CN117886765A - Ultrasonic-assisted NTO crystallization granulation method - Google Patents
Ultrasonic-assisted NTO crystallization granulation method Download PDFInfo
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- CN117886765A CN117886765A CN202410018599.5A CN202410018599A CN117886765A CN 117886765 A CN117886765 A CN 117886765A CN 202410018599 A CN202410018599 A CN 202410018599A CN 117886765 A CN117886765 A CN 117886765A
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 45
- 230000008025 crystallization Effects 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000005469 granulation Methods 0.000 title claims abstract description 22
- 230000003179 granulation Effects 0.000 title claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 58
- 238000003756 stirring Methods 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000012296 anti-solvent Substances 0.000 claims abstract description 20
- 239000012047 saturated solution Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000012798 spherical particle Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 9
- 230000002572 peristaltic effect Effects 0.000 claims description 9
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 26
- 239000002360 explosive Substances 0.000 abstract description 13
- 230000009471 action Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 abstract description 2
- 238000010008 shearing Methods 0.000 abstract description 2
- 230000008878 coupling Effects 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- QJTIRVUEVSKJTK-UHFFFAOYSA-N 5-nitro-1,2-dihydro-1,2,4-triazol-3-one Chemical compound [O-][N+](=O)C1=NC(=O)NN1 QJTIRVUEVSKJTK-UHFFFAOYSA-N 0.000 description 61
- 238000002604 ultrasonography Methods 0.000 description 15
- 239000002994 raw material Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
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- 238000004581 coalescence Methods 0.000 description 2
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- 238000009472 formulation Methods 0.000 description 2
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- 239000012046 mixed solvent Substances 0.000 description 2
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- 230000008569 process Effects 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- -1 1,3, 5-triamino-2, 4, 6-trinitroNitrobenzene Chemical compound 0.000 description 1
- 238000007441 Spherical agglomeration method Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- 239000003380 propellant Substances 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an ultrasonic-assisted NTO crystallization granulation method, which comprises the following steps: (1) dissolving NTO in a solvent to prepare an NTO saturated solution; (2) Adding an antisolvent and a bridging agent into a crystallization reaction kettle, and stirring to uniformly disperse the bridging agent in the antisolvent to obtain a bridging agent-antisolvent system; (3) Dropping the NTO saturated solution into a bridging agent-antisolvent system under stirring, and simultaneously performing ultrasonic treatment to form oil-in-water (O/W) microemulsion, and separating out NTO; (4) Stopping ultrasonic treatment, continuing stirring, and agglomerating NTO monocrystal particles into spherical particles under the action of a shearing flow field; and (5) filtering, washing and drying to obtain NTO spherical particles. In the invention, the ultrasonic and antisolvent coupling crystallization is used for matching with the bridging agent to bond the ultrasonic fusion crystal to prepare large-particle spherical NTO explosive particles with different sizes, the surfaces of the prepared NTO spherical particles have no sharp edges and corners and are smooth, and the sphericity is as high as 90-93%.
Description
Technical Field
The invention belongs to the technical field of energetic material preparation, and particularly relates to an ultrasonic-assisted NTO crystallization granulation method.
Background
3-nitro-1, 2, 4-triazole-5-one (NTO) plays an important role in the field of energetic materials, and has a density of up to 1.93g/cm 3 Detonation energy is equivalent to that of cyclotrimethyltrinitro (RDX), and sensitivity is equivalent to that of 1,3, 5-triamino-2, 4, 6-trinitroNitrobenzene (TATB) is similar, the synthesis is simple, the price is low, and the explosive is an insensitive explosive with great application potential. However, directly synthesized NTO is mostly in a zigzag shape or an irregular rod shape, has particle size distribution of tens to hundreds of micrometers, has low crystal quality, relatively high sensitivity and poor powder processability, and limits the application of the NTO in explosive formulations and propellants.
