acetate is completely volatilized. And pouring the treated AP particles into a watch glass, and putting the watch glass into a constant-temperature constant-humidity box. Air-dried at 25 ℃ and 20% humidity. Thus obtaining the treated AP particles.
Example 5
Raw materials AP, polyacrylate rubber: weighing the fluororubber according to the mass ratio of 98:1:1 for later use. 25ml of ethyl acetate is measured, the polyacrylate rubber is added into the ethyl acetate to be soaked for 24 hours, and the mixture is magnetically stirred for 1 hour to be completely dissolved. 5ml of ethyl acetate was weighed, and the fluororubber was added to the ethyl acetate and soaked for 24 hours, followed by magnetic stirring for 1 hour. So that it is completely dissolved. Adding the raw material AP into an ethyl acetate solution of polyacrylate rubber and fluororubber, and stirring in a mortar lightly until the ethyl acetate is completely volatilized. And pouring the treated AP particles into a watch glass, and putting the watch glass into a constant-temperature constant-humidity box. Air-dried at 25 ℃ and 20% humidity. Thus obtaining the treated AP particles.
Fig. 1 is SEM photographs of the AP particles before and after coating, illustrating that the polyacrylate rubber and the fluororubber are successfully coated on the AP particle surface.
TABLE 1 results of changes in AP hygroscopicity before and after modification
The samples obtained in the respective examples and comparative examples were subjected to a moisture absorption test, and the change in mass was measured by leaving the samples at 25 ℃ under a humidity of 100% for various times. The test results are shown in Table 1. As can be seen from table 1, examples 1 and 2 obtained good coating effects, and the hygroscopicity of the raw material AP was effectively controlled.
Claims (3)
1. The method for reducing the hygroscopicity of ammonium perchlorate is characterized by comprising the following specific steps:
adding ammonium perchlorate into an ethyl acetate solution of fluororubber according to the mass ratio of 97:2:1 of the ammonium perchlorate to the polyacrylate rubber to the fluororubber, slowly dropwise adding the ethyl acetate solution of the polyacrylate rubber while grinding, adding ethanol during grinding, drying in the air, and removing ethyl acetate to obtain the ammonium perchlorate with the surface coated with the polyacrylate rubber and the fluororubber.
2. The method as claimed in claim 1, wherein the ammonium perchlorate has a mean particle size of 155 μm or more.
3. The method according to claim 1, wherein the ammonium perchlorate has an average particle size of 150 to 200 μm.
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| CN113307709A (en) * | 2021-06-11 | 2021-08-27 | 西北工业大学 | Core-shell aluminum @ perchlorate/catalyst composite microsphere and solid propellant based on same |
| CN115650811B (en) * | 2022-11-09 | 2023-08-25 | 湖南恒达烟花有限公司 | Micro-smoke lead agent for fireworks |
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| CN1730532A (en) * | 2005-08-31 | 2006-02-08 | 苏州大学 | Flame-proof polyethylene material and its preparation method |
| CN102718187A (en) * | 2012-07-02 | 2012-10-10 | 南京师范大学 | Hollow ultrafine ammonium perchlorate and preparation method thereof |
| CN105541523A (en) * | 2015-12-15 | 2016-05-04 | 湖北航天化学技术研究所 | Thermoplastic carbon-hydrogen propellant composition |
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| RU2005706C1 (en) * | 1991-07-29 | 1994-01-15 | Центральный научно-исследовательский институт химии и механики | Ignition mixture for explosive cartridges |
| DE102008036649A1 (en) * | 2008-08-06 | 2010-02-18 | Diehl Bgt Defence Gmbh & Co. Kg | Active agent for selectively causing detonation or deflagration |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730532A (en) * | 2005-08-31 | 2006-02-08 | 苏州大学 | Flame-proof polyethylene material and its preparation method |
| CN102718187A (en) * | 2012-07-02 | 2012-10-10 | 南京师范大学 | Hollow ultrafine ammonium perchlorate and preparation method thereof |
| CN105541523A (en) * | 2015-12-15 | 2016-05-04 | 湖北航天化学技术研究所 | Thermoplastic carbon-hydrogen propellant composition |
Non-Patent Citations (2)
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| （甲基）丙烯酸酯聚合物包覆硝酸铵防吸湿改性研究;徐策;《中国优秀硕士学位论文全文数据库工程科技I辑》;20170715(第7期);B017-35页 * |
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