CN105001093A - Method for purifying hexanitrostibene - Google Patents
Method for purifying hexanitrostibene Download PDFInfo
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- CN105001093A CN105001093A CN201510379994.7A CN201510379994A CN105001093A CN 105001093 A CN105001093 A CN 105001093A CN 201510379994 A CN201510379994 A CN 201510379994A CN 105001093 A CN105001093 A CN 105001093A
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Abstract
The invention discloses a method for purifying hexanitrostibene, and the method comprises the following steps: (1) carrying out an oxidation treatment for HNS crude product by using a 20%-50% hydrogen peroxide polar solvent, wherein, the mass of the polar solvent is 10-15 times the mass of the HNS crude product, and removing water-soluble impurities, and the oxidation treatment temperature is 40-50 DEG C; (2) carrying out a purifying treatment for a filter cake obtained in the first step by using aacetone-ethanol nonpolar-polar mixed solvent, whose mass is 8-12 times the mass of the HNS crude product, and removing organic impurities, wherein, the purifying treatment temperature is 50-55 DEG C; (3) carrying out a recrystallization for a substance obtained through filtration in the step (2) by using dimethyl formamide-dimethyl sulphoxide mixed solvent, whose mass is 12-15 times the mass of the HNS crude product, in a condition that the temperature rises to 60-70 DEG C, and then slowly falls to 50 DEG C +-2.5 DEG C, and repeating the process for 6-10 times; (4) finally, carrying out filtration and drying after the temperature slowly falls to the room temperature and obtaining the HNS product. According to the invention, the method containing the polar solvent oxidation treatment, the polar-nonpolar mixed solvent purifying treatment, and the special-purpose mixed solvent high-low temperature disturbance recrystallization treatment is carried out for the HNS crude product, and the high quality HNS product is obtained.
Description
Technical field
The present invention relates to a kind of purification process of heat-resisting single chmical compound explosive hexanitro-stilbene, belong to explosive preparation field.
Background technology
Hexanitro-stilbene (HNS) is a kind of high temperature powder of excellent property, has excellent detonating and explosion transfer performance, is applicable to high/low temperature and the vacuum environment of-200 ~ 250 DEG C.Hexanitro-stilbene is usually used in manufacturing heat-resistant flexible primacord fuse, flexible linear shaped charge and high temperature powder powder charge, for heat-resisting Loading Materials for Initiating Explosive Devices and booster explosive powder charge, is applied in aerospace, subsurface investigation exploitation; And HNS also can be used as the crystal habit modifying agent casting dress tritonal (TNT), to improve the mechanical property of powder charge, reduce the end gap occurred in casting dress heavy caliber ammunition, improve emission security.
HNS is due to its high temperature (+300 DEG C) and the operating characteristic of low temperature (-200 DEG C) and the consistency with tetrafluoroethylene, Bulk plastic bonded explosive (PBX) powder charge of Apollo moonscape test assembly in the senior Apollo system for U.S. NASA can be made, be used for detecting the seismic wave that causes of moonscape.The main body explosive loading of high temperature, ultrahigh-temperature petroleum perforation charge is HNS both at home and abroad at present.
Another very important purposes of HNS manufactures crystallization TNT with it.The essence of crystallization TNT is the TNT pyrotechnic composition containing a small amount of HNS in it.Nineteen sixty-eight Sweden Bofors company first invention crystallization TNT, adds a small amount of HNS and suppresses it excessively cold as nucleator, thus obtain the powder charge of fine structure high-quality in TNT.Research shows: crystallization TNT is not the simple mixtures of TNT and HNS, and wherein part HNS is with title complex (TNT)
2hNS form exists, and this title complex plays nucleator and crystal formation modifying agent.HNS is melted in TNT and forms a large amount of nucleus because its fusing point is very high, makes TNT be frozen into the fine crystals of lack of alignment.
It is on the high side to there is impurity in the universal method products obtained therefrom of the HNS of domestic and international manufacture, and fusing point is low, and tap density is little, batch quality conformance difference, the quality problems such as free-running property is not good.
Summary of the invention
The object of this invention is to provide a kind of purification process of hexanitro-stilbene, obtain high-quality HNS product, the fusing point solving product existence is in the past low, and tap density is little, batch quality conformance difference, the quality problems such as free-running property is not good.
The technical solution realizing the object of the invention is: a kind of purification process of hexanitro-stilbene, comprises the steps:
(1) hydrogen peroxide (H of HNS crude product quality 10-15 20%-50% is doubly adopted
2o
2) polar solvent carries out oxide treatment to HNS crude product, removing water-soluble impurity, its oxidation temperature is 40-50 DEG C;
(2) by the filtration filter cake of (1) step, adopt-polarized mixed solvent nonpolar with HNS crude product quality 8-12 acetone-ethanol doubly, carry out purification process, removing organic impurity, purification process temperature is 50-55 DEG C;
(3) by the filtrate of (2) step, adopt and HNS crude product quality 12-15 dimethyl formamide-methyl-sulphoxide mixed solvent doubly, carry out recrystallization, be first warmed up to 60-70 DEG C, after be slowly cooled to 50 ± 2.5 DEG C, this process circulates 6-10 time repeatedly;
(4) be finally slowly cooled to room temperature, filter, dry, obtain HNS product.
