CN105152969A - Dimethylglyoxime magnesium and preparation method thereof - Google Patents
Dimethylglyoxime magnesium and preparation method thereof Download PDFInfo
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- CN105152969A CN105152969A CN201510511342.4A CN201510511342A CN105152969A CN 105152969 A CN105152969 A CN 105152969A CN 201510511342 A CN201510511342 A CN 201510511342A CN 105152969 A CN105152969 A CN 105152969A
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- magnesium
- combustion
- dimethyl glyoxime
- magnesium compound
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Abstract
The invention discloses a dimethylglyoxime magnesium compound with a structural formula represented in a formula (I). The dimethylglyoxime magnesium compound can be decomposed to produce uniformly distributed nascent magnesium oxide as a main catalytic active component when used as a combustion catalyst and can produce a carbon substance as an assisted catalytic component simultaneously, thereby having excellent catalytic effect on combustion of a slow-combustion solid propellant with a low combustion temperature and capable of greatly reducing combustion speed and pressure intensity indexes under the condition that the combustion speed of the propellant is not increased.
Description
Technical field
The present invention relates to a kind of dimethyl glyoxime magnesium compound, this compound can be used as the combustioncatalysts of solid propellant.
Technical background
Along with the development of sophisticated technology, guided missile, the increase of rocket flight distance and the raising of control accuracy, have higher requirement to pack boronitriding, require that it is lightweight, the working hour is longer, this just requires gas generator propellant, and not only gas production rate is large, combustion gas cleanliness factor is high, and combustion is fast, combustion temperature is lower, but the performance of propelling agent is relevant, combustion temperature is low, the low combustionproperty that will certainly affect propelling agent of quick-fried heat, make propellant burning rate Pressure Exponent become large, incomplete combustion, residue increase.
In the low combustion temperature of double-basis system, low burning rate propellant; usually can delay decomposition rate by adding the higher catalyzer of fusing point, add the catalyzer of point heat of desorption reduce combustion temperature, use the relatively large composition of gas production rate and chemically thermodynamics set out control formula oxygen balance to reduce the methods such as exhaust residue, and then realize that low combustion is warm, low combustionresidue and combustion gas clean.And there are some problems, as Al in the combustioncatalysts that double-basis system gas generator propellant is commonly used
2o
3fusing point is lower, during burning easily and other catalyzer be condensed into macroparticle, be bonded at causing trouble on gas conduct pipe or turbofan; Compound containing Zr, Bi is then too hard, easily breaks turbofan.Containing magnesian double-base state, not only there is combustion flame temperature low, the advantages such as corrosion products such as low, not chloride or chlorine compound of solid content in combustion gas, and it is insensitive with impact to temperature, good mechanical property is had in wide temperature range, simultaneously also can play sound and to shake unstable combustion restraining effect adding of MgO, but the magnesium oxide being used as catalyzer is unstable, easily moisture absorption, in storage process, performance easily changes and then lost efficacy, and seriously limits the work-ing life of such propelling agent.In addition, containing water-soluble substances in propellant formulation, be also unfavorable for prepared by solvent-free pressure stretch technique.
Therefore, need badly and find a kind of itself reaction with water, long storage good security, but decomposition can produce again magnesian magnesium base combustioncatalysts, to meet the needs of novel low combustion temperature, the development of low burning rate solid propellant.
Summary of the invention
In order to solve shortcomings and deficiencies of the prior art, the invention provides a kind of dimethyl glyoxime magnesium compound and preparation method thereof.
Implementation procedure of the present invention is as follows:
Dimethyl glyoxime magnesium compound shown in structural formula (I),
The preparation method of above-mentioned dimethyl glyoxime magnesium compound, comprises the following steps:
(1) solubility magnesium salts is dissolved in wiring solution-forming in deionized water;
(2) dimethyl glyoxime highly basic is dissolved, control solution ph 9 ~ 10, then add soluble magnesium salts solution;
(3) cool after 70 DEG C ~ 90 DEG C reaction 2h ~ 4h, leave standstill;
(4) washing of precipitate, filtration, drying are obtained dimethyl glyoxime magnesium compound.