Researches show that the spherical explosive particles have the advantages of small edges and corners, good flowability and strong processability, so that the probability of forming hot spots by friction and impact is extremely low, the safety performance is high, the density of the explosive is increased, the mechanical properties of processing and formulation are improved, the energy output of the explosive is optimized, and the combustion and detonation performance of the explosive are improved. Thus, the regulation of the morphology of NTO particles has been a focus of attention. For example, patent CN201510673200.8 discloses a high crystal density spherical NTO crystal and a preparation method, and adopts a mixed solvent cooling crystallization mode to obtain NTO spherulitic particles with a particle size of 120-200 μm; patent CN202211569676.3 discloses a recrystallization method of NTO crystal, which adopts a cooling crystallization mode to obtain spheroid particles with the particle size of 200-400 mu m; patent CN202210853143.1 discloses a spherical monocrystal 3-nitro-1, 2, 4-triazole-5-ketone and a preparation method thereof, and adopts an additive auxiliary cooling crystallization method to obtain spherical monocrystal particles with the particle diameter of only a few microns; patent CN202111613994.0 discloses a spherical NTO crystal and a preparation method thereof, and the NTO crystal with the particle size of tens of micrometers is obtained by adopting a mixed solvent cooling crystallization method. The above disclosed methods all adopt a cooling crystallization mode to obtain monocrystalline or polycrystalline particles with different particle sizes and sphericity, but the solvent types are slightly different in proportion, and the particle sizes are only hundreds of micrometers at maximum. No report is made on the preparation method of NTO particles with larger particle size and higher sphericity. No report on the large-particle spherical agglomeration method is found in the review of the recently published methods for the preparation and characterization of spherical explosive crystals (D.Liao, M.Li, J.Wang, et al Journal of Materials Research and technology.27 (2023) 3098-3118).
Disclosure of Invention
The invention aims to further improve the NTO particle characteristics, and discloses an ultrasonic-assisted NTO crystallization granulating method, which is characterized in that two processes of explosive crystallization and granulation are coupled in one operation unit.
The invention adopts a crystallization granulation coupling method for the first time to prepare large-particle-diameter NTO spherical particles with high sphericity, and a plurality of rod-shaped crystals with dozens of micrometers are tightly agglomerated together by taking a bridging agent as a bridge to form larger particles.
The invention is realized by adopting the following technical scheme:
an ultrasonic-assisted NTO crystallization granulation method comprises the following steps:
(1) Dissolving NTO in a solvent to prepare an NTO saturated solution;
(2) Adding an antisolvent and a bridging agent into a crystallization reaction kettle, and stirring to uniformly disperse the bridging agent in the antisolvent to obtain a bridging agent-antisolvent system;
(3) Dropping the NTO saturated solution into a bridging agent-antisolvent system under stirring, and simultaneously performing ultrasonic treatment to form oil-in-water (O/W) microemulsion, and separating out NTO;
(4) Stopping ultrasonic treatment, continuing stirring, and agglomerating NTO monocrystal particles into spherical particles under the action of a shearing flow field;
(5) Filtering, washing and drying to obtain NTO spherical particles.
Optionally, the solvent is N-methylpyrrolidone; the anti-solvent is selected according to the solubility difference and the compatibility with the bridging agent, and is deionized water; the bridging agent is toluene as a binder between crystals.
Optionally, the ratio of the volume of the bridging agent to the mass of the NTO is 0.6-1 ml:1g, and the volume ratio of the solvent to the antisolvent is 1:2-1:5.
Optionally, in the steps (2), (3) and (4), the stirring is to start an electric stirrer and control the rotation speed to be 300-900 rpm, the stirring rates in the steps (2) and (3) are the same, and the stirring rate in the step (4) is the same as or different from that in the step (3).
Optionally, in the step (3), the NTO saturated solution is dripped into the bridging agent-antisolvent system at a dripping speed of 2.5-3.0 ml/min through a peristaltic pump.
The amount of bridging agent determines whether agglomerates can form or not, and optionally, the frequency of the ultrasound in step (3) is 40KHz for 1min20s to 3min20s.
Optionally, in the step (4), the stirring time is controlled to be 30-60 min.
Preferably, the volume ratio of the solvent to the non-solvent is 1:3-1:4.
Preferably, the ultrasonic time is 2min50 s-3 min10s.
Preferably, the ratio of the volume of the bridging agent to the mass of NTO is 0.7-0.8 ml:1g.
The dripping speed of the peristaltic pump is preferably 2.5-2.8 ml/min.
The ultrasonic wave provides energy for nucleation and growth of crystals, the length of the ultrasonic wave also determines whether a conglomerate can be formed finally, the ultrasonic wave is not too long, the ultrasonic wave time can be 1min20 s-3 min20s, and the ultrasonic wave time is preferably 2min50 s-3 min10s.
