CN103212429A - Catalyst for accelerating burning rate used for reducing pressure exponent of nitramine propellant - Google Patents
Catalyst for accelerating burning rate used for reducing pressure exponent of nitramine propellant Download PDFInfo
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- CN103212429A CN103212429A CN2012100243926A CN201210024392A CN103212429A CN 103212429 A CN103212429 A CN 103212429A CN 2012100243926 A CN2012100243926 A CN 2012100243926A CN 201210024392 A CN201210024392 A CN 201210024392A CN 103212429 A CN103212429 A CN 103212429A
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Abstract
The invention relates to a method for preparing LaOCl-Mn composite oxide by using an eleaostearic acid solution combustion method, which comprises the following steps: 1) weighting lanthanum nitrate, manganese chloride and eleaostearic acid according to mol ratio of 1:1:x(x=7.0-10.0), under the oil bath heating condition, melting eleaostearic acid, performing magnetic stirring at constant temperature, melting lanthanum nitrate and manganese chloride solids in the melted eleaostearic acid, controlling the temperature at 110-118 DEG C to generate an uniform eleaostearic acid complex solution, placing in a muffle furnace at 500-600 DEG C, and then combusting to obtain the LaOCl-Mn composite oxide. The obtained LaOCl-Mn composite oxide can be directly used in the nitramine high energy propellant, thereby the pressure exponent of the propellant is reduced, and the combustion performance of the propellant is increased. The employed preparation technology has the advantages of rapidity, simpleness and convenience, the required raw materials are easily available and nontoxic, the preparation technology can realize industrialization easily.
Description
Technical field
The present invention relates to the preparation of LaOCl-Mn composite oxides in the nitramine class solid propellant and to the influence of propellant burning property.
Background technology
The burning rate pressure exponent of solid propellant (being called for short the pressure index) is the important technology parameter of solid propellant rocket, but, special control engine has the high pressure index except that needing solid propellant, general Strategy ﹠ Tactics solid propellant rocket, in order to guarantee that ballistic performance is stablized and the reliability of engine operation, all need solid propellant that low pressure index is arranged.Ammonium nitrate class propellant (high energy NEPE propellant especially, be the polyethers propellant of nitrate plasticising) in because a large amount of ring tetramethylene tetranitro amine (HMX) or RDX (RDX, 1,3,5-trinitro--1,3, the 5-Trianacyclohexane, claim cyclotrimethylene trinitramine again) introducing make the burning rate pressure exponent of propellant obviously improve (more than 0.5), combustion velocity modulation joint difficulty.Therefore for obtaining good engine performance, reduce the key technology that pressure index becomes high energy nitramine class propellants such as NEPE.
Studies show that: nanometer LaCoO
3, nano lanthanum oxide has catalytic action to the thermal decomposition of basic explosive mixture of the RDX that contains AP and RDX; In double base propellant, multiple nano composite oxide can make some double base propellant under low pressure fire speed and improve 2～3 times through after coating, and the pressure index descends, and platform and negative pressure index occur; In high energy NEPE propellant, studies show that: nano-sized carbon lead plumbate and nitrate have good compatibility, to reducing the NEPE Propellants With Lower Pressure Exponent remarkable effect is arranged, content is 1% and made this Propellants With Lower Pressure Exponent reduce to 0.54 and 0.52 at 2% o'clock respectively, near the application level of large-scale guided missile.The oxine slaine all can improve the combustion speed under the NEPE propellant 4.0-10.0MPa pressure, and reduces its burning rate pressure exponent to some extent.More than studies show that: the nano-oxide catalyst has showed effect preferably as burningrate catalyst.But because the combustibility that toxicity plumbous, mantoquita is added present NEPE propellant is still not fully up to expectations, so still need carry out the research work of burningrate catalyst and propellant burning property.
Summary of the invention
Because the preparation method influences the catalytic performance of products obtained therefrom, so the present invention has synthesized the LaOCl-Mn composite oxides by the stearic acid solution combustion method, experiment is found: the powder characteristic of it and gel of stearic acid firing method gained is very different.The present invention is by the lanthanum nitrate of burning different proportion, the stearic acid complex solution that manganese chloride and stearic acid generated, directly obtain the LaOCl-Mn composite oxides, used as nitramine class propellant (as the NEPE propellant, the nitramine modified double base propellant) burningrate catalyst, studies show that: can effectively reduce the pressure index of propellant, improve combustibility.
