CN108191590A - One kind boron powder containing energy and preparation method thereof - Google Patents
One kind boron powder containing energy and preparation method thereof Download PDFInfo
- Publication number
- CN108191590A CN108191590A CN201810078761.7A CN201810078761A CN108191590A CN 108191590 A CN108191590 A CN 108191590A CN 201810078761 A CN201810078761 A CN 201810078761A CN 108191590 A CN108191590 A CN 108191590A
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- CN
- China
- Prior art keywords
- boron powder
- containing energy
- boron
- organic solvent
- acidification
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- Granted
Links
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000020477 pH reduction Effects 0.000 claims abstract description 23
- 239000012948 isocyanate Substances 0.000 claims abstract description 19
- -1 tetrazole compound Chemical class 0.000 claims abstract description 16
- 239000003960 organic solvent Substances 0.000 claims abstract description 15
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 12
- 230000001588 bifunctional effect Effects 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 150000003852 triazoles Chemical class 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000004913 activation Effects 0.000 claims abstract description 3
- 238000013019 agitation Methods 0.000 claims abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 33
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 26
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 6
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 125000005442 diisocyanate group Chemical group 0.000 claims description 5
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005056 polyisocyanate Substances 0.000 claims description 5
- 229920001228 polyisocyanate Polymers 0.000 claims description 5
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 5
- 150000000177 1,2,3-triazoles Chemical class 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 239000000010 aprotic solvent Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 150000000178 1,2,4-triazoles Chemical class 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 229920000728 polyester Polymers 0.000 claims 1
- 229910052796 boron Inorganic materials 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 239000002360 explosive Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 5
- 239000004449 solid propellant Substances 0.000 abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 27
- 238000001035 drying Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000000539 dimer Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- KLSJWNVTNUYHDU-UHFFFAOYSA-N Amitrole Chemical compound NC1=NC=NN1 KLSJWNVTNUYHDU-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 150000003851 azoles Chemical class 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 150000003613 toluenes Chemical class 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- SEPPVOUBHWNCAW-FNORWQNLSA-N (E)-4-oxonon-2-enal Chemical compound CCCCCC(=O)\C=C\C=O SEPPVOUBHWNCAW-FNORWQNLSA-N 0.000 description 1
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 1
- LLBZPESJRQGYMB-UHFFFAOYSA-N 4-one Natural products O1C(C(=O)CC)CC(C)C11C2(C)CCC(C3(C)C(C(C)(CO)C(OC4C(C(O)C(O)C(COC5C(C(O)C(O)CO5)OC5C(C(OC6C(C(O)C(O)C(CO)O6)O)C(O)C(CO)O5)OC5C(C(O)C(O)C(C)O5)O)O4)O)CC3)CC3)=C3C2(C)CC1 LLBZPESJRQGYMB-UHFFFAOYSA-N 0.000 description 1
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- 125000006840 diphenylmethane group Chemical class 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- DGTNSSLYPYDJGL-UHFFFAOYSA-N phenyl isocyanate Chemical compound O=C=NC1=CC=CC=C1 DGTNSSLYPYDJGL-UHFFFAOYSA-N 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 125000003831 tetrazolyl group Chemical group 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B33/00—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide
- C06B33/08—Compositions containing particulate metal, alloy, boron, silicon, selenium or tellurium with at least one oxygen supplying material which is either a metal oxide or a salt, organic or inorganic, capable of yielding a metal oxide with a nitrated organic compound
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B27/00—Compositions containing a metal, boron, silicon, selenium or tellurium or mixtures, intercompounds or hydrides thereof, and hydrocarbons or halogenated hydrocarbons
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation methods of the boron powder containing energy, include the following steps：Step 1: acidification, boron powder is scattered in organic solvent, adds acid and carry out mechanical agitation activation, filter, is dry, obtain acidification boron powder；Step 2: isocyanates is grafted, acidification boron powder is dispersed in the organic solvent through Non-aqueous processing, adds in the compound containing difunctionality or more bifunctional isocyanate's groups, reaction is after a certain period of time, filtered, dry, obtains isocyanates grafting boron powder.Step 3: containing that can modify, isocyanates grafting boron powder is dispersed in the organic solvent through Non-aqueous processing, addition triazole or tetrazole compound, reaction is after a certain period of time, filtered, dry, obtains the boron powder containing energy.The present invention also provides one kind boron powder containing energy.The powder of the boron containing energy of the present invention has relatively low critical reaction temperature, may be used as the metal incendiary composition in explosive, solid propellant, pyrotechnic composition.
