CN103396281B - High nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) close cobalt (III) and preparation method thereof - Google Patents
High nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) close cobalt (III) and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of high nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) and close cobalt (III) and preparation method thereof, ion centered by cobalt (III) ion, part is the complex cation of 2 5-diazanyl tetrazolium ions and 4 hydrone composition complexes, and extraneous anion is perchlorate; Molecular formula is [Co (NH3)4(CH3N6)2]ClO4. The present invention is preferred nitrogen content as explosive part, has been designed novel high nitrogen coordination priming kind up to 84% 5-diazanyl tetrazolium (5-HT), has improved output power, has reduced mechanical sensitivity.
Description
Technical field
The present invention relates to a kind of high nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) and close cobalt (III) (letterClaim BHCP) and preparation method thereof.
Background technology
Complex is the safe insensitiveness priming of a quasi-representative, in recent decades the researcher one of domestic and international primingThe straight priming kind in this field development of new. Complex priming structure is by interior boundary and extraneous two partsComposition. The interior boundary of central ion and ligand composition complex, is called coordination ion or ligand molecule. Its structureGeneral formula is generally divided three classes:
Without extraneous complex priming: [M+2or3(R)3～4(X-1)2～3]，
The complex priming that complex cation forms: [M+2or3(R)3～5(X)0～3]Y0～2，
Complex anion complex priming: N1～4[M+2or3(R)0～5(X)1～6]。
In above-mentioned general formula:
Central ion M, affects complexes stability, is generally the transition metal ions such as Co, Ni, Cd, Cu.
Neutral ligand R, affects the basic chemical property of complex, is generally ammonia, hydrazine, guanidine etc. and has lone pair electronsSubstituent.
The explosive X ligand of anion, has reproducibility, affects the sensitivity of priming, be generally triazole tetrazolium, nitrine,Picryl and substituent.
Extraneous anion Y, has oxidisability, affects the sensitivity of priming, is generally NO3 -、ClO4 -、Cl-Deng.
Extraneous cation N, by the sensitivity of salify effects priming, is generally Na, NH4Deng alkali, alkaline earth goldBelong to.
Therefore, the performance of complex priming depend on form the central ion of complex, various part,The combination property of extraneous ion. In fact this few part functional group has formed the internal oxidation-Reduction Body of complexSystem. By structure optimization, can design sensitivity and power priming kind not etc., wherein to priming performance shadowRinging of paramount importance factor is explosive X ligand.
Several typical coordination priming at present with using value has: the perchloric acid taking 5-nitro tetrazolium as partFour ammonia two (5-nitro tetrazolium) close cobalt (III) (being called for short BNCP), molecular formula: [Co (NH3)4(CN5O2)2]ClO4；
The two-fold nitrogen of perchloric acid four ammonia taking nitrine root as part closes cobalt (III) (being called for short DACP), molecular formula:[Co(NH3)4(N3)2]ClO4；
Perchloric acid three carbohydrazides taking carbohydrazide as part close cadmium (II) (being called for short CCP), molecular formula:［Cd(NH2NHCONHNH2)3］(ClO4)2；
Nitric acid three hydrazines taking hydrazine hydrate as part close nickel (II) (being called for short NHN), molecular formula: [Ni (N2H4)3](NO3)2；
In the middle of above priming, nitrogen content is respectively: BNCP:N% is 43.14%(molecular weight 454.3); DACP:N% is 45.08%(molecular weight 310.6); CCP:N% is 9.6%(molecular weight 581.4); NHN:N% is 40.2%(molecular weight 278.8).
The molecular structure of priming be oxidation element (being mainly oxygen) with combustible element (being mainly carbon, hydrogen) by everyThe liptinite connecting from element N, therefore N is of paramount importance element in priming, N element can reduce molecular linkCan, regulate initial decomposition energy (being sensitivity). The functional group of nitrogen element composition is called explosive group, and N element is more,Explosion product number of moles of gas is more, and brisance is larger. Excellent always high nitrogen molecular structure of priming, high nitrogen canTo improve energy and the density of priming molecule.
