Purification method of energetic plasticizer A3
By mixing the method of mixing the coarse product of the plastic increase agent A3 and the solvents, the problem of high energy consumption and impurities in existing technologies is difficult to separate, and the capable plastic increase agent A3 with high purity and high income is achieved. Suitable for large -scale production.
Patent Information
- Application Number
- CN202411294628.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-14
- Publication Date
- 2025-01-28
AI Technical Summary
The prior art has problems such as high energy consumption, low equipment tolerance, long distillation time, and difficulty in separation of impurities when preparing energy-containing plasticizer A3, resulting in unstable product purity and yield.
Adopt a mix of coarse products containing plasticizers A3 and solvent according to the quality ratio 1: (0.5 ~ 5), cooling to -30 to 5 ℃ for crystallization, and the purification method of filtering, washing and drying. A3 and impurities.
It improves the purity and revenue of the capable plastic increase A3, simplifies the process of process, reduces energy consumption, improves the stability of product quality, and is suitable for large -scale production.
Smart Images
Figure CN119371316A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a method for purifying an energetic plasticizer A3, and belongs to the field of compound purification. Background Art
[0002] Energetic plasticizer A3 is a mixture of bis(2,2-dinitropropanol)acetal (BDNPA) and bis(2,2-dinitropropanol)formal (BDNPF) compounded in equal mass ratios, and has the advantages of good stability and excellent plasticizing properties. Energetic plasticizer A3, as a high-energy insensitive energetic plasticizer, is widely used in the fields of propellants and mixed explosives. At present, a three-step synthesis method is generally used to prepare a crude energetic plasticizer A3, and then the crude energetic plasticizer A3 is purified by high vacuum distillation to obtain energetic plasticizer A3. Specifically, the various components of energetic plasticizer A3 are first synthesized, and the organic solvent in each component is removed by reduced pressure distillation, and then the fractions are purified by high vacuum distillation. The components are compounded in an equal mass ratio of 1:1 to obtain energetic plasticizer A3. The above process still has the following problems: 1. The distillation temperature is high, usually 180-200°C, which consumes a lot of energy, and the high temperature affects the tolerance of the equipment, reducing the service life of the equipment; 2. The distillation time is long, and the distillation process of a single batch of less than 50kg takes 10-12 hours, which limits the production capacity; 3. The boiling points of the two-component monomers of the A3 product are very high, requiring extremely high vacuum and high distillation temperature, which increases the distillation energy consumption and places high requirements on the vacuum degree of the equipment; 4. The boiling points of some impurities in the A3 crude product are close to those of the A3 product. During distillation, it is necessary not only to slowly increase the temperature according to the procedure, but also to assemble a distillation tower to purify the A3 product by segmented fractionation. The actual operation process is difficult and the operation process is complicated; 5. The two-component monomers are weakly decomposed at a higher temperature, and new impurities are generated during the distillation process, which makes the quality of the A3 product unstable, and the A3 product is lost and the yield is low. Summary of the invention
[0003] The present invention provides a method for purifying an energetic plasticizer A3, which can improve the purity and yield of the energetic plasticizer A3, and the purification process is simple and the purification cycle is short.
[0004] The present invention provides a method for purifying an energetic plasticizer A3, comprising the following steps: mixing a crude energetic plasticizer A3 with a solvent in a mass ratio of 1:(0.5-5) to obtain a mixed solution; cooling the mixed solution to -30-5°C for crystallization, filtering, washing and drying to obtain the energetic plasticizer A3; wherein the solvent comprises one or more of water, an alcohol solvent, ethyl acetate, acetone, petroleum ether, THF, DMF and toluene.
[0005] Optionally, the alcohol solvent includes one or more of methanol, ethanol, and isopropanol.
[0006] Optionally, the mass ratio of the crude energetic plasticizer A3 to the solvent is 1:(1-3).
[0007] Optionally, the mixed solution is cooled to -20 to 0°C for crystallization, and filtered, washed and dried to obtain the energetic plasticizer A3.
[0008] Optionally, the mixed solution is cooled to -15 to -5°C for crystallization, and filtered, washed and dried to obtain the energetic plasticizer A3.
[0009] Optionally, the mixed solution is cooled to -15 to -10°C for crystallization, and filtered, washed and dried to obtain the energetic plasticizer A3.
[0010] Optionally, the crude energetic plasticizer A3 is melted to obtain molten crude energetic plasticizer A3; the molten crude energetic plasticizer A3 is mixed with the solvent in a mass ratio of 1:(0.5-5) to obtain the mixed solution.