Description
Technical field
The present invention relates to a kind of energetic materials and preparation method thereof, and in particular to one kind boron powder containing energy and preparation method thereof,
It is with a wide range of applications in various explosives, solid propellant, pyrotechnic composition.
Background technology
Modern war proposes increasingly higher demands to weapon system, realizes the high-energy of weapons and ammunitions and efficiently injures
Effect, which becomes, is primarily upon one of focus, and it is Major Technology to improve the energy of energetic material and energy utilization efficiency.
It is common mode using high activity metal incendiary agent in explosive, solid propellant, pyrotechnic composition.In various metal incendiary compositions,
The unit mass combustion heat of boron is 1.9 times of aluminium, and volume calorific value is 1.66 times of aluminium, has splendid application prospect.
Although boron has higher combustion heat value, its fusing point, boiling point higher (boron fusing point 2350K, boiling point
4200K), and boron particles surface easily forms fine and close higher boiling oxidation film (boron oxide fusing point 723K, boiling point 2133K), isolation
Contact of the incendiary agent with oxidant not only hinders the igniting (boron firing temperature 1900K~2500K) of incendiary agent, is also unfavorable for
The self-holding progress of combustion reaction, this causes the ignition performance of boron very undesirable, and energy utilization efficiency reaches far away theoretical
Reaction calorific value.The burning of boron powder and aluminium powder has approximate characteristic, but ignition condition is more harsh.Therefore how to improve boron
Ignition performance, become one of the critical issue for improving composite explosives energy utilization efficiency, the relevant technologies are for improving
The ignition performance of aluminium, which also has, promotes reference value.
The method for improving the metallic particles ignition performances such as boron element at present mainly has：(a) the unformed boron powder of fine,
Increasing specific surface area reduces critical reaction temperature；(b) cladding energetic material release heat improves the surface temperature of boron particles, example
Such as AP, glycidol azide polyethers (GAP), BAMO, potassium hyperchlorate, NaN3, perfluorinated aliphatic acid etc.；(c) covering material chemistry is anti-
The oxidation film of particle surface, such as LiF, Viton A, silane etc. should be removed；(d) surface cladding combustible material and boron particles are anti-
Low ignition point compound should be generated, such as magnesium, titanium, zirconium can generate low ignition point metal boride with boron；(e) combustion catalysis is added
Agent, such as the metal powder of lithium, magnesium, titanium, zirconium, lead, copper, iron, chromium, bismuth, tin, oxide, salt and complex etc..
Invention content
The purpose of the present invention is to provide one kind boron powder containing energy and preparation method thereof.
The invention is realized in this way：
A kind of preparation method of the boron powder containing energy, includes the following steps：
Step 1: acidification
Boron powder is scattered in organic solvent, acid is added and carries out mechanical agitation activation, the sour mass ratio with boron powder is 1/100
It is filtered after~1/5,10~30 hours, is dry, obtaining acidification boron powder；
Organic solvent can be that acetone, acetonitrile, tetrahydrofuran, N,N-dimethylformamide, dimethyl sulfoxide (DMSO) etc. are non-proton
One kind of solvent, acid can be sulfuric acid, hydrochloric acid and nitric acid.
Step 2: isocyanates is grafted
Acidification boron powder is dispersed in the organic solvent through Non-aqueous processing, is added in containing difunctionality or more Bifunctional phenyliso cyanic acid
The compound of ester group, isocyanate compound are 1/20~1/2 with acidification boron powder mass ratio, and room temperature~70 DEG C are stirred to react one
It is filtered, dry after fixing time, obtain isocyanates grafting boron powder.