In the middle of the complex priming of current research and development, BNCP is the priming kind that combination property is the most excellent.Its security is than good many of conventional priming lead azide, good heat resistance, and quick-fried heat, bulking value are larger, 5S bursting point362 DEG C, explosion velocity 6200m/s, is 30mg to RDX limit explosive quantity. BNCP can replace lead azide etc. to detonateMedicine is in flame, bridge silk formula detonator, particularly SCB detonator and laser initiation igniting. But through answering in recent yearsFind with test, although BNCP in small-sized detonator, can be reliable by flame, machinery, heat bridge silk equal excitation energyDetonate, but the power of detonating needs further to improve, the mechanical sensitivities such as shock, friction need further bluntHelp to change.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of high nitrogen coordination priming, there is good heat stableProperty, compare more insensitiveness of existing priming.
The technical solution adopted for the present invention to solve the technical problems is: a kind of high nitrogen coordination priming perchloric acid fourAmmonia two (5-diazanyl tetrazolium) closes cobalt (III), ion centered by cobalt (III) ion, and part is 2 5-diazanyls fourThe complex cation of oxazolinium ion and 4 hydrone composition complexes, extraneous anion is perchlorate; Molecular formula is[Co(NH3)4(CH3N6)2]ClO4, structural formula is
The present invention also provides the preparation method of above-mentioned high nitrogen coordination priming, comprises the following steps:
(1) CTCN and distilled water are fully stirred to formation suspension, the mass concentration of suspension is 5%～7%;
(2) add the rare HClO of mass concentration as 16% taking the speed of 5ml per minute4, emit CO2, CTCN withHClO4Mol ratio be 1: 2.7, now reactant liquor is without CO2Bubble formation, pH≤2 of reactant liquor;
(3) be warmed up to 80 DEG C～90 DEG C, add 5-HT, the mol ratio of CTCN and 5-HT is 1: 2.2;
(4) under constant temperature, stir, continue reaction after 2 hours, separate out yellow crystal;
(5) cool to room temperature, filters out solid product, washs solid product with ethanol, 60 DEG C ± 5 DEG C oven dry,To BHCP.
The invention has the beneficial effects as follows: the present invention is preferred nitrogen content is up to 84% 5-diazanyl tetrazolium (5-HT) conductExplosive part, has designed novel high nitrogen coordination priming kind---BHCP, has improved output power, reducesMechanical sensitivity.
It is that raw material synthesize novel high nitrogen coordination priming BHCP that the present invention adopts CTCN and 5-HT.
During BHCP is synthetic, key technology is to control the temperature of reaction, material proportion, charging sequence, reaction time and anti-Answer the pH value of liquid, the typical reaction step of the present invention's design all obtains qualified BHCP, and productive rate reaches 50.1%.
BHCP outward appearance is yellow fine crystallization body, epigranular. Particle mean size is at 2 μ m～5 μ m.
Brief description of the drawings
Fig. 1 is outward appearance and the crystal morphology figure of BHCP;
Fig. 2 is the energy spectrum analysis figure of BHCP;
Fig. 3 is the infared spectrum analysis chart of BHCP;
Fig. 4 is the 1HNMR analysis chart of BHCP;
Fig. 5 is the DSC thermal decomposition figure (10 DEG C/min of heating rate) of BHCP.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is further described, and technical scheme of the present invention includes but are not limited toFollowing embodiment.
Product embodiments:
The invention provides a kind of high nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) and close cobalt (III), with cobaltIon centered by (III) ion, part is that 2 5-diazanyl tetrazolium ions and 4 hydrones form complexesComplex cation, extraneous anion is perchlorate, its nitrogen content reaches 52.8% (molecular weight 424.5); Molecular formula is[Co(NH3)4(CH3N6)2]ClO4, structural formula is
This compound and synthetic have no so far domestic and foreign literature report, and not about the patent report of BHCP.