The present invention adopts with following scheme to realize:
The preparation method of LaOCl-Mn composite oxides: (1) is lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: (7-10), and weighing lanthanum nitrate, manganese chloride, stearic acid.Under the oil bath heating condition, earlier with the stearic acid fusion, under the constant temperature magnetic agitation, lanthanum nitrate, manganese chloride solid are fused in the fusion stearic acid, 110～118 ℃ of temperature controls make it generate uniform stearic acid complex solution, are placed in the 500-600 ℃ of Muffle furnace, after making its burning, obtain LaOCl-Mn composite oxides product.
When the present invention also provides different stearic acid ratios to synthesize the LaOCl-Mn composite oxides to add different amount to the influence of high energy nitramine class NEPE propellant burning property.The LaOCl-Mn composite oxides are directly added, and addition is 0.5-5.0%; Prescription solid content～75%.Adhesive composition: PET/N-100; Plasticizer: NG/TEGDN; Filler: HMX/AP/Al.
NEPE propellant preparation: each sample is pressed the design parameter preparation, with the vertical kneader vacuum kneading of HKV-II type, cast, 50 ℃ solidified after 7 days, the propellant sample is made 5mm * 5mm * 100mm medicinal strip and coat with polyvinyl alcohol, utilize static constant voltage to fire fast instrument and measure combustion speed at 20 ℃, method of testing is with reference to GJB-770B-2005 method 706.1.
Nitramine modified double base propellant prescription is formed: the catalyst addition is 1.1-2.1%, and all the other are RDX, nitrocotton, and nitre is sweet etc.
Experiment shows: by adding the 0.5%-3.0%LaOCl-Mn composite oxides, improved propellant and fire speed when low pressure, reduced its combustion speed when high pressure, significantly reduced the pressure index of nitramine class propellant.
The present invention has following advantage and effect:
For the preparation method, raw material used in the present invention is easy to get, and nontoxic.The preparation technology who is adopted has fast simple, and is convenient, and easily realizes characteristics such as industrialization.Prepared LaOCl-Mn composite oxides and propellant compatibility are good, need not processing such as coating.These advantages are that lead commonly used at present, mantoquita burningrate catalyst are incomparable.
Description of drawings
Fig. 1 is a lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: 8 sample LaOCl-Mn composite oxides SEM figure shows that the gained powder is the nanometer aggregation.The X-ray is shown as the mixture of LaOCl and amorphous powder, i.e. the LaOCl-Mn composite oxides.
The specific embodiment
Embodiment 1
Lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: 7, weighing lanthanum nitrate, manganese chloride, stearic acid.Under the oil bath heating condition, earlier with the stearic acid fusion, under the constant temperature magnetic agitation, lanthanum nitrate, manganese chloride solid are fused in the fusion stearic acid, 112 ℃ of temperature controls make it generate uniform stearic acid complex solution, are placed in the 500-600 ℃ of Muffle furnace, after making its burning, obtain the LaOCl-Mn composite oxides.
Make high energy NEPE nitramine class propellant according to following proportioning.Adopt PET/NG/TG class NEPE propellant formulation (Al:15%～18%, AP:15～20%), composition and content are as follows: PET/N-100 is an adhesive composition, content 7%～8%; NG/TEGDN is a plasticizer, content 18%～20%; Solid packing reserves 72%～75%.Wherein, the relative molecular mass Mn=4280 of PET, hydroxyl value: 26.4mgKOH/g, chain link is than n (EO)/n (THF)=50/50, average functionality f=1.9, N-100 average functionality 3.92, NCO content 5.32mmol/g.The 0.5%LaOCl-Mn composite oxides.
Each sample is pressed the design parameter preparation, and with the vertical kneader vacuum kneading of HKV-II type, cast, 50 ℃ solidified 7 days.The propellant sample is made 5mm * 5mm * 100mm medicinal strip and with the polyvinyl alcohol coating, utilized static constant voltage to fire fast instrument 20 ℃ of mensuration combustion speed, and method of testing is with reference to GJB-770B-2005 method 706.1.
