CN104592277A - Spheroidized preparation method of cuprous decahydrodecaborate tetraethylammonium - Google Patents
Spheroidized preparation method of cuprous decahydrodecaborate tetraethylammonium Download PDFInfo
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- CN104592277A CN104592277A CN201510075728.5A CN201510075728A CN104592277A CN 104592277 A CN104592277 A CN 104592277A CN 201510075728 A CN201510075728 A CN 201510075728A CN 104592277 A CN104592277 A CN 104592277A
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- Prior art keywords
- cuprous
- decahydro
- tetraethylammonium
- tetraethylammonium borate
- solvent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 title abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- WAWBMJIRULKJPO-UHFFFAOYSA-N tetraethylazanium borate Chemical compound [O-]B([O-])[O-].CC[N+](CC)(CC)CC.CC[N+](CC)(CC)CC.CC[N+](CC)(CC)CC WAWBMJIRULKJPO-UHFFFAOYSA-N 0.000 claims description 57
- BQFCCCIRTOLPEF-UHFFFAOYSA-N chembl1976978 Chemical compound CC1=CC=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 BQFCCCIRTOLPEF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 7
- 239000004449 solid propellant Substances 0.000 abstract description 4
- 239000002360 explosive Substances 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 239000008187 granular material Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- 229940063013 borate ion Drugs 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/022—Boron compounds without C-boron linkages
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a spheroidized preparation method of cuprous decahydrodecaborate tetraethylammonium. The method comprises the following steps: (1) dissolving cuprous decahydrodecaborate tetraethylammonium in 0.5-50 times of a solvent A by mass at 0-200 DEG C, wherein the solvent A is dimethylsulfoxide, N, N-dimethylformamide, acetonitrile or N-methyl-2-pyrrolidinone; (2) adding 0.5-200 times of a solvent B in mass into the solution obtained in the step (1) at 0-150 DEG C while stirring and stirring and uniformly and fully mixing, wherein the solvent B is ethanol, methanol, isopropanol, normal butanol, water and acetone; and (3) cooling the mixed system obtained in the step (2) under stirring to (-15)-50 DEG C and filtering, washing and drying to obtain the spheroidized cuprous decahydrodecaborate tetraethylammonium, wherein the length-diameter ratio reaches 1.1 and the yield reaches 95%. The method disclosed by the invention is used for spheroidized granule preparation process of cuprous decahydrodecaborate tetraethylammonium. The product as a functional fuel with a high heat value and a high burning rate is used in a solid propellant or a fuel-enriched explosive.
Description
Technical field
The present invention relates to the spheroidization preparation method that a kind of decahydro ten tetraethylammonium borate is cuprous, belong to energetic material field.
Background technology
Polyhedral boranes, owing to having the delocalization of boron cage electronics and having the chemical stability of aromaticity, resistance toheat and excellence, are applied to multiple fields such as high energy fuels, functional materials, biological medicine and catalyzer.Cuprous decahydro ten borate ion owing to containing cuprous ion and cage structure in molecule of decahydro ten tetraethylammonium borate, for both having had aluminium powder combustion catalysis function in solid propellant or fuel-air explosive, have due to high heating value again and improve the function of calorific value, because of but a kind of using value more much higher body hydroborates.But the cuprous granularity of decahydro ten tetraethylammonium borate that prior art is obtained by chemical reactive synthesis is less, and profile is irregular, mostly in styloid, length-to-diameter ratio is comparatively large, is 2-5, there is the problem such as processing performance and mechanical property variation when being applied to propellant formulation.Spheroidization crystallization can improve explosive wastewater mechanical property, processing characteristics (rheological property) and tamped density etc.Therefore, for improving the application performance of this compound, need develop its spheroidization crystallization technique.The sign of solid particulate spheroidization can adopt its length-to-diameter ratio to represent itself and spherical degree of closeness.
Document [Zhang Lun, Zhang Guomin etc., Wuhan University Journal (natural science edition) 1989,2,67-70] in disclose a kind of two tetraethyl ammonium of decahydro ten boric acid and copper chloride solution of adopting and carry out the cuprous synthetic method of Reactive Synthesis decahydro ten tetraethylammonium borate, but do not mention the spheroidization preparation method of this compound.
Summary of the invention
The technical problem to be solved in the present invention is high for the product particle length-to-diameter ratio existed in above-mentioned prior art, the deficiency that spheroidization degree is low, there is provided a kind of length-to-diameter ratio close to 1, the spheroidization preparation method of granules that decahydro ten tetraethylammonium borate that spheroidization degree is high is cuprous.