Described solubility magnesium salts is magnesium nitrate, magnesium chloride or magnesium sulfate, and highly basic is NaOH, KOH or sodium methylate.
Advantage of the present invention and positively effect: synthesis technique of the present invention is simple, synthesize the dimethyl glyoxime magnesium compound obtained and produce magnesium oxide that be evenly distributed, nascent state as main catalytic active component as decomposable asymmetric choice net during combustioncatalysts, produce auxiliary catalysis component carbon species simultaneously, can further improve the catalytic effect to low combustion temperature deflagration solid propellant.
Accompanying drawing explanation
Fig. 1 is the XRD figure of dimethyl glyoxime magnesium compound solid phase degradation production;
Fig. 2 is the combustion speed-pressure curve add dimethyl glyoxime magnesium of the present invention in composite modified double base propellant after.
Embodiment
embodiment 1the preparation of dimethyl glyoxime magnesium compound
(1) taking the dimethyl glyoxime of 34.75g (0.3mol), be scattered in 250mL deionized water, is 9 by sodium hydroxide solution regulator solution pH value; Take 76.8g (0.3mol) three nitric hydrate magnesium 100mL deionized water dissolving and be configured to solution, join in above-mentioned solution, be uniformly mixed;
(2) at 70 DEG C of constant temperature, stirring reaction 2h, then cools, leaves standstill;
(3) precipitate with deionized water repeatedly washed, filter, drying can obtain white dimethyl glyoxime magnesium compound 47.2g, productive rate 90.4%.
The sign of dimethyl glyoxime magnesium compound
1, infrared spectra (KBr, cm
-1) υ: 3208,2930,1939,1636,1445,1384,1364,1141,981,906.
2, organic element analysis
Molecular formula: C
4h
6n
2o
2mg2H
2o
Theoretical value (%): C27.54, H5.78, N16.06.
Measured value (%): C27.51, H5.68, N16.02.
3, X-ray fluorescence spectra analysis
The observed value of metal is (%): Mg13.03,
The theoretical value of metal is (%): Mg13.93.
Said structure appraising datum confirms that obtaining material is dimethyl glyoxime magnesium dihydrate.
embodiment 2the preparation of dimethyl glyoxime magnesium compound
(1) taking the dimethyl glyoxime of 1.38g (0.012mol), be scattered in 10mL deionized water, is 9 by sodium hydroxide solution regulator solution pH value; Take 3.07g (0.012mol) three nitric hydrate magnesium 10mL deionized water dissolving and be configured to solution, join in above-mentioned solution, be uniformly mixed;
(2) at 70 DEG C of constant temperature, stirring reaction 2h, then cools, leaves standstill;
(3) precipitate with deionized water repeatedly washed, filter, drying can obtain white dimethyl glyoxime magnesium compound 1.69g, productive rate 80.9%.
The solid phase degradation production of dimethyl glyoxime magnesium compound is analyzed
Dimethyl glyoxime magnesium dihydrate is placed in crucible and calcines 1 hour with 500 DEG C, obtain white powder.X-ray diffraction shows (as shown in Figure 1), five diffraction peaks 36.74,42.82,62.20,74.24 and 78.30 (111) corresponding respectively to face-centered cubic MgO, (200), (220), (311) and (222) crystal face.
The application of dimethyl glyoxime magnesium compound
Containing two methyl and two oximidos in dimethyl glyoxime structure, as can be seen from its structural analysis, the glyoxime parent of a part can with the reactive magnesium of a part, the Mg content obtained in compound is higher, be expected to the combustionproperty that effectively can regulate double-basis system solid propellant, below by way of by after composite to dimethyl glyoxime magnesium and conventional Pb-Cu salt composite catalyst, be added in composite modified double base propellant and investigate its combustion catalysis performance.
In experiment adopt the basic components of composite modified double base propellant sample to be: double-basis tackiness agent (NC+NG) 72%, Cyclotrimethylene trinitramine (RDX) 16%, functional agent 12%.Spice presses 500g batching, and catalyzer is outer dosage, and add-on is 6.6%, wherein dimethyl glyoxime magnesium compound be 3%, Pb-Cu salt composite catalyst 3%; The blank propelling agent sample of control group is not containing catalyzer.
