A method for improving the yield of hexabenzylhexaazaisowurtzitane
The synthesis of HBIW using a continuous stirred tank reactor solves the problems of long reaction time and low product yield in existing technologies, achieving efficient and safe HBIW synthesis suitable for industrial production.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-04
- Publication Date
- 2026-03-24
AI Technical Summary
Existing HBIW synthesis methods suffer from problems such as long reaction time, low product yield, numerous side reactions, and difficult post-processing, making them difficult to implement in industrial applications.
HBIW was synthesized using a continuous stirred tank reactor (CSTR). The reactants and acid were fed into different reactors by injection pumps and peristaltic pumps, respectively, and the temperature was controlled at 10-30℃. The product was purified by recrystallization to obtain light yellow needle-like crystals.
It effectively improves the synthesis efficiency and safety of HBIW, with a yield of 76.82%-88.62%, simplifies the post-processing, and is suitable for industrial production.
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Figure CN117186110B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of energetic materials, and relates to a method for improving the yield of preparation of hexabenzylhexaazaisowurtzitane. BACKGROUND
[0002] Hexabenzylhexaazaisowurtzitane (HBIW) has a cage structure and is an energetic material, and is extremely unstable in an acidic condition due to the presence of an amino group and is easily destroyed, and the aromatic ring of the benzyl group has stronger nitration competition ability than the tertiary amine in the cage, so that the nitrolysis reaction cannot be directly performed, and the HBIW can be prepared through various reactions to be an intermediate in a nitration reaction and be an important raw material for synthesizing energetic materials.
[0003] CL-20 is a hot spot in the field of energetic materials at present, although there are various CL-20 synthesis precursors, but the yield of the product obtained after the reaction of the linear condensation and the amine with a substituent on the benzene ring and the aldehyde is low, there are many by-products, and the subsequent steps are difficult to perform, so that the HBIW is still the main precursor for synthesizing the CL-20. As a ring of the subsequent reaction, the industrialization thereof is also the research target of us.
[0004] At present, the synthesis of the HBIW mostly adopts the one-pot method, the formic acid is used as a catalyst, the reaction process is complex, there are many by-products, the yield of the small test is 70-80%, and the yield of the industrial amplification is 55-65%. The stable yield of the small test synthesis is only 73% through the repeated literature method, so that the synthesis process needs to be explored, and the suitable reaction condition needs to be found.
[0005] Although there are many literatures reporting the preparation of the HBIW, most of these methods have one or more of the following shortcomings: long reaction time, low product yield, high reaction cost, many side reactions, and difficult post-processing. These problems have not been solved. SUMMARY
[0006] The purpose of the application is to provide a method for improving the yield of preparation of the HBIW.
[0007] In order to achieve the above purpose, the technical scheme of the application is: a method for synthesizing the HBIW by using a continuous stirred tank reactor.
[0008] The synthesis method disclosed by the application comprises the following specific steps:
[0009] Step 1) the mixed solution of acetonitrile and water, benzylamine and glyoxal are simultaneously sent into a first continuous stirred tank reactor (CSTR-1) through an injection pump to perform a mixing reaction, the reaction is performed for 0.5-1.5 h, and the reaction temperature of the CSTR-1 is controlled to be 10-30 DEG C.
[0010] Step 2) The reaction solution in step (1) is transferred to the second continuous stirred tank reactor (CSTR-2) by peristaltic pump, and the acid is sent into CSTR-2 by injection pump, and the reaction is continued for 0.5-1.5h, and the temperature in CSTR-2 is controlled at 10-30℃, and then the target product is obtained.
[0011] Step 3) The crude product obtained in step (2) is recrystallized with a solvent to obtain light yellow needle-shaped crystals.
[0012] Compared with the prior art, the present application has the following advantages: the present application uses a stirred tank continuous reactor to synthesize HBIW, effectively overcoming the problems of long synthesis time, uneven mixing of substances, and low yield, and improving the yield and safety of the reaction. It is expected to become a new method for preparing HBIW. BRIEF DESCRIPTION OF DRAWINGS
[0013] Figure 1 System device diagram containing CSTR.
[0014] Figure 2 DSC diagram of reaction product.
[0015] Figure 3 Infrared diagram of reaction product.
