CN105152969B - Dimethyl glyoxime magnesium and preparation method thereof - Google Patents
Dimethyl glyoxime magnesium and preparation method thereof Download PDFInfo
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- CN105152969B CN105152969B CN201510511342.4A CN201510511342A CN105152969B CN 105152969 B CN105152969 B CN 105152969B CN 201510511342 A CN201510511342 A CN 201510511342A CN 105152969 B CN105152969 B CN 105152969B
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- dimethyl glyoxime
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Abstract
A kind of dimethyl glyoxime magnesium compound the invention discloses structural formula as shown in (I),Decomposable asymmetric choice net produces magnesia be evenly distributed, nascent state as main catalytic active component when it is used as combustion catalyst, auxiliary catalysis component carbonizable substance is produced simultaneously, there is excellent catalytic effect to the burning of low burn temperature deflagration solid propellant, burning rate pressure exponent can be significantly reduced while propellant burning rate is not improved.
Description
Technical field
The present invention relates to a kind of dimethyl glyoxime magnesium compound, the compound can be used as the combustion catalysis of solid propellant
Agent.
Technical background
With the development of sophisticated technology, guided missile, the increase of rocket flight distance and the raising of control accuracy, to solid gas
Generator proposes requirement higher, it is desirable to which its lightweight, working time is longer, and this requires gas generator propellant not only gas production
Greatly, combustion gas cleanliness factor is high, and burn rate, combustion temperature are lower, but the performance of propellant is related, and combustion temperature is low, and quick-fried heat is low certainly will
The combustibility of propellant can be influenceed, propellant burning rate Pressure Exponent is become big, incomplete combustion, residue increase.
In terms of biradical system's low burn temperature, low burning rate propellant, it will usually delayed point by the catalyst for adding fusing point higher
Solution speed, addition decompose the catalyst degradation combustion temperature of heat absorption, use the relatively large composition of gas production and chemically thermodynamics
The oxygen balance that control of setting out is formulated realizes low burn temperature, low combustion residue and combustion gas cleaning to reduce the methods such as exhaust residue.
And the conventional combustion catalyst of biradical system's gas generator propellant be present, such as Al2O3Fusing point is relatively low, during burning easily and other
Catalyst is condensed into big particle, is bonded at causing trouble on gas conduct pipe or turbofan；Compound containing Zr, Bi is then too hard, easily beats
Bad turbofan.Double-base state containing magnesia not only has that combustion flame temperature is low, and solid content is low in combustion gas, be free of
The advantages of corrosion products such as chlorine or chlorine compound, and it is insensitive to temperature and impact, have good within the scope of temperature wider
Good mechanical property, while the addition of MgO may also function as sound and vibration rough burning inhibitory action, but the magnesia as catalyst
Unstable, easy moisture absorption, performance easily changes and then fails during storage, seriously limits the use longevity of such propellant
Life.Additionally, containing water-soluble substances in propellant formulation, also it is unfavorable for prepared by solvent-free pressure stretch technique.
Therefore, need searching one kind itself badly not reacted with water, storage good security long, but decomposition can produce the magnesium of magnesia again
Base combustion catalyst, the need for meeting new low burn temperature, the development of low burning rate solid propellant.
The content of the invention
In order to solve shortcomings and deficiencies of the prior art, the present invention provides a kind of dimethyl glyoxime magnesium compound and its system
Preparation Method.
Implementation process of the invention is as follows：
Dimethyl glyoxime magnesium compound shown in structure formula (I),
The preparation method of above-mentioned dimethyl glyoxime magnesium compound, comprises the following steps：
(1) soluble magnesium salt is dissolved in wiring solution-forming in deionized water；
(2) dimethyl glyoxime highly basic is dissolved, control solution ph is subsequently adding soluble magnesium salt molten 9~10
Liquid；
(3) cooling, standing after reacting 2h~4h at 70 DEG C~90 DEG C；
(4) by washing of precipitate, filter, be dried to obtain dimethyl glyoxime magnesium compound.