Stirring provides varying degrees of shear, the speed of stirring determining the size of the final agglomerated particle size, and the stirring rate is 300 to 900rpm, preferably 350 to 900rpm.
In order to obtain a dried NTO crystal product, after the stirring is finished, filtering, washing and drying are carried out. Filtering in vacuum mode, washing with deionized water, and vacuum drying at 70-90 deg.c for 6-10 hr.
Compared with the prior art, the invention has at least the following beneficial effects:
in the invention, the ultrasonic and antisolvent coupled crystallization is used to bond the ultrasonic fusion crystal together with the bridging agent to prepare large-particle spherical NTO explosive particles with different sizes, the introduction of the ultrasonic and bridging agent has great influence on the crystal morphology and coalescence, and the initial morphology and the coalescence compactness of the crystal are directly determined. The surface of the prepared NTO spherical particles has no sharp edges and corners, the sphericity is as high as 90% -93%, and the particle size is adjustable according to various specifications (such as 556 μm, 965 μm, 1323 μm, 1788 μm, 6650 μm, etc.).
Drawings
FIG. 1 is an electron microscope image of the raw material NTO crystals used in the present invention.
FIG. 2 is a photograph of NTO crystals prepared in example 1 (the minimum square length in the figure is 1 mm).
Fig. 3 is an electron microscopy image of the NTO crystals prepared by filtration immediately after stopping ultrasound in example 1.
Fig. 4 (a) is a photograph of a real object (the minimum square length in the figure is 1 mm) of the NTO crystal prepared in example 2, (b) is an electron microscope photograph, and (c) is a surface microscope photograph of the particles.
Fig. 5 (a) is a photograph of a real object (the minimum square length in the figure is 1 mm) of the NTO crystal prepared in example 3, (b) is an electron microscope photograph, and (c) is a surface microscope photograph of the particles.
Fig. 6 (a) is a photograph of a real object (minimum square length of 1mm in the figure) of the NTO crystal prepared in example 4, (b) is an electron microscope photograph, and (c) is a surface microscope photograph of the particles.
Fig. 7 (a) is a photograph of a real object (minimum square length of 1mm in the figure) of the NTO crystal prepared in example 5, (b) is an electron microscope photograph, and (c) is a surface microscope photograph of the particles.
Fig. 8 (a) is an electron microscope photograph of particles filtered immediately after the ultrasound was turned off without using a bridging agent in the comparative example, and (b) is an electron microscope photograph of final particles without using a bridging agent in the comparative example.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In the following embodiments, NTO crystals are provided by the institute of chemical materials of China engineering physical institute; n-methylpyrrolidone was purchased from Shanghai Ala Biotechnology Co., ltd; toluene was purchased from Colon Chemicals Inc. of Chemicals, inc.; deionized water was prepared by laboratory.
Example 1
An ultrasonic-assisted NTO crystallization granulation method comprises the following steps:
firstly, 1.25g of NTO raw material is dissolved in 4ml of N-methylpyrrolidone at 25 ℃ to prepare saturated solution, 12ml of deionized water is poured into a crystallization reaction kettle, the temperature of the crystallization reaction kettle is controlled to be kept at about 25 ℃, then 0.9ml of toluene is added, an electric stirrer is started, the stirring speed is regulated to 350rpm, 4ml of saturated solution is dripped into the deionized water at the dripping speed of 2.6ml/min by a peristaltic pump, simultaneously ultrasound (the frequency is 40KHz and the same applies below), ultrasound is turned off after 1min for 30s, then after 50min of stirring at 500rpm, the solution is filtered, washed and dried to obtain NTO spherical agglomerates.
FIG. 2 is a photograph of the NTO explosive particles prepared in this example, and it can be seen from FIG. 2 that the NTO explosive particles prepared in this example are uniform in size and have an average particle diameter of 6650. Mu.m; the appearance of the particles is free from sharp edges and corners, is spherical, has compact surface and better free-flowing property. Fig. 3 is a sample of crystals obtained by suction filtration immediately after the ultrasonic treatment was stopped in example 1. The average particle size was measured to be 26 μm, which can be seen to be consistent with the crystal morphology on the final sample morphology surface.