Organic solvent can be acetone, acetonitrile, tetrahydrofuran, N,N-dimethylformamide, dimethyl sulfoxide (DMSO), benzene, toluene,
One kind of the aprotic solvent such as ethyl acetate, the compound containing difunctionality or more bifunctional isocyanate's groups are different for toluene two
Cyanate (TDI), isophorone diisocyanate (IPDI), diphenyl-methane -4,4 '-diisocyanate (MDI), dimer (fatty acid) yl
One in diisocyanate (DDI), hexamethylene diisocyanate (HDI), poly methylene poly phenyl poly isocyanate (PAPI)
Kind, the reaction time is 5~24 hours.
Step 3: containing that can modify
Isocyanates grafting boron powder is dispersed in the organic solvent through Non-aqueous processing, adds in triazole or four azole chemical combination
Object, azole compounds are 1/10~3/10 with isocyanates grafting boron powder mass ratio, and room temperature~70 DEG C are stirred to react certain time
Afterwards, it is filtered, dry, obtain the boron powder containing energy.
Organic solvent can be acetone, acetonitrile, tetrahydrofuran, N,N-dimethylformamide, dimethyl sulfoxide (DMSO), benzene, toluene,
One kind of the aprotic solvent such as ethyl acetate, triazole or tetrazole compound for 1,2,3-triazoles, 1,2,4- triazoles, 3- amino-
1,2,4- triazoles, 3- methyl-1s, 2,4- triazoles, 1,2,3,4- tetrazoliums, 5- amino -1,2,3,4- tetrazoliums, 5- nitros -1,2,3,4-
One kind in tetrazolium, reaction time are 5~24 hours.
It is another object of the present invention to provide a kind of boron powder containing energy.
One kind boron powder containing energy is that the preparation method of the boron powder provided by the present invention containing energy is prepared, and with as follows
Structure：
Using pure boron powder particles as core, to contain the compound of difunctionality or more bifunctional isocyanate's groups as company
Connect molecule；Using triazole or tetrazole compound as the molecule containing energy.
The boron powder containing energy prepared using the method for the present invention, is had relatively low critical reaction temperature, may be used as explosive, solid
Metal incendiary composition in propellant, pyrotechnic composition.
Description of the drawings
Fig. 1 is the boron powder structure diagram containing energy.
Specific embodiment
It is the specific example of several application technical solution of the present invention below, they are only provided as an example, are not intended as to this
The application limitation of invention.All operating conditions, the equivalent replacement of material composition and ratio or equivalent exchange, the protection in the present invention
Within the scope of.
A kind of boron powder containing energy provided in an embodiment of the present invention, as shown in Figure 1, the boron powder of the present invention containing energy, with list
Matter boron powder particles are core, can be with to contain the compound A of difunctionality or more bifunctional isocyanate's groups as connection molecule
Be toluene di-isocyanate(TDI) (TDI), isophorone diisocyanate (IPDI), diphenyl-methane -4,4 '-diisocyanate (MDI),
Dimer (fatty acid) yl diisocyanate (DDI), hexamethylene diisocyanate (HDI), poly methylene poly phenyl poly isocyanate
(PAPI)；Using triazole or tetrazole compound B as containing can molecule, can be 1,2,3-triazoles, 1,2,4- triazoles, 3- amino -1,
2,4- triazoles, 3- methyl-1s, 2,4- triazoles, 1,2,3,4- tetrazoliums, 5- amino -1,2,3,4- tetrazoliums, 5- nitros -1,2,3,4- four
Azoles.
With the embodiment of several specific preparation methods, the present invention is further illustrated below.
Embodiment 1：
5.0g boron powder is dispersed in 100mL acetone, 0.5g nitric acid (mass fraction 65~68%) is added dropwise, is stirred at room temperature
10h, filtering, drying obtain acidification boron powder.Acidification boron powder, 1.8g toluene di-isocyanate(TDI)s are added to 100mL dry toluenes
In, 70 DEG C are stirred to react 10h, and filtration drying obtains toluene di-isocyanate(TDI) grafting boron powder, is then dispersed in the anhydrous N of 50mL, N-
In dimethylformamide, 1.0g 1,2,3-triazoles is added in, 50 DEG C are stirred to react 10h, and filtering, drying obtain about 5.2g boron containing energy
Powder.