[0016] Figure 4 NMR 1H diagram of reaction product. DETAILED DESCRIPTION
[0017] The total synthesis route of the target compound is as follows:
[0018]
[0019] The technical solutions of the present application are further specifically described below by the accompanying drawings Figure 1 , total synthesis route and examples.
[0020] In combination Figure 1 , the device of the reaction system includes CSTR, injection pump and peristaltic pump. The reactants are transported to the first continuous stirred tank reactor (CSTR-1) by the injection pump through the polytetrafluoroethylene tube, mixed and reacted for 0.5-1.5h, and then the obtained reaction solution is sent to the second continuous stirred tank reactor (CSTR-2) by the peristaltic pump through the polytetrafluoroethylene tube, and the acid is sent to CSTR-2 by the injection pump, mixed and reacted to obtain the target product.
[0021] The method for preparing HBIW comprises the following steps: firstly, raw materials are fed into CSTR-1 for mixing reaction for 0.5-1.5 hours to obtain a reaction solution; and then the reaction solution is sent to CSTR-2 through a peristaltic pump while acid is added, so that the substances in the reaction solution are subjected to a series of cyclization and protonation to form the final product HBIW.
[0022] Step 1) a mixed solution of acetonitrile and water, benzylamine and glyoxal are simultaneously fed into CSTR-1 through a syringe pump for mixing reaction, the reaction is carried out for 0.5-1.5 hours, and the reaction temperature of CSTR-1 is controlled at 10-30℃.
[0023] Step 2) the solution after reaction in step (1) is transferred to CSTR-2 through a peristaltic pump, while acid is fed into CSTR-2 through a syringe pump, and the reaction is continued for 0.5-1.5 hours, and the temperature in CSTR-2 is controlled at 10-30℃, thereby obtaining the target product.
[0024] Step 3) after the reaction is completed, the mixed solution is filtered, and recrystallization is carried out with a solvent to obtain light yellow needle-shaped crystals, and the purity of the product is analyzed by means of nuclear magnetic resonance and DSC.
[0025] Further, in step (1), the volume ratio of acetonitrile to water is 10:1-40:1.
[0026] Further, in step (1), the molar ratio of benzylamine to glyoxal is controlled at 2:0.5-2:1.
[0027] Further, in step (2), the acid used is selected from any one of formic acid, acetic acid, sulfamic acid, p-toluenesulfonic acid and benzoic acid.
[0028] Further, in step (2), the molar ratio of acid to benzylamine is controlled at 1:0.03-1:0.1.
[0029] Further, in step (3), the solvent is selected from ethyl acetate or acetone.
[0030] Example 1
[0031] First, benzylamine (176 mmol, 18.85 g) and glyoxal (70.4 mmol, 10.215 g) were weighed, 160 mL of acetonitrile and 8 mL of water were measured, and the acetonitrile and water were mixed uniformly. Under the stirring speed of 500 r / min, benzylamine (122.91 μL / min), glyoxal (50.63 μL / min), and the mixed solution of acetonitrile and water (1.05 mL / min) were fed into CSTR-1 at a specified flow rate by a syringe pump, the reaction temperature was controlled at 12°C, and the reaction time was 40 min. Then, formic acid (7.26 mmol, 0.3795 g) was weighed, and the reaction solution in CSTR-1 was fed into CSTR-2 by a peristaltic pump, while formic acid (2.95 μL / min) was fed into CSTR-2 by a syringe pump, the reaction temperature was controlled at 15°C, and the reaction time was 40 min. During the reaction, the reactor 2 was in a constant temperature water bath, which facilitated the temperature adjustment and the control of the reaction temperature. The obtained product was filtered under reduced pressure by a Buchner funnel, and the filter cake was washed with acetonitrile, and then dried to obtain a crude product, with a yield of 87.56%. Then, the crude product was boiled in acetone, and recrystallized, and the recrystallization temperature was controlled below 70°C, and the refined product was obtained, with a refining yield of 88.62%.
[0032] Figure 2 The DSC graph of the reaction product. Figure 3 The infrared graph of the reaction product. Figure 4 The nuclear magnetic resonance 1H graph of the reaction product, and the nuclear magnetic information of the product is as follows: 1 H NMR (500 MHz, CDCl3) δ 7.26 (s, 72H), 4.13 (s, 27H), 3.99 (s, 1H), 3.58 (s, 10H), 3.48 (s, 37H).