[0011] Optionally, the process of cooling the mixed solution to -30 to 5°C for crystallization includes: placing the mixed solution in a cooling medium at -30 to 5°C for crystallization.
[0012] Optionally, stirring is performed during the crystallization process, and the stirring speed is 200 to 1000 r / min.
[0013] Optionally, stirring is performed during the crystallization process, and the stirring speed is 300 to 800 r / min.
[0014] The present invention provides a purification method for an energetic plasticizer A3, which can effectively separate the energetic plasticizer A3 and impurities in a crude product, and improve the purity of the energetic plasticizer A3. The method has a simple process flow, low requirements on equipment, low energy consumption, and stable product quality, and is suitable for workshop scale-up production, which significantly improves the convenience and economic benefits of production, and is of great significance for promoting the application of the energetic plasticizer A3 in the actual charging process. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 is a flow chart of a purification method of an energetic plasticizer A3 according to some embodiments;
[0016] Figure 2 is the HPLC chromatogram of BDNPF;
[0017] Figure 3 is the high performance liquid chromatogram of BDNPA;
[0018] Figure 4This is the high performance liquid chromatogram of the energetic plasticizer A3 of Example 1. DETAILED DESCRIPTION
[0019] In order to make the purpose, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0020] The embodiment of the present invention provides a method for purifying an energetic plasticizer A3, comprising the following steps: mixing a crude energetic plasticizer A3 with a solvent in a mass ratio of 1:(0.5-5) to obtain a mixed solution; cooling the mixed solution to -30-5°C for crystallization, filtering, washing, and drying to obtain the energetic plasticizer A3; wherein the solvent comprises one or more of water, an alcohol solvent, ethyl acetate, acetone, petroleum ether, THF, DMF, and toluene.
[0021] According to the research and analysis of the inventors, the crude energetic plasticizer A3 contains impurities such as part of the intermediates, a small amount of raw materials and impurity components generated during the synthesis of the intermediates. These impurities have different solubilities from the energetic plasticizer A3 in the above-mentioned solvent. In the above-mentioned purification process, the crude energetic plasticizer A3 and the above-mentioned solvent are first fully mixed in a mass ratio of 1: (0.5-5) to make the energetic plasticizer A3 completely dissolved in the above-mentioned solvent, and part of the impurities are insoluble in the above-mentioned solvent, so that the energetic plasticizer A3 and the insoluble impurities are effectively separated. The obtained mixed solution includes the energetic plasticizer A3 and soluble impurities. The mixed solution is then cooled to -30-5°C for crystallization (or refining). Within this temperature range, the solubility of the soluble impurities in the mixed solution is less than that of the energetic plasticizer A3, so that the energetic plasticizer A3 can be crystallized and soluble impurities cannot be crystallized, thereby effectively separating the energetic plasticizer A3 and the soluble impurities, and finally obtaining an energetic plasticizer A3 with a higher purity.
[0022] Therefore, the embodiment of the present invention achieves effective separation of energetic plasticizer A3 and impurities in the crude energetic plasticizer A3 by controlling the solvent type, the mass ratio of the crude product to the solvent, the cooling temperature and other conditions, and can also avoid the monomer of the energetic plasticizer A3 from being weakly decomposed under the action of high temperature and generating new impurities during the high-temperature distillation process, thereby safely and conveniently improving the purity and yield of the energetic plasticizer A3, and realizing the refining of the energetic plasticizer A3; in addition, the above-mentioned purification process of the energetic plasticizer A3 also has the advantages of simple operation procedures, low requirements for equipment, low energy consumption, stable product quality, short refining cycle, high production convenience, less organic waste residue discharge, green environmental protection, etc., and is easy to carry out workshop scale-up production. In the scale-up production, by multiplying each batch of feed, the production capacity, economic benefits and environmental benefits can be significantly improved, and the quality of the obtained energetic plasticizer A3 is stable and the purity is high, so that it exhibits good performance in the charging process, which is of great significance to promoting the application of the energetic plasticizer A3 in the actual charging process.