For solving the problems of the technologies described above, the spheroidization preparation method that a kind of decahydro ten tetraethylammonium borate provided by the invention is cuprous, comprises the steps:
(1) at 0 ~ 200 DEG C of temperature, be dissolved in solvent orange 2 A by cuprous for decahydro ten tetraethylammonium borate, solvent orange 2 A is methyl-sulphoxide, DMF, acetonitrile or N-Methyl pyrrolidone; Wherein, decahydro ten tetraethylammonium borate is cuprous is 1:0.5 ~ 50 with the mass ratio of solvent orange 2 A.
(2) at 0 ~ 150 DEG C of temperature, under stirring, in the solution of step (1) gained, solvent B is added; Solvent B is ethanol, methyl alcohol, Virahol, propyl carbinol, water or acetone; Wherein, decahydro ten tetraethylammonium borate is cuprous is 1:0.5 ~ 200 with the mass ratio of solvent B.
(3) under stirring, the mixing solutions of step (2) gained is cooled to-15 DEG C ~ 50 DEG C, refilters, washs, dry, decahydro ten tetraethylammonium borate obtaining spheroidization is cuprous, particle aspect ratio 1.1 ~ 1.3.
The preferred version of the spheroidization preparation method that decahydro ten tetraethylammonium borate of the present invention is cuprous, comprises the following steps:
(1) at 90 DEG C of temperature, be dissolved in acetonitrile by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate cuprous with acetonitrile mass ratio be 1:2.
(2) at 90 DEG C of temperature, add methyl alcohol under stirring in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:30 with the mass ratio of methyl alcohol.
(3) under stirring, the mixing solutions of step (2) gained is cooled to-10 DEG C, refilters, washs, dry, decahydro ten tetraethylammonium borate obtaining spheroidization is cuprous, and its median size is 100 microns, and length-to-diameter ratio is 1.1.
Invention advantage:
The cuprous spheroidization particle aspect ratio of decahydro ten tetraethylammonium borate prepared by the present invention is 1.1, and compared to existing technology, length-to-diameter ratio is the sintetics of 2 ~ 5, and spheroidization degree is higher, for in solid propellant, processing performance is good, is easy to levelling, reduces the consumption of binding agent etc.
Embodiment
The spheroidization crystallization that embodiment 1 decahydro ten tetraethylammonium borate is cuprous
(1) at 90 DEG C of temperature, be dissolved in acetonitrile by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate cuprous with acetonitrile mass ratio be 1:2.
(2) at 90 DEG C of temperature, add methyl alcohol under stirring state in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:30 with the mass ratio of methyl alcohol.
(3) carried out being cooled to-10 DEG C by the mixed system of step (2) gained under stirring state, then decahydro ten tetraethylammonium borate of carrying out filtering, washing, be drying to obtain spheroidization is cuprous, its median size is 100 microns, and length-to-diameter ratio is 1.1.
The spheroidization crystallization that embodiment 2 decahydro ten tetraethylammonium borate is cuprous
(1) at 0 DEG C of temperature, be dissolved in DMF by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate is cuprous is 1:50 with the mass ratio of DMF.
(2) at 0 DEG C of temperature, add ethanol under stirring state in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:200 with the mass ratio of ethanol.
(3) carried out being cooled to-15 DEG C by the mixed system of step (2) gained under stirring state, then decahydro ten tetraethylammonium borate of carrying out filtering, washing, be drying to obtain spheroidization is cuprous, its median size is 200 microns, and length-to-diameter ratio is 1.2.
The spheroidization crystallization that embodiment 3 decahydro ten tetraethylammonium borate is cuprous
(1) at 200 DEG C of temperature, be dissolved in methyl-sulphoxide by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate cuprous with methyl-sulphoxide mass ratio be 1:0.5.
(2) at 150 DEG C of temperature, add water under stirring state in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:0.5 with the mass ratio of water.
(3) carried out being cooled to 50 DEG C by the mixed system of step (2) gained under stirring state, then decahydro ten tetraethylammonium borate of carrying out filtering, washing, be drying to obtain spheroidization is cuprous, its median size is 50 microns, and length-to-diameter ratio is 1.2.
The spheroidization crystallization that embodiment 4 decahydro ten tetraethylammonium borate is cuprous
(1) at 50 DEG C of temperature, be dissolved in N-Methyl pyrrolidone by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate is cuprous is 1:12 with the mass ratio of N-Methyl pyrrolidone.
(2) at 50 DEG C of temperature, add Virahol under stirring state in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:50 with the mass ratio of Virahol.
(3) carried out being cooled to 0 DEG C by the mixed system of step (2) gained under stirring state, then decahydro ten tetraethylammonium borate of carrying out filtering, washing, be drying to obtain spheroidization is cuprous, its median size is 150 microns, and length-to-diameter ratio is 1.2.