[0033] Experimental Example 2
[0034] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (98.32 μL / min), the glyoxal (35.43 μL / min), the mixed solution of acetonitrile and water (0.84 mL / min) are sent into CSTR-1 through the syringe pump at a specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 50 min, formic acid (8.58 mmol, 0.4485 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 through the peristaltic pump at a certain speed, at the same time, the formic acid (2.79 μL / min) is sent into CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature is controlled at 20 ℃, the reaction is 50 min, and the target product is obtained. During the reaction process, the reactor 2 is in constant temperature water bath, which is convenient for temperature adjustment and reaction temperature control. The obtained product is reduced pressure filtration through the Buchner funnel, and the filter cake is washed with acetonitrile, and dried to obtain the crude product, and the yield is 86.22%; the crude product is boiled in acetone, and is refined by recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 87.42%.
[0035] Experimental Example 3
[0036] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (79.2 mmol, 11.492 g) are weighed, 140 mL of acetonitrile and 7 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (163.88 μL / min), the glyoxal (75.95 μL / min), the mixed solution of acetonitrile and water (1.225 mL / min) are sent into CSTR-1 through the syringe pump at a specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 30 min, formic acid (8.58 mmol, 0.4485 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 through the peristaltic pump at a certain speed, at the same time, the formic acid (4.64 μL / min) is sent into CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature is controlled at 20 ℃, the reaction is 30 min, and the target product is obtained. During the reaction process, the reactor 2 is in constant temperature water bath, which is convenient for temperature adjustment and reaction temperature control. The obtained product is reduced pressure filtration through the Buchner funnel, and the filter cake is washed with acetonitrile, and dried to obtain the crude product, and the yield is 76.82%; the crude product is boiled in acetone, and is refined by recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 86.33%.
[0037] Experimental Example 4
[0038] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (163.88 μL / min), the glyoxal (59.04 μL / min), the mixed solution of acetonitrile and water (1.4 mL / min) are sent into CSTR-1 by the injection pump at the specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 30 min, formic acid (7.26 mmol, 0.3795 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 by the peristaltic pump at a certain speed, at the same time, the formic acid (3.92 μL / min) is sent into CSTR-2 by the injection pump at a certain flow rate, the reaction temperature is controlled at 20 ℃, the reaction is 30 min, and the target product is obtained. During the reaction process, the reactor 2 is in the constant temperature water bath, so as to facilitate the temperature adjustment and the control of the reaction temperature. The obtained product is filtered by a Buchner funnel under reduced pressure, the filter cake is washed with acetonitrile, and the crude product is obtained after drying, and the yield is 84.08%; the crude product is refined by acetone boiling and recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 87.62%.
[0039] Experimental Example 5
[0040] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (163.88 μL / min), the glyoxal (59.04 μL / min), the mixed solution of acetonitrile and water (1.4 mL / min) are sent into CSTR-1 by the injection pump at the specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 30 min, formic acid (7.26 mmol, 0.3795 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 by the peristaltic pump at a certain speed, at the same time, the formic acid (3.92 μL / min) is sent into CSTR-2 by the injection pump at a certain flow rate, the reaction temperature is controlled at 20 ℃, the reaction is 30 min, and the target product is obtained. During the reaction process, the reactor 2 is in the constant temperature water bath, so as to facilitate the temperature adjustment and the control of the reaction temperature. The obtained product is filtered by a Buchner funnel under reduced pressure, the filter cake is washed with acetonitrile, and the crude product is obtained after drying, and the yield is 84.08%; the crude product is refined by acetone boiling and recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 87.62%.
[0041] Experimental Example 6
[0042] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (98.32 μL / min), the glyoxal (35.42 μL / min), the mixed solution of acetonitrile and water (0.84 mL / min) are sent into CSTR-1 through the syringe pump at a specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 50 min, formic acid (8.58 mmol, 0.4485 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 through the peristaltic pump at a certain speed, at the same time, the formic acid (2.79 μL / min) is sent into CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature is controlled at 10 ℃, the reaction is 50 min, and the target product is obtained. During the reaction process, the reactor 2 is in constant temperature water bath, which is convenient for temperature adjustment and reaction temperature control. The obtained product is filtered under reduced pressure through a Buchner funnel, and the filter cake is washed with acetonitrile, and dried to obtain a crude product, and the yield is 80.12%; the crude product is boiled in acetone, and is refined by recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 87.45%.