[0023] As described above, the energetic plasticizer A3 is a mixture of bis(2,2-dinitropropanol)acetal (BDNPA) and bis(2,2-dinitropropanol)formal (BDNPF) compounded in an equal mass ratio. The crude energetic plasticizer A3 of the embodiment of the present invention can be a crude energetic plasticizer A3 prepared by a conventional method in the art. For example, the process for preparing the crude energetic plasticizer A3 includes: preparing a key intermediate-2,2-dinitropropanol by catalyzing with a catalyst potassium ferrocyanide; and then The key intermediate 2,2-dinitropropanol is used as a raw material to synthesize bis(2,2-dinitropropanol)acetal (BDNPA) and bis(2,2-dinitropropanol)formal (BDNPF) respectively; finally, BDNPF and BDNPA are compounded in an equal mass ratio to obtain a crude energetic plasticizer A3. The purification method of the embodiment of the present invention can be used to purify the crude energetic plasticizer A3, thereby improving the purity and yield of the energetic plasticizer A3, and the purification process is simple and the purification cycle is short.
[0024] In addition, some solvent may remain in the crude energetic plasticizer A3. In order to avoid affecting the purification effect, the solvent in the crude energetic plasticizer A3 needs to be removed in advance.
[0025] A too high or too low mass ratio of the crude energetic plasticizer A3 to the solvent is not conducive to improving the purity and yield of the energetic plasticizer A3. The reason is that when the above mass ratio is too high, the crude energetic plasticizer A3 is mixed with too much solvent, so that the concentration of the energetic plasticizer A3 in the mixed solution is low, resulting in the energetic plasticizer A3 in the mixed solution being difficult to crystallize, which is not conducive to the purification of the energetic plasticizer A3 and reduces its yield. When the mass ratio is too high, too little solvent is insufficient to dissolve all the energetic plasticizer A3, resulting in the loss of the energetic plasticizer A3, which is not conducive to improving the yield of the energetic plasticizer A3. In the embodiment of the present invention, the mass ratio of the crude energetic plasticizer A3 to the solvent is 1:(0.5-5). By mixing the crude energetic plasticizer A3 with the solvent according to the above mass ratio, all the energetic plasticizer A3 can be dissolved, and the concentration of the energetic plasticizer A3 in the mixed solution is relatively high, which is easy to crystallize, thereby helping to improve the purity and yield of the energetic plasticizer A3.
[0026] Exemplarily, the mass ratio of the crude energetic plasticizer A3 to the solvent may be a:b, where a=1, 0.5≤b≤5. Exemplarily, a is 1, and b is 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5 or a range consisting of any two of them.
[0027] The process of mixing the crude energetic plasticizer A3 with the solvent in a mass ratio of 1:(0.5-5) to obtain a mixed solution includes: mixing the crude energetic plasticizer A3 with the solvent in a mass ratio of 1:(0.5-5), filtering, and obtaining a mixed solution. In the above mixing process, the energetic plasticizer A3 is dissolved in the solvent, while the insoluble impurities are insoluble in the solvent. The insoluble impurities can be removed by filtering, thereby achieving effective separation of the energetic plasticizer A3 and the insoluble impurities.
[0028] Furthermore, the mass ratio of the crude energetic plasticizer A3 to the above-mentioned solvent is preferably 1:(1-3), which is more conducive to improving the purification effect of the energetic plasticizer A3 and making the purity and yield of the energetic plasticizer A3 higher.
[0029] Specifically, when the impurity content in the crude energetic plasticizer A3 is high, the crude energetic plasticizer A3 is in liquid form and can be directly purified through the above-mentioned purification process; when the impurity content in the crude energetic plasticizer A3 is low, the crude energetic plasticizer A3 is in solid form, and the crude energetic plasticizer A3 needs to be melted first to obtain molten crude energetic plasticizer A3; then the molten crude energetic plasticizer A3 is mixed with a solvent in a mass ratio of 1:(0.5-5) to obtain a mixed solution, and then the mixed solution is crystallized to allow the energetic plasticizer A3 to crystallize out.
[0030] The process of cooling the mixed solution to -30 to 5°C for crystallization may specifically be a process of cooling the mixed solution to -30 to 5°C for recrystallization. In this case, the purification process is a recrystallization purification process.
[0031] Recrystallization is a purification method through dissolution and recrystallization, specifically, the separation of components in a solid mixture by utilizing their different solubility in a certain solvent. Therefore, the above-mentioned purification process of the solid energetic plasticizer A3 crude product is also a recrystallization purification process.
[0032] Existing crystallization (or recrystallization) technologies mainly include cooling crystallization, injection method, vacuum distillation method, and supercritical method. Among them, the cooling crystallization method is used for purification in the embodiment of the present invention, which helps to improve the purity and yield of the energetic plasticizer A3, and also has the advantages of simple operation process, low requirements for equipment, low energy consumption, stable product quality, and short refining cycle.