Described soluble magnesium salt is magnesium nitrate, magnesium chloride or magnesium sulfate, and highly basic is NaOH, KOH or sodium methoxide.
Advantage of the present invention and good effect：Synthesis technique of the present invention is simple, the dimethyl glyoxime magnesium chemical combination that synthesis is obtained
Decomposable asymmetric choice net produces the be evenly distributed, magnesia of nascent state as main catalytic active component when thing is as combustion catalyst, together
When produce auxiliary catalysis component carbonizable substance, can further improve the catalytic effect to low burn temperature deflagration solid propellant.
Brief description of the drawings
Fig. 1 is the XRD of dimethyl glyoxime magnesium compound solid phase catabolite；
Fig. 2 is that the burn rate-pressure curve after dimethyl glyoxime magnesium of the present invention is added in modified double base propellant.
Specific embodiment
Embodiment 1The preparation of dimethyl glyoxime magnesium compound
(1) dimethyl glyoxime of 34.75g (0.3mol) is weighed, is scattered in 250mL deionized waters, use NaOH
Solution regulation solution ph is 9；Weigh the nitric hydrate magnesium 100mL deionized water dissolvings of 76.8g (0.3mol) three be configured to it is molten
Liquid, is added in above-mentioned solution, is uniformly mixed；
(2) in 70 DEG C of constant temperature, then stirring reaction 2h cools down, stands；
(3) precipitation deionized water repeatedly washed, filtered, drying can be obtained white dimethyl glyoxime magnesium compound
47.2g, yield 90.4%.
The sign of dimethyl glyoxime magnesium compound
1st, infrared spectrum (KBr, cm-1)υ:3208,2930,1939,1636,1445,1384,1364,1141,981,906.
2nd, organic element analysis
Molecular formula:C4H6N2O2Mg·2H2O
Theoretical value (%):C 27.54,H 5.78,N 16.06.
Measured value (%):C 27.51,H 5.68,N16.02.
3rd, X-ray fluorescence spectra analysis
The measured value of metal is (%):Mg 13.03,
The theoretical value (%) of metal:Mg 13.93.
Said structure appraising datum confirms that it is dimethyl glyoxime magnesium dihydrate to obtain material.
Embodiment 2The preparation of dimethyl glyoxime magnesium compound
(1) dimethyl glyoxime of 1.38g (0.012mol) is weighed, is scattered in 10mL deionized waters, use NaOH
Solution regulation solution ph is 9；Weigh the nitric hydrate magnesium 10mL deionized water dissolvings of 3.07g (0.012mol) three be configured to it is molten
Liquid, is added in above-mentioned solution, is uniformly mixed；
(2) in 70 DEG C of constant temperature, then stirring reaction 2h cools down, stands；
(3) precipitation deionized water repeatedly washed, filtered, drying can be obtained white dimethyl glyoxime magnesium compound
1.69g, yield 80.9%.
The solid phase catabolite analysis of dimethyl glyoxime magnesium compound
Dimethyl glyoxime magnesium dihydrate is placed in crucible and is calcined 1 hour with 500 DEG C, obtain white powder.X-ray is spread out
Firing table is bright (as shown in Figure 1), and five diffraction maximums 36.74,42.82,62.20,74.24 and 78.30 correspond respectively to face-centered cubic
(111) of MgO, (200), (220), (311) and (222) crystal face.
The application of dimethyl glyoxime magnesium compound
Contain two methyl and two oximidos in dimethyl glyoxime structure, a molecule is can be seen that from its structural analysis
Glyoxime parent can reactive magnesium with a molecule, the content of magnesium obtained in compound is higher, is expected to effectively adjust biradical
It is the combustibility of solid propellant, is compounded with the Pb-Cu salt composite catalyst of routine below by way of by dimethyl glyoxime magnesium
Afterwards, added in modified double base propellant and investigating its combustion catalysis performance.