The spheroidization crystallization that embodiment 5 decahydro ten tetraethylammonium borate is cuprous
(1) at 120 DEG C of temperature, be dissolved in methyl-sulphoxide by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate is cuprous is 1:1 with the mass ratio of methyl-sulphoxide.
(2) at 120 DEG C of temperature, add propyl carbinol under stirring state in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:10 with the mass ratio of propyl carbinol.
(3) carried out being cooled to 20 DEG C by the mixed system of step (2) gained under stirring state, then decahydro ten tetraethylammonium borate of carrying out filtering, washing, be drying to obtain spheroidization is cuprous, its median size is 230 microns, and length-to-diameter ratio is 1.3.
The spheroidization crystallization that embodiment 6 decahydro ten tetraethylammonium borate is cuprous
(1) at 150 DEG C of temperature, be dissolved in methyl-sulphoxide by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate is cuprous is 1:0.8 with the mass ratio of methyl-sulphoxide.
(2) at 150 DEG C of temperature, add acetone under stirring state in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:15 with the mass ratio of acetone.
(3) under stirring state, the mixed system of step (2) gained is cooled to 25 DEG C, then decahydro ten tetraethylammonium borate of carrying out filtering, washing, be drying to obtain spheroidization is cuprous, its median size is 270 microns, and length-to-diameter ratio is 1.2.
Claims (2)
1. the spheroidization preparation method that decahydro ten tetraethylammonium borate is cuprous, comprises the steps:
(1) at 0 ~ 200 DEG C of temperature, be dissolved in solvent orange 2 A by cuprous for decahydro ten tetraethylammonium borate, solvent orange 2 A is methyl-sulphoxide, DMF, acetonitrile or N-Methyl pyrrolidone; Wherein, decahydro ten tetraethylammonium borate is cuprous is 1:0.5 ~ 50 with the mass ratio of solvent orange 2 A;
(2) at 0 ~ 150 DEG C of temperature, under stirring, in the solution of step (1) gained, solvent B is added; Solvent B is ethanol, methyl alcohol, Virahol, propyl carbinol, water or acetone; Wherein, decahydro ten tetraethylammonium borate is cuprous is 1:0.5 ~ 200 with the mass ratio of solvent B;
(3) under stirring, the mixing solutions of step (2) gained is cooled to-15 DEG C ~ 50 DEG C, refilters, washs, dry, decahydro ten tetraethylammonium borate obtaining spheroidization is cuprous, particle aspect ratio 1.1 ~ 1.3.
2. the spheroidization preparation method that decahydro ten tetraethylammonium borate according to claim 1 is cuprous, comprises step as follows:
(1) at 90 DEG C of temperature, be dissolved in acetonitrile by cuprous for decahydro ten tetraethylammonium borate, wherein decahydro ten tetraethylammonium borate cuprous with acetonitrile mass ratio be 1:2;
(2) at 90 DEG C of temperature, add methyl alcohol under stirring in the solution of step (1) gained, wherein decahydro ten tetraethylammonium borate is cuprous is 1:30 with the mass ratio of methyl alcohol;
(3) under stirring, the mixing solutions of step (2) gained is cooled to-10 DEG C, refilters, washs, dry, decahydro ten tetraethylammonium borate obtaining spheroidization is cuprous, and its median size is 100 microns, and length-to-diameter ratio is 1.1.
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|---|---|---|---|
| CN201510075728.5A CN104592277B (en) | 2015-02-12 | 2015-02-12 | A kind of cuprous spheroidization preparation method of decahydro ten tetraethylammonium borate |
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| CN201510075728.5A CN104592277B (en) | 2015-02-12 | 2015-02-12 | A kind of cuprous spheroidization preparation method of decahydro ten tetraethylammonium borate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB962954A (en) * | 1961-06-30 | 1964-07-08 | Du Pont | Boron compounds |
| CN101624394A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof |
-
2015
- 2015-02-12 CN CN201510075728.5A patent/CN104592277B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB962954A (en) * | 1961-06-30 | 1964-07-08 | Du Pont | Boron compounds |
| CN101624394A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof |
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| NICHOLAS BLAGDEN等: ""Ordered Aggregation of Benzamide Crystals Induced Using a "Motif Capper" Additive"", 《CRYSTAL GROWTH & DESIGN》 * |
| 张伦 等: ""硼化合物的研究 XVII. 含Cu-H-B键的(C2H5)4NB10H10Cu和(CH3)4NB12H12Cu的合成"", 《武汉大学学报 （自然科学版）》 * |
| 欧育湘编著: "《炸药学（第1版）》", 28 February 2014, 北京理工大学出版社 * |
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| 王相元 等: ""炸药结晶晶形控制技术研究进展"", 《山西化工》 * |
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