Embodiment 2：
10.0g boron powder is dispersed in 200mL acetone, 1.0g hydrochloric acid (mass fraction 35~37%) is added dropwise, is stirred at room temperature
15h, filtering, drying obtain acidification boron powder.Acidification boron powder, 4.5g isophorone diisocyanate are added to the anhydrous second of 200mL
In nitrile, 70 DEG C are stirred to react 20h, and filtration drying obtains isophorone diisocyanate grafting boron powder, be then dispersed in 100mL without
In water-acetonitrile, 1,2,4- triazole of 2.0g 3- amino is added in, 70 DEG C are stirred to react 10h, and filtering, drying obtain about 11.3g containing energy
Boron powder.
Embodiment 3：
5.0g boron powder is dispersed in 100mL tetrahydrofurans, 0.5g sulfuric acid (mass fraction 30%) is added dropwise, is stirred at room temperature
10h, filtering, drying obtain acidification boron powder.Acidification boron powder, 2.5g diphenyl-methanes -4,4 '-diisocyanate are added to 100mL
In anhydrous propanone, reaction 15h is stirred at room temperature, filtration drying obtains diphenyl-methane -4, and 4 '-diisocyanate is grafted boron powder, then
It is dispersed in 100mL anhydrous propanones, adds in 1,2,3,4- tetrazoliums of 0.7g, reaction 10h is stirred at room temperature, filtering, drying obtain about
5.5g boron powder containing energy.
Embodiment 4：
20.0g boron powder is dispersed in 200mL acetone, 1.8g nitric acid (mass fraction 65~68%) is added dropwise, is stirred at room temperature
For 24 hours, it filters, is dry, obtaining acidification boron powder.Acidification boron powder, 3.7g toluene di-isocyanate(TDI)s are added to 200mL dry toluenes
In, 40 DEG C are stirred to react 20h, and filtration drying obtains toluene di-isocyanate(TDI) grafting boron powder, is then dispersed in 100mL anhydrous dimethyls
In base sulfoxide, 3.0g 5- amino -1,2 is added in, 3,4- tetrazoliums, 40 DEG C are stirred to react 10h, and filtering, drying obtain about 22.0g and contain
It can boron powder.
Embodiment 5：
5.0g boron powder is dispersed in 100mL acetonitriles, 1.0g hydrochloric acid (mass fraction 35~37%) is added dropwise, is stirred at room temperature
20h, filtering, drying obtain acidification boron powder.Will acidification boron powder, that 5.5g dimer (fatty acid) yl diisocyanates are added to 100mL is anhydrous
In toluene, 60 DEG C are stirred to react 10h, and filtration drying obtains dimer (fatty acid) yl diisocyanate grafting boron powder, is then dispersed in
In 50mL anhydrous dimethyl sulphoxides, 1.0g 5- nitros -1,2 are added in, 3,4- tetrazoliums, 60 DEG C are stirred to react 20h, filter, is dry,
Obtain about 6.5g boron powder containing energy.
Embodiment 6：
10.0g boron powder is dispersed in 100mL acetone, 2.0g sulfuric acid (mass fraction 30%) is added dropwise, is stirred at room temperature for 24 hours,
Filtering, drying obtain acidification boron powder.Will acidification boron powder, that 4.0g poly methylene poly phenyl poly isocyanates are added to 100mL is anhydrous
In benzene, 40 DEG C are stirred to react 10h, and filtration drying obtains poly methylene poly phenyl poly isocyanate grafting boron powder, is then dispersed in
In 100mL anhydrous dimethyl sulphoxides, 1.0g 5- nitros -1,2 are added in, 3,4- tetrazoliums, 40 DEG C are stirred to react 20h, filter, is dry,
Obtain about 12.5g boron powder containing energy.
The above-mentioned 6 groups powder of the boron containing energy are applied to pyrotechnic composition B/KNO3Instead of common boron powder, tested through differential scanning calorimetry anti-
Temperature is answered, the results are shown in Table 1, makes pyrotechnic composition B/KNO using the boron powder containing energy3Critical reaction temperature shifts to an earlier date 10~30 DEG C.