[0033] In the above purification process, the mixed solution includes energetic plasticizer A3 and soluble impurities, and the mixed solution is cooled to -30 to 5°C for crystallization (or recrystallization). In this temperature range, energetic plasticizer A3 is easy to precipitate, and soluble impurities are not easy to precipitate, thereby achieving effective separation of energetic plasticizer A3 and soluble impurities, and improving the purity and yield of energetic plasticizer A3. Exemplarily, the temperature after the above cooling can be -30°C, -25°C, -20°C, -15°C, -10°C, -5°C, 0°C, 5°C, or a range consisting of any two of them.
[0034] In some embodiments, the process of cooling the mixed solution to -30 to 5° C. for crystallization includes: placing the mixed solution in a cooling medium at -30 to 5° C. for crystallization. The cooling medium may include an ethanol solution, and the volume fraction of ethanol in the ethanol solution may be 93 to 97%, for example, 93%, 95%, 97, or a range consisting of any two thereof.
[0035] Further, the mixed solution is cooled to -20 to 0°C for crystallization, filtered, washed and dried to obtain energetic plasticizer A3. In this temperature range, energetic plasticizer A3 is more likely to precipitate, while soluble impurities are less likely to precipitate, so that the energetic plasticizer A3 and soluble impurities are better separated, thereby increasing the purity and yield of energetic plasticizer A3.
[0036] Furthermore, the mixed solution is cooled to -15 to -5°C for crystallization, filtered, washed and dried to obtain energetic plasticizer A3. In this temperature range, energetic plasticizer A3 is more likely to precipitate, while soluble impurities are less likely to precipitate, so that the energetic plasticizer A3 and soluble impurities are better separated, thereby increasing the purity and yield of energetic plasticizer A3.
[0037] Furthermore, the mixed solution is cooled to -15 to -10°C for crystallization, filtered, washed and dried to obtain energetic plasticizer A3. In this temperature range, energetic plasticizer A3 is more likely to precipitate, while soluble impurities are less likely to precipitate, thereby optimizing the separation effect of energetic plasticizer A3 and soluble impurities, thereby maximizing the purity and yield of energetic plasticizer A3.
[0038] In order to further improve the effect of crystallization, stirring is performed during the above crystallization process, and the stirring speed can be 200-1000 r / min, so that the precipitated crystal particles of the energetic plasticizer A3 are of moderate size, and rapid stirring (speed higher than 1000 r / min) is avoided to make the crystal particles of the energetic plasticizer A3 smaller, and slow stirring (speed lower than 1000 r / min) is avoided to make the crystal particles of the energetic plasticizer A3 smaller, which is beneficial to improving the purity and yield of the energetic plasticizer A3.
[0039] Illustratively, the stirring speed may be 200 r / min, 300 r / min, 400 r / min, 500 r / min, 600 r / min, 700 r / min, 800 r / min, 900 r / min, 1000 r / min or a range consisting of any two of them.
[0040] Furthermore, stirring is performed during the crystallization process, and the stirring speed is 300-800 r / min, which is conducive to the crystal precipitation of the energetic plasticizer A3, increases the yield of the energetic plasticizer A3, and facilitates the crystal particles of the energetic plasticizer A3 to be more uniform.
[0041] In some embodiments, the stirring time is 1 to 4 hours, such as 1 hour, 2 hours, 3 hours, 4 hours or a range consisting of any two thereof.
[0042] The process of the purification method of the embodiment of the present invention is as follows Figure 1 shown.
[0043] The solubility of energetic plasticizer A3 in different types of solvents is different, and different types of solvents have different polarities, so different types of solvents have an important influence on the purity and yield of energetic plasticizer A3. In the embodiment of the present invention, the solvent includes one or more of water, alcohol solvents, ethyl acetate, acetone, petroleum ether, THF, DMF, and toluene, which helps to effectively separate energetic plasticizer A3 from impurities and improve the purity and yield of energetic plasticizer A3. In addition, these solvents are relatively cheap and easy to obtain, which is conducive to reducing production costs.
[0044] According to further research by the inventors, when the solvent used includes an alcohol solvent, it is beneficial to significantly improve the purity and yield of the energetic plasticizer A3. Further, when the alcohol solvent includes one or more of methanol, ethanol, and isopropanol, the raw materials and other impurities remaining in the crude energetic plasticizer A3 that have not been completely reacted can be better removed, further improving the purity and yield of the energetic plasticizer. Among them, the alcohol solvent is preferably ethanol, because ethanol helps to improve the precipitation effect of the energetic plasticizer A3 crystals, improves the yield of the energetic plasticizer A3, and helps to reduce costs, with little pollution.