Experimental result shows: 1) Zhi Bei LaOCl-Mn composite oxides are compatible with NEPE propellant system, and propellant preparation and curing show no obvious abnormalities (portal or stability variation etc.), all the propellant sample of the even compact that can make.2) catalyst is less to the influence of medicine slurry curing reaction, and the medicine slurry solidified through 7 days can obtain normal propellant sample.
The combustion speed of propellant with the pass of pressure index is: r=bP
nR in the formula, b, P and n are respectively combustion speed, experimental constant, pressure and pressure index.With ln (r)-ln (P) mapping, gained the results are shown in Table 1.From table 1 as seen, increase by 0.5% gained LaOCl-Mn composite oxides obvious combustion speed when having increased low pressure, the combustion speed when having reduced high pressure, thereby the obvious pressure index that has reduced the NEPE propellant.
Embodiment 2
Lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: 10, weighing lanthanum nitrate, manganese chloride, stearic acid.Under the oil bath heating condition, earlier with the stearic acid fusion, under the constant temperature magnetic agitation, lanthanum nitrate, manganese chloride solid are fused in the fusion stearic acid, 117 ℃ of temperature controls make it generate uniform stearic acid complex solution, are placed in the 500-600 ℃ of Muffle furnace, after making its burning, obtain LaOCl-Mn composite oxides product.
Propellant preparation and combustibility method of testing are added 1.0% gained LaOCl-Mn composite oxides product with embodiment 1 in the NEPE propellant.
Experimental result shows: the LaOCl-Mn composite oxides of preparation are compatible with NEPE propellant system, and catalyst is less to the influence of medicine slurry curing reaction, and the medicine slurry solidified through 7 days can obtain normal propellant sample.
With ln (r)-ln (P) mapping, gained the results are shown in Table 1.From table 1 as seen, increase by 1.0% gained LaOCl-Mn composite oxides obvious combustion speed when having increased low pressure, the combustion speed when having reduced high pressure, thereby the obvious pressure index that has reduced the NEPE propellant.
Table 1LaOCl-Mn composite oxides are to the influence of NEPE propellant burning property
Embodiment 3
Lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: 8, weighing lanthanum nitrate, manganese chloride, stearic acid.Under the oil bath heating condition, earlier with the stearic acid fusion, under the constant temperature magnetic agitation, lanthanum nitrate, manganese chloride solid are fused in the fusion stearic acid, 117 ℃ of temperature controls make it generate uniform stearic acid complex solution, are placed in the 500-600 ℃ of Muffle furnace, after making its burning, obtain LaOCl-Mn composite oxides product.
Nitramine modification propellant preparation: the propellant formulation that does not add any catalyst: NC (nitrocotton) adds that NG (nitre is sweet) is 41.5%, RDX is 55.7%, function additive and other are 2.8%, catalyst-free; The prescription that adds catalyst: NG adds that NC is 41.3%, RDX is 55.7%, and function additive and other are 2.0%, catalyst is 1.1%.The gained experimental result sees Table 2.
Embodiment 4
Lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: 9, weighing lanthanum nitrate, manganese chloride, stearic acid.Under the oil bath heating condition, earlier with the stearic acid fusion, under the constant temperature magnetic agitation, lanthanum nitrate, manganese chloride solid are fused in the fusion stearic acid, 117 ℃ of temperature controls make it generate uniform stearic acid complex solution, are placed in the 500-600 ℃ of Muffle furnace, after making its burning, obtain LaOCl-Mn composite oxides product.
Nitramine modification propellant preparation: the propellant formulation that does not add any catalyst: NC (nitrocotton) adds that NG (nitre is sweet) is 41.5%, RDX is 55.7%, function additive and other are 2.8%, catalyst-free; The prescription that adds catalyst: NG adds that NC is 41.1%, RDX is 53.9%, and function additive and other are 2.0%, catalyst is 3.0%.The gained experimental result sees Table 2.
From table 2 as seen, increase a spot of LaOCl-Mn composite oxides obvious combustion speed when having increased low pressure, the combustion speed when having reduced high pressure, thus reduced the pressure index of propellant, and improved the combustibility of propellant accordingly.