Example 2
An ultrasonic-assisted NTO crystallization granulation method comprises the following steps:
firstly, dissolving 2.5g of NTO raw material in 8ml of N-methylpyrrolidone at 25 ℃ to prepare a saturated solution, pouring 24ml of deionized water into a crystallization reaction kettle, controlling the temperature of the crystallization reaction kettle to be 25 ℃, then adding 2ml of toluene, starting an electric stirrer, dripping 8ml of saturated solution into the deionized water at the dripping speed of 2.8ml/min by a peristaltic pump at the stirring speed of 600rpm, simultaneously starting ultrasound, closing ultrasound after 3min for 10s, subsequently stirring for 60min at 500rpm, filtering, washing and drying the solution to obtain NTO spherical agglomerates.
Fig. 4 (a) is a physical picture of the obtained particles, fig. 4 (b) is an electron microscope picture, and fig. 4 (c) is an electron microscope picture of the surface of the prepared NTO particles, from which it can be seen that the prepared NTO particles are uniform in size, and have an average particle diameter of 1788 μm and a sphericity of 91.1%; the appearance of the particles has no sharp edges and corners, the sphericity is high, the surface is compact, and the flowability is good.
Example 3
An ultrasonic-assisted NTO crystallization granulation method comprises the following steps:
firstly, dissolving 1.88g of NTO raw material in 6ml of N-methylpyrrolidone at 25 ℃ to prepare saturated solution, pouring 24ml of deionized water into a crystallization reaction kettle, controlling the temperature of the crystallization reaction kettle to be kept at 25 ℃, then adding 1.5ml of toluene, starting an electric stirrer, dripping 6ml of saturated solution into the deionized water at the dripping speed of 2.8ml/min by using a peristaltic pump at the stirring speed of 700rpm, simultaneously starting ultrasound, closing ultrasound after 3min, stirring for 55min at 500rpm, filtering, washing and drying to obtain NTO spherical agglomerates.
Fig. 5 (a) is a picture of the obtained sample, fig. 5 (b) is an electron microscope picture of the sample, fig. 5 (c) is an electron microscope picture of the surface of the prepared sample particles, and it can be seen from the figure that the prepared NTO particles are uniform in size, and have an average particle diameter of 1323 μm and a sphericity of 93%; the appearance of the particles has no sharp edges and corners, the sphericity is high, the granularity is uniform, the surface is compact, and the flowability is good.
Example 4
An ultrasonic-assisted NTO crystallization granulation method comprises the following steps:
firstly, dissolving 2.5g of NTO raw material in 8ml of N-methylpyrrolidone at 25 ℃ to prepare saturated solution, pouring 28ml of deionized water into a crystallization reaction kettle, controlling the temperature of the crystallization reaction kettle to be kept at 25 ℃, then adding 1.8ml of toluene, starting an electric stirrer, dripping 8ml of saturated solution into the deionized water at a dripping speed of 2.6ml/min through a peristaltic pump at a stirring speed of 800rpm, simultaneously starting ultrasound, turning off ultrasound after 3min, stirring for 50min at 500rpm, filtering, washing and drying the solution to obtain NTO spherical agglomerates.
Fig. 6 (a) is a picture of the resulting NTO sample, fig. 6 (b) is an electron microscope picture of the sample, and fig. 6 (c) is an electron microscope picture of the surface of the prepared sample particles, from which it can be seen that the prepared NTO particles are uniform in size, have an average particle diameter of 1187 μm, and have a sphericity of 92.6%; the appearance of the particles has no sharp edges and corners, the sphericity is high, the surface is compact, and the flowability is good.
Example 5
An ultrasonic-assisted NTO crystallization granulation method comprises the following steps:
firstly, dissolving 2.5g of NTO raw material in 8ml of N-methylpyrrolidone at 25 ℃ to prepare saturated solution, pouring 24ml of deionized water into a crystallization reaction kettle, controlling the temperature of the crystallization reaction kettle to be kept at 25 ℃, then adding 1.9ml of toluene, starting an electric stirrer, dripping 8ml of saturated solution into the deionized water at the dripping speed of 2.8ml/min by using a peristaltic pump at the stirring speed of 700rpm, simultaneously starting ultrasound, closing ultrasound after 3min for 10s, subsequently adjusting the rotating speed of 900rpm, stirring for 1h, filtering the solution, and drying to obtain NTO spherical agglomerates.