The present invention also provides the preparation method of above-mentioned high nitrogen coordination priming, comprises the following steps:
(1) reaction bulb is placed in to water-bath, installs mixer, temperature is taken into account temperature controller, firing equipment etc.;
(2) CTCN and distilled water are fully stirred to formation suspension, the mass concentration of suspension is 5%～7%;
(3) add rare HClO of 16% with the speed of about 5ml per minute4, emit CO2, CTCN and HClO4RubYou are than being 1: 2.7, and now reactant liquor is without CO2Bubble formation, pH≤2 of reactant liquor;
(4) bath temperature is raised to 80 DEG C～90 DEG C, progressively adds 5-HT, the mol ratio of CTCN and 5-HT with little spoonIt is 1: 2.2;
(5) under constant temperature, stir, continue reaction after 2 hours, separate out yellow crystal;
(6) cool to room temperature, filters out solid product, washs solid product with ethanol, 60 DEG C ± 5 DEG C oven dry,To BHCP.
Embodiment of the method:
Reaction equation of the present invention is:
Comprise the following steps: install the synthesizers such as stirring, water-bath, the water of the CTCN of 12g and 180ml is addedEnter in high pin beaker (CTCN suspension concentration is: 6.25%), and as reaction end liquid. Under agitation slowly drip78ml concentration is rare HClO of 16%4(the 70%HClO of 18ml4Add 60ml distilled water), emit whole CO2，PH≤2 of reactant liquor. Then by heating water bath to 80 DEG C～90 DEG C, slowly add the 5-HT of 10.2g in batches. Reaction2.0 hour. Then cooling value room temperature, filters, and distilled water, ethanol washing are dried product in 60 DEG C of water-bath baking ovens.
Synthetic technological condition is: the concentration of CTCN suspension is: 5%～7%(quality); Raw material CTCN: 5-HT:HClO4Mol ratio be 1: 2.2: 2.7, reaction temperature is 80 DEG C～90 DEG C, the reaction time is 2.0 hours, reactionPH≤2 of liquid.
According to above BHCP synthesis step and fixed process conditions, 8 batches of stable batch synthetic tests are carried out continuously.Productive rate is 45.2%～50.1%.
BHCP outward appearance: yellow fine crystallization body, epigranular. Particle mean size is at 1 μ m～3 μ m. See Fig. 1.
BHCP energy dispersion analysis of spectrum: the results are shown in Figure 2. The qualitative analysis show only exist C, N, O, Co,Cl element.
Infared spectrum: the U.S. Magna-760 of Buddhist nun's high-tensile strength company Fourier infrared spectrograph (KBr compressing tablet, sweep limits4000～400cm-1). See Fig. 3. In BNCP molecular structure, contain NO2，NO2Shuttle belt be positioned at 1546cm-1、1321cm-1. And in the molecular structure of BHCP containing NO2, NO in infared spectrum2Characteristic peak disappear.
Nuclear magnetic resonance 1H analyzes: see Fig. 4, from figure, can draw: BHCP exists the nuclear-magnetism of the H of two kinds of environment to be total toThe peak that shakes, the nuclear substituted diazanyl hydrogen of amino hydrogen and tetrazolium, ratio is 3:1. This conforms to structural formula.
DSC heat is analyzed: the U.S. Q1000 of TA company type dsc analysis instrument (N2Atmosphere, flow velocity is 20mL/min,10 DEG C/min of heating rate). The unimodal decomposition of BHCP, exothermic peak temperature is: 292.45 DEG C. Thermal decomposition is directly to decompose,Exothermic peak type is sharp-pointed, and temperature span is little, and thermal discharge is large, has significant priming exothermic characteristic.
According to 5 seconds lag phase assay methods of GJB5891.20-2006 standard, measure 5 seconds bursting points of BHCP,And contrast with BNCP, tester is BFY-II type bursting point tester.