In step (1), oxidation treatment time is 1-2h.
In step (2), acetone-ethanol is nonpolar-polarized mixed solvent in the mass ratio of acetone and ethanol be 0.8-1:1; The purification process time is 1-2h.
In step (3), in dimethyl formamide-methyl-sulphoxide mixed solvent, dimethyl formamide and methyl-sulphoxide mass ratio are 0.7-0.85:0.15-0.3.
Compared with prior art, advantage of the present invention is:
(1) by carrying out the method for polar solvent oxide treatment, polar-nonpolar mixed solvent purification process and the process of special mixed solvent high/low temperature disturbance recrystallization to HNS crude product, obtain high-quality HNS product, its fusing point reaches 317-318 DEG C; Purity more than 99.5%; Tap density improves 20%-30%, reaches 0.60-0.75g/cm3.
(2) product particle is evenly distributed, smooth surface, and free-running property improves 30%-45%.
(3) quality product consistence is obviously improved.
Embodiment
First, adopt the hydrogen peroxide polar solvent oxide treatment of HNS crude product quality 10-15 30%-50% doubly, removing water-soluble impurity, its oxidation temperature 40-50 DEG C, oxidization time 1-2h; Second step, by the filtration filter cake of the first step, adopts and HNS quality 8-12 acetone-ethanol (mass ratio 0.8-1:1) nonpolar-polarized mixed solvent doubly, carry out purification process, removing organic impurity, purification process temperature 50-55 DEG C, purification process time 1-2h; 3rd step, by the filtrate of second step, adopt HNS quality 12-15 special dimethyl formamide-methyl-sulphoxide mixed solvent (mass ratio 0.7-0.85:0.15-0.3) doubly, the method for close limit high/low temperature disturbance recrystallization process, during recrystallization process, first be warming up to 60-70 DEG C, slowly be cooled to 50 ± 2.5 DEG C again, this cooling, temperature-rise period carries out its objective is disturbance recrystallization process for 6-10 time in turn, smooth even with particle size distribution of promotion HNS particle surface; 4th step, is finally slowly cooled to room temperature, filters, dry, obtains high-quality HNS product.
After above-mentioned process, obtain high-quality HNS product, the fusing point solving product existence is in the past low, and tap density is little, batch quality conformance difference, the quality problems that free-running property is not good.
Example 1 prepares 10g level HNS
Adopt the hydrogen peroxide (H of 100ml 50%
2o
2) polar solvent oxide treatment, oxidation temperature 40 DEG C, oxidization time 1h; Second step, by the filtration filter cake of the first step, adopts the mixed solvent of 40ml acetone-40ml ethanol composition, carries out purification process, purification process temperature 55 DEG C, purification process time 1h; 3rd step, by the filtrate of second step, 60ml dimethyl formamide-40ml methyl-sulphoxide mixed solvent is adopted to carry out recrystallization process, treatment temp 70 DEG C, slowly be cooled to 50 DEG C, within the scope of 50 ± 2.5 DEG C, carry out the disturbance of lowering the temperature, the 6 next round streams that heat up carry out, promote smooth even with particle size distribution of HNS particle surface; 4th step, is finally slowly cooled to room temperature, filters, dry, obtains high-quality HNS product.
Implementation result: its fusing point 317-318 DEG C; Purity 99.7%; Tap density; 0.69g/cm
3; Product particle is evenly distributed, smooth surface, and free-running property improves 38%.
Example 2 prepares 100g level HNS
Adopt the hydrogen peroxide (H of 1000ml40%
2o
2) polar solvent oxide treatment, oxidation temperature 50 DEG C, oxidization time 1h; Second step, by the filtration filter cake of the first step, adopts the mixed solvent of 400ml acetone-400ml ethanol composition, carries out purification process, purification process temperature 55 DEG C, purification process time 1h; 3rd step, by the filtrate of second step, 600ml dimethyl formamide-400ml methyl-sulphoxide mixed solvent is adopted to carry out recrystallization process, treatment temp 70 DEG C, slowly be cooled to 50 DEG C, within the scope of 50 ± 2.5 DEG C, carry out the disturbance of lowering the temperature, the 10 next round streams that heat up carry out, promote smooth even with particle size distribution of HNS particle surface; 4th step, is finally slowly cooled to room temperature, filters, dry, obtains high-quality HNS product.
Implementation result: its fusing point 317-318 DEG C; Purity 99.7%; Tap density 0.72g/cm3; Product particle is evenly distributed, smooth surface, and free-running property improves 41%.