[0045] Since the solubility of the energetic plasticizer A3 in the solvent is related to the temperature, in the above purification process, it is necessary to select a suitable cooling temperature in combination with different types of solvents to achieve a better purification effect. In some embodiments, the solvent includes ethanol, the cooling temperature is -20 to 0°C, the crystallization (or recrystallization) efficiency is high, the purification effect is good, the purity and yield of the energetic plasticizer A3 are maximized, and the quality of the energetic plasticizer A3 is effectively improved.
[0046] In the above purification process, the crude energetic plasticizer A3 is mixed with the solvent in a mass ratio of 1:(0.5-5) to obtain a mixed solution; the mixed solution is cooled to -30-5°C for crystallization and other processes can be carried out in a reactor, and the above reactor can be a conventional reactor in the art, such as an ordinary enamel reactor.
[0047] The present invention is described in more detail below through specific examples and comparative examples.
[0048] Example 1
[0049] This embodiment provides a method for purifying an energetic plasticizer A3, comprising the following steps:
[0050] The crude energetic plasticizer A3 and ethanol are mixed in a mass ratio of 1:2 to obtain a mixed solution;
[0051] The mixed solution was placed in a 95% (v / v) ethanol solution at -25°C for crystallization. During the crystallization process, the solution was stirred at a speed of 300 r / min. After filtering, washing and drying, energetic plasticizer A3 was obtained.
[0052] Comparative Example 4
[0053] This comparative example provides a method for purifying an energetic plasticizer A3, comprising the following steps:
[0054] 1) First, the BDNPF crude concentrate is heated in an oil bath, and the temperature of the oil bath is controlled at 75±5°C to remove the residual solvent in the BDNPF crude concentrate; then the temperature is slowly raised to 180-200°C, and the vacuum degree is maintained at 10-25Pa, and high vacuum distillation is started, and the fraction at 158-160°C is collected to obtain the purified BDNPF finished product;
[0055] 2) First, the BDNPA crude concentrate is heated in an oil bath, and the temperature of the oil bath heating is controlled at 75±5°C to remove the residual solvent in the BDNPA crude concentrate; then the temperature is slowly raised to 180-200°C, and the vacuum degree is maintained at 10-25Pa, and high vacuum distillation is started, and the fraction of 158-160°C is collected to obtain the purified BDNPA finished product;
[0056] 3) The purified BDNPF finished product and the BDNPA finished product are mixed in an equal mass ratio to obtain an energetic plasticizer A3.
[0057] Referring to the process of Example 1, the energetic plasticizer A3 of Examples 2 to 31 and Comparative Examples 1 to 3 were purified respectively.
[0058] The reaction parameters of each embodiment and comparative example are summarized in Table 1.
[0059] Table 1 Reaction parameters of each embodiment and comparative example
[0060]
[0061]
[0062] Test example
[0063] 1. The following parameters of the above embodiments and comparative examples were tested:
[0064] 1) Purity of energetic plasticizer A3: The energetic plasticizer A3 purified in the above-mentioned examples and comparative examples was subjected to high performance liquid chromatography analysis (HPLC analysis), and the peak area ratio of the energetic plasticizer A3 was obtained by referring to the area normalization method, which is the purity of the energetic plasticizer A3. The specific results are shown in Table 2;
[0065] Taking Example 1 as an example, the energetic plasticizer A3 of Example 1 was subjected to HPLC analysis to obtain an HPLC chromatogram of the energetic plasticizer A3 as shown below: Figure 4 As shown, Figure 4 The data of the retention time (min), peak width (min), peak area, peak height and peak area proportion (%) of the energetic plasticizer A3 are shown in Table 4;
[0066] BDNPF was analyzed by high performance liquid chromatography. The high performance liquid chromatography of BDNPF is shown in Figure 2As shown, Figure 2 The data of retention time (min), peak width (min), peak area, peak height and peak area proportion (%) of BDNPF are shown in Table 2;
[0067] BDNPA was analyzed by high performance liquid chromatography. The high performance liquid chromatography of BDNPA is as follows: Figure 3 As shown, Figure 3 The data of retention time (min), peak width (min), peak area, peak height and peak area ratio (%) of BDNPA are shown in Table 3.