Solid propellant sample adopts the solvent-free companding shaping technique of routine of the ripe-pressure stretch of absorptions-expelling water-put-be cut into medicinal strip to prepare.The combustion speed of sample adopts target collimation method to record.By coated for processed Φ 5mm × 150mm little powder column side polyvinyl alcohol solution dipping 6 times and dry, then carry out Burning rate testing filling in nitrogen slow-action formula Burning velometer.Test temperature is 20 DEG C, pressure range 4MPa ~ 14MPa.
In fig. 2, u is combustion speed, and p is pressure, and a is modified double base blank formula, and b is the composite modified double base propellant formula containing dimethyl glyoxime magnesium compound.As can be seen from the figure, after the dimethyl glyoxime magnesium compound that the embodiment 1 adding 3.0% prepares, increasing does not appear in propellant burning rate, and even under 12MPa and 14MPa, combustion is fast lower than blank propellant formulation; Meanwhile, reduction Pressure Exponent (n) successful containing catalyzer propelling agent is better than blank formula, and n=0.35 in 4MPa ~ 12Mpa pressure range, presents double based propellant.
In addition, composite modified double base propellant formula containing dimethyl glyoxime magnesium compound also has a feature, namely its burning rate pressure exponent is better than high pressure area (8 ~ 12MPa is 0.45) low pressure area (4 ~ 8MPa is 0.34), this feature has practicality very much, because most gasifier operating pressure is not high, is generally 4 ~ 10MPa, low pressure area Pressure Exponent is good, just adapt with the Working environment of gasifier, be conducive to gasifier smooth working, retention is stablized.
Visible, this catalyzer shows excellent combustion catalysis effect to low combustion temperature deflagration solid propellant, significantly can reduce burning rate pressure exponent while not improving propellant burning rate.
Claims (4)
1. a dimethyl glyoxime magnesium compound, is characterized in that structural formula is as shown in (I):
2. the preparation method of dimethyl glyoxime magnesium compound described in claim 1, is characterized in that comprising the following steps:
(1) solubility magnesium salts is dissolved in wiring solution-forming in deionized water;
(2) dimethyl glyoxime highly basic is dissolved, control solution ph 9 ~ 10, then add soluble magnesium salts solution;
(3) cool after 70 DEG C ~ 90 DEG C reaction 2h ~ 4h, leave standstill;
(4) washing of precipitate, filtration, drying are obtained dimethyl glyoxime magnesium compound.
3. the preparation method of dimethyl glyoxime magnesium compound according to claim 2, is characterized in that: described solubility magnesium salts is magnesium nitrate, magnesium chloride or magnesium sulfate.
4. the preparation method of dimethyl glyoxime magnesium compound according to claim 2, is characterized in that: described highly basic is NaOH, KOH or sodium methylate.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240689A (en) * | 1998-07-08 | 2000-01-12 | 中国科学技术大学 | Process for preparing superfine powder by thermolyzing metal complex |
| JP2012106236A (en) * | 2010-10-22 | 2012-06-07 | Kyushu Univ | Photo-reduction catalyst including base-metal complex and titanium dioxide |
| 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 |
-
2015
- 2015-08-19 CN CN201510511342.4A patent/CN105152969B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240689A (en) * | 1998-07-08 | 2000-01-12 | 中国科学技术大学 | Process for preparing superfine powder by thermolyzing metal complex |
| JP2012106236A (en) * | 2010-10-22 | 2012-06-07 | Kyushu Univ | Photo-reduction catalyst including base-metal complex and titanium dioxide |
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| ARRISON PHILIP G.，STOBART STEPHEN R.: "Derivatives of divalent germanium, tin, and lead.I.Protolysis of cyclopentadienyltin(II) compounds by hydroxy derivatives.Tin(II) oximes and hydroxyamines", 《JOURNAL OF THE CHEMICAL SOCIETY, DALTON TRANSACTIONS:INORGANIC CHEMISTRY》 * |
| 蔡林: "《摄影大百科辞典》", 30 September 1994, 四川科学技术出版社 * |
| 覃光明 等: "《固体推进剂装药设计》", 30 April 2013, 国防工业出版社 * |
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