Example 3 prepares 100g level HNS
Adopt the hydrogen peroxide (H of 1100ml 30%
2o
2) polar solvent oxide treatment, oxidation temperature 50 DEG C, oxidization time 1.5h; Second step, by the filtration filter cake of the first step, adopts the mixed solvent of 500ml acetone-300ml ethanol composition, carries out purification process, purification process temperature 50 C, purification process time 1h; 3rd step, by the filtrate of second step, 650ml dimethyl formamide-350ml methyl-sulphoxide mixed solvent is adopted to carry out recrystallization process, treatment temp 70 DEG C, slowly be cooled to 50 DEG C, within the scope of 50 ± 2.5 DEG C, carry out the disturbance of lowering the temperature, the 8 next round streams that heat up carry out, promote smooth even with particle size distribution of HNS particle surface; 4th step, is finally slowly cooled to room temperature, filters, dry, obtains high-quality HNS product.
Implementation result: fusing point 317-318 DEG C; Purity 99.6%; Tap density 0.73g/cm3; Product particle is evenly distributed, smooth surface, and free-running property improves 45%.
Example 4 is prepared with the high-quality of 1kg level HNS
Adopt the hydrogen peroxide (H of 15L 30%
2o
2) polar solvent oxide treatment, oxidation temperature 50 DEG C, oxidization time 2h; Second step, by the filtration filter cake of the first step, adopts the mixed solvent of 4L acetone-4L ethanol composition, carries out purification process, purification process temperature 55 DEG C, purification process time 2h; 3rd step, by the filtrate of second step, 8L dimethyl formamide-2L methyl-sulphoxide mixed solvent is adopted to carry out recrystallization process, treatment temp 70 DEG C, slowly be cooled to 50 DEG C, within the scope of 50 ± 2.5 DEG C, carry out the disturbance of lowering the temperature, the 8 next round streams that heat up carry out, promote smooth even with particle size distribution of HNS particle surface; 4th step, is finally slowly cooled to room temperature, filters, dry, obtains high-quality HNS product.
Implementation result: fusing point reaches 317-318 DEG C; Purity 99.7%; Tap density 0.72g/cm3; Product particle is evenly distributed, smooth surface, and free-running property improves 41%.
Claims (4)
1. a purification process for hexanitro-stilbene, is characterized in that, comprises the steps:
(1) adopt the hydrogen peroxide polar solvent of HNS crude product quality 10-15 20%-50% doubly to carry out oxide treatment to HNS crude product, removing water-soluble impurity, its oxidation temperature is 40-50 DEG C;
(2) by the filtration filter cake of (1) step, adopt-polarized mixed solvent nonpolar with HNS crude product quality 8-12 acetone-ethanol doubly, carry out purification process, removing organic impurity, purification process temperature is 50-55 DEG C;
(3) by the filtrate of (2) step, adopt and HNS crude product quality 12-15 dimethyl formamide-methyl-sulphoxide mixed solvent doubly, carry out recrystallization, be first warmed up to 60-70 DEG C, after be slowly cooled to 50 ± 2.5 DEG C, this process circulates 6-10 time repeatedly;
(4) be finally slowly cooled to room temperature, filter, dry, obtain HNS product.
2. the purification process of hexanitro-stilbene as claimed in claim 1, it is characterized in that, in step (1), oxidation treatment time is 1-2h.
3. the purification process of hexanitro-stilbene as claimed in claim 1, is characterized in that, in step (2), acetone-ethanol is nonpolar-polarized mixed solvent in the mass ratio of acetone and ethanol be 0.8-1:1; The purification process time is 1-2h.
4. the purification process of hexanitro-stilbene as claimed in claim 1, it is characterized in that, in step (3), in dimethyl formamide-methyl-sulphoxide mixed solvent, dimethyl formamide and methyl-sulphoxide mass ratio are 0.7-0.85:0.15-0.3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510379994.7A CN105001093A (en) | 2015-07-01 | 2015-07-01 | Method for purifying hexanitrostibene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859561A (en) * | 2016-04-28 | 2016-08-17 | 刘更力 | Crystallization process of needle-like 2,4-dinitrotoluene crystals |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0132990A2 (en) * | 1983-07-22 | 1985-02-13 | The Secretary of State for Defence in Her Britannic Majesty's Government of the United Kingdom of Great Britain and | Production of hexanitrostilbene (HNS) |
-
2015
- 2015-07-01 CN CN201510379994.7A patent/CN105001093A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0132990A2 (en) * | 1983-07-22 | 1985-02-13 | The Secretary of State for Defence in Her Britannic Majesty's Government of the United Kingdom of Great Britain and | Production of hexanitrostilbene (HNS) |
Non-Patent Citations (2)
| Title |
|---|
| 盛涤伦 等: "高纯高比表面积HNS的研究", 《火工品》 * |
| 陆明 等: "六硝基芪合成新方法", 《南京理工大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859561A (en) * | 2016-04-28 | 2016-08-17 | 刘更力 | Crystallization process of needle-like 2,4-dinitrotoluene crystals |
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Application publication date: 20151028 |