[0068] 2) Yield of energetic plasticizer A3: The purified energetic plasticizer A3 was weighed, and the yield of energetic plasticizer A3 was obtained by dividing the mass of the purified energetic plasticizer A3 by the mass of the crude energetic plasticizer A3. The results are shown in Table 5.
[0069] 2. Test results
[0070] Table 2 Figure 2 Retention time (min), peak width (min), peak area, peak height and peak area ratio (%) of BDNPF
[0071] Retention time (min) Peak width (min) Peak area Peak height Peak area ratio (%) 1.897 0.22 10.95 3.14 0.20 2.031 0.37 59.81 10.47 1.09 7.089 0.77 5406.20 424.30 98.71
[0072] from Figure 2 As can be seen from Table 2, the purity (peak area ratio) of BDNPF is close to 98.71%.
[0073] Table 3 Figure 3 Retention time (min), peak width (min), peak area, peak height and peak area ratio (%) of BDNPA
[0074] Retention time (min) Peak width (min) Peak area Peak height Peak area ratio (%) 2.042 0.20 11.91 2.37 0.03 3.184 0.28 21.46 3.79 0.06 4.041 0.53 55.65 7.48 0.16 5.307 0.70 43.49 4.06 0.12 6.310 1.11 223.71 16.57 0.64 7.131 0.74 89.99 5.26 0.26 8.644 1.63 34569.98 2101.97 98.73
[0075] from Figure 3 As can be seen from Table 3, the purity (peak area percentage) of BDNPA is close to 98.73%.
[0076] Table 4 Figure 4 Retention time (min), peak width (min), peak area, peak height and peak area ratio (%) of energetic plasticizer A3
[0077] Retention time (min) Peak width (min) Peak area Peak height Peak area ratio (%) 2.961 0.26 23.64 3.98 0.21 3.654 0.41 40.56 4.27 0.36 4.148 0.34 13.77 1.73 0.12 5.490 0.53 69.16 5.55 0.62 6.550 0.72 61.30 3.51 0.55 7.397 0.78 5651.74 383.98 50.29 9.093 1.12 5378.92 298.90 47.86
[0078] from Figure 4 It can be seen from Table 4 that the purity (peak area ratio) of the energetic plasticizer A3 of Example 1 is close to 98.15% (50.29%+47.86%).
[0079] Table 5 Purity and yield of products
[0080]
[0081]
[0082] Data Analysis:
[0083] The purification method of the energetic plasticizer A3 provided in the embodiment of the present invention is helpful to improve the purity and yield of the energetic plasticizer A3.
[0084] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for purifying an energetic plasticizer A3, characterized in that: The following steps are involved: The crude energetic plasticizer A3 and the solvent are mixed in a mass ratio of 1:(0.5-5) to obtain a mixed solution; Cooling the mixed solution to -30 to 5°C for crystallization, filtering, washing and drying to obtain the energetic plasticizer A3; Wherein, the solvent includes one or more of water, alcohol solvent, ethyl acetate, acetone, petroleum ether, THF, DMF, and toluene.
2. The purification method according to claim 1, characterized in that The alcohol solvent includes one or more of methanol, ethanol and isopropanol.
3. The purification method according to claim 1, characterized in that The mass ratio of the crude energetic plasticizer A3 to the solvent is 1:(1-3).
4. The purification method according to claim 1, characterized in that The mixed solution is cooled to -20 to 0°C for crystallization, and filtered, washed and dried to obtain the energetic plasticizer A3.
5. The purification method according to claim 4, characterized in that The mixed solution is cooled to -15 to -5°C for crystallization, and filtered, washed and dried to obtain the energetic plasticizer A3.
6. The purification method according to claim 5, characterized in that The mixed solution is cooled to -15 to -10°C for crystallization, and filtered, washed and dried to obtain the energetic plasticizer A3.
7. The purification method according to claim 1, characterized in that Melting the crude energetic plasticizer A3 to obtain molten crude energetic plasticizer A3; The molten crude energetic plasticizer A3 is mixed with the solvent in a mass ratio of 1:(0.5-5) to obtain the mixed solution.
8. The purification method according to claim 1, characterized in that The process of cooling the mixed solution to -30 to 5°C for crystallization comprises: The mixed solution is placed in a cooling medium at -30 to 5° C. for crystallization.
9. The purification method according to claim 1 or 4, characterized in that: Stirring is performed during the crystallization process, and the stirring speed is 200 to 1000 r / min.
10. The purification method according to claim 9, characterized in that Stirring is performed during the crystallization process, and the stirring speed is 300 to 800 r / min.