The basic components of modified double base propellant sample are employed in experiment：Biradical adhesive (NC+NG) 72%, black rope
The present (RDX) 16%, function additive 12%.Spice presses 500g dispensings, and catalyst is outer dosage, and addition is 6.6%, wherein diformazan
Base glyoxime magnesium compound is 3%, Pb-Cu salt composite catalyst 3%；Control group blank propellant sample is free of catalyst.
Solid propellant sample using the ripe-pressure stretch of absorption-expelling water-put-be cut into medicinal strip the solvent-free companding shaping work of routine
It is prepared by skill.The burn rate of sample is measured using target collimation method.By processed Φ 5mm × 150mm small grains side polyvinyl alcohol
Solution impregnation is coated 6 times and dried, and then carries out Burning rate testing in nitrogen charging slow-action formula Burning velometer.Test temperature is 20 DEG C, pressure
Strong scope 4MPa~14MPa.
In fig. 2, u is burn rate, and p is pressure, and a is modified double base blank formula, and b is magnesium compound containing dimethyl glyoxime
Modified double base propellant formula.It can be seen that the dimethyl glyoxime that the embodiment 1 of addition 3.0% is prepared
After magnesium compound, increasing does not occur in propellant burning rate, or even burn rate is less than blank propellant formulation under 12MPa and 14MPa；
Meanwhile, reduction Pressure Exponent (n) effect containing catalyst propellant is substantially better than blank formula, in 4MPa~12Mpa pressure models
Interior n=0.35 is enclosed, double based propellant is presented.
Additionally, the modified double base propellant formula containing dimethyl glyoxime magnesium compound also has a feature, i.e. its burn rate
Pressure Exponent is better than higher-pressure region (8~12MPa is 0.45) in low-pressure area (4~8MPa is 0.34), and this feature has practicality very much,
Because most gas generator operating pressures are not high, generally 4~10MPa, low-pressure area Pressure Exponent is good, with gas generator
Working environment be just adapted, be conducive to gas generator smooth working, keep stable performance.
It can be seen that, the catalyst shows excellent combustion catalysis effect to low burn temperature deflagration solid propellant, can be not
Burning rate pressure exponent is significantly reduced while improving propellant burning rate.
Claims (4)
1. a kind of dimethyl glyoxime magnesium compound, it is characterised in that structural formula is as shown in (I)：
2. the preparation method of dimethyl glyoxime magnesium compound described in claim 1, it is characterised in that comprise the following steps：
(1) soluble magnesium salt is dissolved in wiring solution-forming in deionized water；
(2) dimethyl glyoxime highly basic is dissolved, control solution ph is subsequently adding soluble magnesium salting liquid 9~10；
(3) cooling, standing after reacting 2h~4h at 70 DEG C~90 DEG C；
(4) by washing of precipitate, filter, be dried to obtain dimethyl glyoxime magnesium compound.
3. the preparation method of dimethyl glyoxime magnesium compound according to claim 2, it is characterised in that：Described is solvable
Property magnesium salts be magnesium nitrate, magnesium chloride or magnesium sulfate.
4. the preparation method of dimethyl glyoxime magnesium compound according to claim 2, it is characterised in that：Described highly basic
It is NaOH, KOH or sodium methoxide.
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| CN1103257C (en) * | 1998-07-08 | 2003-03-19 | 中国科学技术大学 | Process for preparing superfine powder by thermolyzing metal complex |
| JP5806080B2 (en) * | 2010-10-22 | 2015-11-10 | 国立大学法人九州大学 | Photoreduction catalyst for reducing olefins |
| EP2548973A1 (en) * | 2011-07-20 | 2013-01-23 | Centre National de la Recherche Scientifique | New actinomycete strain composition and its use |
| CN104628498A (en) * | 2015-02-12 | 2015-05-20 | 西安近代化学研究所 | Energetic polyoxide compound super-thermite and preparation method thereof |
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Granted publication date: 20170704 Termination date: 20200819 |