Pyrotechnic composition B/KNO before and after the application of table 1 boron powder containing energy3Reaction temperature
| Boron powder/potassium nitrate mass ratio | Boron powder | Reaction temperature/DEG C |
| 1/9 | Common boron powder | 570 |
| 1/9 | Embodiment 1 | 548 |
| 2/8 | Common boron powder | 540 |
| 2/8 | Embodiment 2 | 523 |
| 3/7 | Common boron powder | 537 |
| 3/7 | Embodiment 3 | 517 |
| 3/7 | Embodiment 4 | 525 |
| 3/7 | Embodiment 5 | 507 |
| 5/5 | Common boron powder | 510 |
| 5/5 | Embodiment 6 | 491 |
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiments of the present invention are simultaneously not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modifications and embodiment, these modifications and embodiment will be fallen in principle disclosed in the present application
Within scope and spirit.
Claims (5)
1. a kind of preparation method of the boron powder containing energy, it is characterised in that include the following steps：
Step 1: acidification
Boron powder is scattered in organic solvent, acid is added and carries out mechanical agitation activation, the sour mass ratio with boron powder is 1/100~1/
It is filtered after 5,10~30 hours, is dry, obtaining acidification boron powder；
Step 2: isocyanates is grafted
Acidification boron powder is dispersed in the organic solvent through Non-aqueous processing, is added in containing difunctionality or more bifunctional isocyanate's bases
The compound of group, isocyanate compound are 1/20~1/2 with acidification boron powder mass ratio, and room temperature~70 DEG C are stirred to react a timing
Between after, it is filtered, dry, obtain isocyanates grafting boron powder；
Step 3: containing that can modify
Isocyanates grafting boron powder is dispersed in the organic solvent through Non-aqueous processing, adds in triazole or tetrazole compound, azoles
Class compound is 1/10~3/10 with isocyanates grafting boron powder mass ratio, and room temperature~70 DEG C are stirred to react after a certain period of time, warp
Filtering, dry, acquisition boron powder containing energy.
2. the preparation method of the boron powder containing energy according to claim 1, it is characterised in that：
In step 1, organic solvent is that acetone, acetonitrile, tetrahydrofuran, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO) etc. are non-proton
One kind of solvent, acid are one kind in sulfuric acid, hydrochloric acid and nitric acid.
3. the preparation method of the boron powder containing energy according to claim 1, it is characterised in that：
In step 2, organic solvent is acetone, acetonitrile, tetrahydrofuran, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO), benzene, first
One kind of the aprotic solvent such as benzene, ethyl acetate, the compound containing difunctionality or more bifunctional isocyanate's groups are toluene
Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenyl-methane -4,4 '-diisocyanate (MDI), two polyesters
In fat acid diisocyanate (DDI), hexamethylene diisocyanate (HDI), poly methylene poly phenyl poly isocyanate (PAPI)
One kind, the reaction time be 5~24 hours.
4. the preparation method of the boron powder containing energy according to claim 1, it is characterised in that：
In step 3, organic solvent is acetone, acetonitrile, tetrahydrofuran, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO), benzene, first
One kind of the aprotic solvent such as benzene, ethyl acetate, triazole or tetrazole compound are 1,2,3-triazoles, 1,2,4- triazoles, 3- ammonia
Base -1,2,4- triazoles, 3- methyl-1s, 2,4- triazoles, 1,2,3,4- tetrazoliums, 5- amino -1,2,3,4- tetrazoliums, 5- nitro -1,2,
One kind in 3,4- tetrazoliums, reaction time are 5~24 hours.
5. one kind boron powder containing energy, it is characterised in that：It is the preparation of the boron powder containing energy as described in Claims 1-4 any claim
What method was prepared, and have the following structure：
Using pure boron powder particles as core, divided using the compound for containing difunctionality or more bifunctional isocyanate's groups as connection
Son；Using triazole or tetrazole compound as the molecule containing energy.
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