In sum, by adding the LaOCl-Mn composite oxides of different proportion, improved the combustion speed when low pressure of nitramine class propellant, reduced its combustion speed when high pressure, significantly reduced the pressure index of nitramine class propellant, and the composite oxides amount that adds is many more, effect is obvious more.The LaOCl-Mn composite oxides are the good burningrate catalysts of nitramine class propellant.
Table 2LaOCl-Mn composite oxides are to the influence of nitramine modification propellant burning property
Claims (1)
1. method that reduces nitramine class propellant burning rate pressure exponent, it is characterized in that: the LaOCl-Mn composite oxides that use the preparation of stearic acid solution combustion method, the LaOCl-Mn composite oxides of 0.5-3.0% are directly added in the nitramine class high-energy propellant, and the preparation method of described LaOCl-Mn composite oxides is as follows:
Lanthanum nitrate in molar ratio: manganese chloride: stearic acid=1: 1: x (x=7.0-10.0), weighing lanthanum nitrate, manganese chloride and stearic acid are under the oil bath heating condition, earlier with the stearic acid fusion, under the constant temperature magnetic agitation, with lanthanum nitrate, the manganese chloride solid is fused in the fusion stearic acid, 110～118 ℃ of temperature controls, make it generate uniform stearic acid complex solution, be placed in the 500-600 ℃ of Muffle furnace, make its burning after, obtain LaOCl-Mn composite oxides product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777458A (en) * | 2014-12-26 | 2016-07-20 | 比亚迪股份有限公司 | Automatic ignition powder for gas generator of air bag restraint system of automobile and preparation method of automatic ignition powder |
| CN106336334A (en) * | 2015-09-01 | 2017-01-18 | 湖北航天化学技术研究所 | Formula for reducing high pressure exponent of solid propellant |
| CN107056565A (en) * | 2016-12-09 | 2017-08-18 | 湖北航天化学技术研究所 | A kind of Pressure Exponent conditioning agent of solid propellant |
| CN110455862A (en) * | 2019-08-19 | 2019-11-15 | 宜宾北方川安化工有限公司 | A method of adjusting civilian SOLID PROPELLANT COMBUSTION performance |
| CN114230420A (en) * | 2021-12-10 | 2022-03-25 | 宜宾北方川安化工有限公司 | Emulsification process of lead salt and lead-containing organic matter |
-
2012
- 2012-01-20 CN CN2012100243926A patent/CN103212429A/en active Pending
Non-Patent Citations (3)
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| ZHI-XIN WEI ET AL.: "Combustion synthesis and effect of LaMnO3 and LaOCl powder mixture on HMX thermal decomposition", 《THERMOCHIMICA ACTA》 * |
| 刘海燕: "LaBO_3(B=Fe,Mn,Co)的制备及其对TNT废水的光催化研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 卫芝贤等: "硬脂酸溶胶-凝胶法制备超细LaCoO3及对硝胺改性双基推进剂燃烧性能的影响研究", 《兵工学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105777458A (en) * | 2014-12-26 | 2016-07-20 | 比亚迪股份有限公司 | Automatic ignition powder for gas generator of air bag restraint system of automobile and preparation method of automatic ignition powder |
| CN106336334A (en) * | 2015-09-01 | 2017-01-18 | 湖北航天化学技术研究所 | Formula for reducing high pressure exponent of solid propellant |
| CN107056565A (en) * | 2016-12-09 | 2017-08-18 | 湖北航天化学技术研究所 | A kind of Pressure Exponent conditioning agent of solid propellant |
| CN107056565B (en) * | 2016-12-09 | 2020-07-21 | 湖北航天化学技术研究所 | Pressure index regulator of solid propellant |
| CN110455862A (en) * | 2019-08-19 | 2019-11-15 | 宜宾北方川安化工有限公司 | A method of adjusting civilian SOLID PROPELLANT COMBUSTION performance |
| CN114230420A (en) * | 2021-12-10 | 2022-03-25 | 宜宾北方川安化工有限公司 | Emulsification process of lead salt and lead-containing organic matter |
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Application publication date: 20130724 |