Fig. 7 (a) is a sample picture of the resulting ntu, fig. 7 (b) is an electron microscope picture of the sample, and fig. 7 (c) is an electron microscope picture of the surface of the prepared sample particles, from which it can be seen that the prepared ntu particles are uniform in size, have a measured average particle size of 627 μm, and have a sphericity of 88.1%; the appearance of the particles has no sharp edges and corners, the sphericity is high, the surface is compact, and the flowability is good.
In the comparative example, no bridging agent was used
Firstly, dissolving 2.5g of NTO raw material in 8ml of N-methylpyrrolidone at 25 ℃ to prepare saturated solution, pouring 24ml of deionized water into a crystallization reaction kettle, controlling the temperature of the crystallization reaction kettle to be kept at 25 ℃, starting an electric stirrer, regulating the stirring speed to 600rpm, dripping 8ml of saturated solution into the deionized water at the dripping speed of 2.8ml/min by using a peristaltic pump, simultaneously starting ultrasonic waves, closing the ultrasonic waves after 2min for 55min, and then stirring for 50min at 500rpm, filtering, washing and drying the solution to obtain NTO agglomerates.
Fig. 8 (a) is a graph of the prepared sample after the ultrasound is turned off without the bridging agent, and fig. 8 (b) is an electron microscope graph of the final sample, and it can be seen that after the ultrasound, the irregular aggregate can be formed by stirring for a certain time. The average particle diameter of the particles in FIG. 8 (a) was 27. Mu.m, and the average particle diameter of the aggregates in FIG. 8 (b) was 78. Mu.m. The toluene has a crucial role in the crystal agglomeration process as demonstrated by the introduction or absence of a bridging agent.
Although the invention has been described herein with reference to illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure. More specifically, various variations and modifications may be made to the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure. In addition to variations and modifications in the component parts and/or arrangements, other uses will be apparent to those skilled in the art.
Claims (10)
1. An ultrasonic-assisted NTO crystallization granulation method is characterized by comprising the following steps:
(1) Dissolving NTO in a solvent to prepare an NTO saturated solution;
(2) Adding an antisolvent and a bridging agent into a crystallization reaction kettle, and stirring to uniformly disperse the bridging agent in the antisolvent to obtain a bridging agent-antisolvent system;
(3) Dropping the NTO saturated solution into a bridging agent-antisolvent system under stirring, and simultaneously performing ultrasonic treatment to form oil-in-water microemulsion, and separating out NTO;
(4) Stopping ultrasonic treatment, and continuing stirring to enable NTO monocrystal particles to be coalesced into spherical particles;
(5) Filtering, washing and drying to obtain NTO spherical particles.
2. The ultrasonic-assisted ntu crystallization granulation method of claim 1, wherein the solvent is N-methyl pyrrolidone, the anti-solvent is deionized water, and the bridging agent is toluene.
3. The ultrasonic-assisted ntu crystallization granulation method according to claim 2, wherein the ratio of the volume of the bridging agent to the mass of the ntu is 0.6-1 ml:1g, and the volume ratio of the solvent to the antisolvent is 1:2-1:5.
4. The ultrasonic-assisted NTO crystallization granulation method according to claim 1, wherein the stirring in the steps (2), (3) and (4) is to start an electric stirrer and control the rotation speed to 300-900 rpm, the stirring rates in the steps (2) and (3) are the same, and the stirring rate in the step (4) is the same as or different from that in the step (3).
5. The ultrasonic-assisted ntu crystallization granulation method according to claim 1, wherein the NTO saturated solution is dripped into the bridging agent-antisolvent system in step (3) by peristaltic pump at a dripping rate of 2.5-3.0 ml/min.
6. The ultrasonic-assisted NTO crystallization granulation method according to claim 1, wherein the ultrasonic frequency of step (3) is 40KHz, and the time is 1min20 s-3 min20s.
7. The ultrasonic-assisted NTO crystallization granulation method according to claim 1, wherein the stirring time is controlled to be 30-60 min in the step (4).
8. The ultrasonic-assisted ntu crystallization granulation method of claim 3, wherein the volume ratio of solvent to non-solvent is 1:3-1:4.
9. The ultrasonic-assisted ntu crystallization granulation method according to claim 6, wherein the ultrasonic time is 2min50 s-3 min10s.
10. The ultrasonic-assisted ntu crystallization granulation method according to claim 6, wherein the ratio of the volume of the bridging agent to the mass of the ntu is 0.7-0.8 ml:1g.
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