5 seconds bursting points of table 1:BHCP
| Title | DSC decomposition peak/DEG C | 5 seconds bursting points/DEG C |
| BHCP | 293.4（10℃/min） | 325 |
| BNCP | 290.3（10℃/min） | 362 |
Through contrasting: decomposition peak, the 5 seconds bursting points of BHCP are suitable with BNCP.
With reference to GJB5891.17-2006, utilize the German Nai Chi DSC204F1 of company tester, in normal temperature～400 DEG CIn scope, under the atmosphere protection of nitrogen, select different heating rates to carry out heat analysis to noval chemical compound sample. InstituteThe data that obtain are carried out analyzing and processing by Kissinger method, calculate the activation energy of this compound. In table 2,3.
Table 2: the activation energy of the Novel detonating medicine calculating by Kissinger method
The contrast of the activation energy of table 3:BHCP and BNCP and conventional priming
| Priming | BHCP | BNCP | Powder LA | CMC-LA | |
| Activation energy/kJmol-1 | 145.8 | 180.3 | 99.40 | 129.8 |
BHCP decomposition activation energy reaches 145.8kJmol-1, be greater than conventional priming powder lead azide and CMC nitrineChange lead, there is good thermostability.
BHCP and the sense of BNCP shock are measured according to GJB772A-97 method 601.1 impact sensitivity explosion probability methodsThe contrast of degree, test condition adopts the test condition of general explosive: the quality of dropping hammer: 2.0kg, drop height 25cm, dose30mg. Test result is in table 4:
Table 4: the mechanical impacting sensitivity of (fiery explosive standard) contrast under unconfined condition
| Title | BHCP | BNCP |
| Sparking rate/% | 10（8；12） | 30（24；36） |
| Send out and count/send out | 50 | 50 |
Result shows: the obvious insensitiveness of BHCP is in BNCP.
According to GJB5891.22-2006 Loading Materials for Initiating Explosive Devices mechanical impacting sensitivity determination of test method BHCP and BNCP hitHit the contrast of sensitivity, test condition: the quality of dropping hammer: 0.8kg, the pressure of dose 20mg(39.2MPa is pressed onFire in a stove before fuel is added broad-mouthed receptacle for holding liquid). Lifting and lowering method calculates 50% ignition drop height and standard deviation. Test result is in table 5:
Table 5: the mechanical impacting sensitivity of (Loading Materials for Initiating Explosive Devices standard) contrast under constraints
| Title | BHCP | BNCP |
| 50% drop height/cm | 16.1 | 10.6 |
| σ/cm | 1.5 | 2.5 |
| Send out and count/send out | 30 | 30 |
Result shows: the obvious insensitiveness of BHCP is in BNCP.
According to GJB5891.24-2006 Loading Materials for Initiating Explosive Devices friction sensitivity determination of test method BHCP and BNCP friction senseThe contrast of degree, test condition adopts: pivot angle: 50 °; Gauge pressure: 0.64MPa, dose 20mg. Two groups (each 25)The probability of the blast of calculation sample. Test result is in table 6:
Table 6: the mechanical friction sensitivity contrast (50 °) of Loading Materials for Initiating Explosive Devices standard
| Title | BHCP | BNCP |
| Sparking rate/% | 76（68，84） | 86（80，92） |
| Send out and count/send out | 50 | 50 |
Result shows: BHCP insensitiveness is in BNCP.