[0043] Experimental Example 7
[0044] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (98.32 μL / min), the glyoxal (35.42 μL / min), the mixed solution of acetonitrile and water (0.84 mL / min) are sent into CSTR-1 through the syringe pump at a specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 50 min, formic acid (8.58 mmol, 0.4485 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 through the peristaltic pump at a certain speed, at the same time, the formic acid (2.79 μL / min) is sent into CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature is controlled at 10 ℃, the reaction is 50 min, and the target product is obtained. During the reaction process, the reactor 2 is in constant temperature water bath, which is convenient for temperature adjustment and reaction temperature control. The obtained product is filtered under reduced pressure through a Buchner funnel, and the filter cake is washed with acetonitrile, and dried to obtain a crude product, and the yield is 80.12%; the crude product is boiled in acetone, and is refined by recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 87.45%.
[0045] Experimental Example 8
[0046] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (70.4 mmol, 10.215 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (122.91 μL / min), the glyoxal (50.63 μL / min), the mixed solution of acetonitrile and water (1.05 mL / min) are sent into CSTR-1 through the syringe pump at the specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 40 min, formic acid (9.9 mmol, 0.5175 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 through the peristaltic pump at a certain speed, at the same time, the formic acid (4.02 μL / min) is sent into CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature is controlled at 15 ℃, the reaction is 40 min, and the target product is obtained. During the reaction process, the reactor 2 is in the constant temperature water bath, so as to facilitate the temperature adjustment and the control of the reaction temperature. The obtained product is filtered under reduced pressure through the Buchner funnel, the filter cake is washed with acetonitrile, and the crude product is obtained after drying, and the yield is 85.26%; the crude product is refined through acetone boiling and recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 88.19%.
[0047] Experimental Example 9
[0048] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (70.4 mmol, 10.215 g) are weighed, 160 mL of acetonitrile and 8 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (122.91 μL / min), the glyoxal (50.63 μL / min), the mixed solution of acetonitrile and water (1.05 mL / min) are sent into CSTR-1 through the syringe pump at the specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 40 min, formic acid (9.9 mmol, 0.5175 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 through the peristaltic pump at a certain speed, at the same time, the formic acid (4.02 μL / min) is sent into CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature is controlled at 15 ℃, the reaction is 40 min, and the target product is obtained. During the reaction process, the reactor 2 is in the constant temperature water bath, so as to facilitate the temperature adjustment and the control of the reaction temperature. The obtained product is filtered under reduced pressure through the Buchner funnel, the filter cake is washed with acetonitrile, and the crude product is obtained after drying, and the yield is 85.26%; the crude product is refined through acetone boiling and recrystallization, the recrystallization temperature is controlled below 70 ℃, and the refining rate is 88.19%.
[0049] Experimental Example 10
[0050] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 4 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (98.32 μL / min), the glyoxal (35.42 μL / min), the mixed solution of acetonitrile and water (0.82 mL / min) are sent into CSTR-1 by the injection pump at the specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 50 min, formic acid (8.58 mmol, 0.4485 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 by the peristaltic pump at a certain speed, at the same time, the formic acid (2.78 μL / min) is sent into CSTR-2 by the injection pump at a certain flow rate, the reaction temperature is controlled at 10 ℃, the reaction is 50 min, the target product is obtained, during the reaction process, the reactor 2 is in the constant temperature water bath, which is convenient for the temperature adjustment and the control of the reaction temperature. The obtained product is filtered by the Buchner funnel under reduced pressure, the filter cake is washed by acetonitrile, and the crude product is obtained by drying, the yield is 80.15%; the crude product is refined by boiling in ethyl acetate and recrystallization, the recrystallization temperature is controlled below 70 ℃, the refining rate is 85.08%.