Measure BHCP and BNCP is quiet according to GJB5891.27-2006 Loading Materials for Initiating Explosive Devices electrostatic spark sensitivity test methodThe contrast of spark sensitivity, lifting and lowering method calculates 50% ignition voltage and 50% firing energy. Test result is in table 7:
Table 7: the electrostatic spark sensitivity contrast of Loading Materials for Initiating Explosive Devices standard
Result shows: BHCP electrostatic spark is very low, misfire according to Loading Materials for Initiating Explosive Devices standard testing, obviously insensitiveness in BNCP。
BHCP and the sense of BNCP heated filament are measured according to GJB5891.26-2006 Loading Materials for Initiating Explosive Devices heated filament sensitivity test methodThe contrast of degree. Test condition: electrode plug is phenolic glass fiber moulding compound, strengthening cap is aluminium punching. Lifting and lowering method meterCalculate 50% firing current. Test result is in table 8:
Table 8: the hot wire sensitivity contrast of Loading Materials for Initiating Explosive Devices standard
BHCP insensitiveness is in BNCP and lead azide, but bridge silk can reliably be got angry.
According to GJB5891.25-2006 Loading Materials for Initiating Explosive Devices flame sensitivity determination of test method BHCP and the sense of BNCP flameThe contrast of degree. Test condition: black powder post (WJ636) igniting, lifting and lowering method calculates 50% and gets angry highly. Test resultIn table 9:
Table 9: the flame sensitivity contrast of Loading Materials for Initiating Explosive Devices standard
| Sample | 50% ignition height/cm | Standard deviation | Sparking rate/% under 2cm | Send out number |
| BHCP | 12.5 | 1.2 | 30 | |
| BNCP | 80%，76% | 50 |
The flame sensitivity of BHCP is sensitive to BNCP.
The invention discloses perchloric acid four ammonia two (5-diazanyl tetrazolium) and close cobalt (III) (being called for short HBCP) and system thereofPreparation Method and performance. The outward appearance of DACP is yellow fine crystallization body, and particle mean size is at 2 μ m～5 μ m. It is to pass throughNitric acid carbonic acid four cobaltammines (III) (CTCN) exist with 5-diazanyl tetrazolium (5-HT), perchloric acid (HClO4)At the temperature of 80 DEG C～90 DEG C, reaction makes. The synthesis technique of this novel high nitrogen priming is simple, pollutes few. HeatDecomposition temperature is: 292.4 DEG C～293.4 DEG C; Within 5 seconds, retardation bursting point is 325 DEG C; Shock and friction sensitivity, static senseSpend obvious insensitiveness and close cobalt (III) (being called for short BNCP) in perchloric acid four ammonia two (5-nitro tetrazolium), and flame sensitivityBe sensitive to BNCP.
Claims (1)
1. high nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) close a preparation method for cobalt (III), itsMiddle high nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium) close cobalt (III), with cobalt (III) ionCentered by ion, part is the complex cation of 2 5-diazanyl tetrazolium ions and 4 amino molecules composition complexes,Extraneous anion is perchlorate; Molecular formula is [Co (NH3)4(CH3N6)2]ClO4, structural formula is
Described method is characterized in that, comprises the steps:
(1) CTCN and distilled water are fully stirred to formation suspension, the mass concentration of suspension is 5%～7%;
(2) add the rare HClO of mass concentration as 16% taking the speed of 5ml per minute4, emit CO2, CTCN withHClO4Mol ratio be 1: 2.7, now reactant liquor is without CO2Bubble formation, pH≤2 of reactant liquor;
(3) be warmed up to 80 DEG C～90 DEG C, add 5-HT, the mol ratio of CTCN and 5-HT is 1: 2.2;
(4) under constant temperature, stir, continue reaction after 2 hours, separate out yellow crystal;
(5) cool to room temperature, filters out solid product, washs solid product with ethanol, 60 DEG C ± 5 DEG C oven dry,Close cobalt (III) to high nitrogen coordination priming perchloric acid four ammonia two (5-diazanyl tetrazolium).
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| CN107722022B (en) * | 2016-08-12 | 2020-10-02 | 西安固能新材料科技有限公司 | Compound and preparation method thereof |
| CN107056848A (en) * | 2017-06-02 | 2017-08-18 | 南京理工大学 | A kind of ammonia of priming perchloric acid four double (5 nitro tetrazoliums) closes the synthetic method of cobalt |
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