[0051] Experimental example 11
[0052] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (61.6 mmol, 8.9332 g) are weighed, 160 mL of acetonitrile and 4 mL of water are measured, the acetonitrile and water are mixed uniformly, under the stirring speed of 500 r / min, the benzylamine (98.32 μL / min), the glyoxal (35.42 μL / min), the mixed solution of acetonitrile and water (0.82 mL / min) are sent into CSTR-1 by the injection pump at the specified flow rate, the reaction temperature is controlled at 12 ℃, the reaction time is 50 min, formic acid (8.58 mmol, 0.4485 g) is measured, the reaction liquid in CSTR-1 is sent into CSTR-2 by the peristaltic pump at a certain speed, at the same time, the formic acid (2.78 μL / min) is sent into CSTR-2 by the injection pump at a certain flow rate, the reaction temperature is controlled at 10 ℃, the reaction is 50 min, the target product is obtained, during the reaction process, the reactor 2 is in the constant temperature water bath, which is convenient for the temperature adjustment and the control of the reaction temperature. The obtained product is filtered by the Buchner funnel under reduced pressure, the filter cake is washed by acetonitrile, and the crude product is obtained by drying, the yield is 80.15%; the crude product is refined by boiling in ethyl acetate and recrystallization, the recrystallization temperature is controlled below 70 ℃, the refining rate is 85.08%.
[0053] Experimental example 11
[0054] Firstly, benzylamine (176 mmol, 18.85 g) and glyoxal (70.4 mmol, 10.215 g) were weighed, 160 mL of acetonitrile and 8 mL of water were measured, and the acetonitrile and water were mixed uniformly. Under the stirring speed of 500 r / min, the benzylamine (122.91 μL / min), the glyoxal (50.63 μL / min), and the mixed solution of acetonitrile and water (1.05 mL / min) were fed into the CSTR-1 through the syringe pump at a specified flow rate, the reaction temperature was controlled at 16 ℃, and the reaction time was 40 min. Then, formic acid (7.26 mmol, 0.3795 g) was weighed, and the reaction solution in the CSTR-1 was fed into the CSTR-2 through the peristaltic pump at a certain speed, while the formic acid (2.94 μL / min) was fed into the CSTR-2 through the syringe pump at a certain flow rate, the reaction temperature was controlled at 20 ℃, and the reaction time was 40 min. During the reaction, the reactor 2 was in the constant temperature water bath, which was convenient for temperature adjustment and reaction temperature control. The obtained product was reduced pressure filtered through a Buchner funnel, and the filter cake was washed with acetonitrile, and then dried to obtain the crude product, and the yield was 82.16%. The crude product was boiled in acetone, and then recrystallized to obtain the refined product, and the recrystallization temperature was controlled below 70 ℃, and the refining rate was 87.64%.
[0055] Comparative Example 1
[0056] In a 100 mL three-necked flask, 40 mL of acetonitrile and 2 mL of water were added as solvents, 5 g of benzylamine and 0.22 g of formic acid were sequentially added, and after stirring for 20 min, 3.05 g of 40% glyoxal aqueous solution was slowly added dropwise, and the feeding time was about 10 min. During the feeding process, the reaction liquid temperature should not exceed 25 ℃, and after the dropwise addition was completed, the room temperature reaction was carried out for 20-30 h, and the final product was obtained. The reaction was filtered, and the filter cake was washed with acetonitrile, and then dried at 60 ℃ to obtain a yellowish crude product. The average yield of multiple repeated experiments was 73%, and then the crude product was boiled in acetone, and then recrystallized to obtain the refined product, and the refining rate was 86-88%.
Claims
1. A process for improving the yield of hexabenzylhexaazaisowurtzitane production, characterized by, The method comprises the following steps: (1) feeding a mixed solution of acetonitrile and water, benzylamine and glyoxal into a first continuous stirred tank reactor through injection pumps simultaneously for mixing and homogeneous reaction, and reacting for a period of time, and the reaction formula is as follows: ； (2) transferring the solution after reaction in step (1) into a second continuous stirred tank reactor through a peristaltic pump, adding an acid as a catalyst, and continuing to react for a period of time to obtain a crude product, and the reaction formula is as follows: ； (3) recrystallizing the crude product obtained in step (2) with a solvent to obtain light yellow needle-shaped crystals; In step (1), the mixed solution of benzylamine, glyoxal, acetonitrile and water is fed into the first continuous stirred tank reactor through injection pumps simultaneously, and the reaction time is 0.5-1.5 hours. In step (2), the acid and the solution after reaction in step (1) are fed into the second continuous stirred tank reactor simultaneously, and the reaction time is 0.5-2 hours.
2. The process of claim 1, wherein the yield of hexabenzylhexaazaisowurtzitane is increased. In step (1), the molar ratio of benzylamine to glyoxal is 2:0.5-2:
1.
3. The process of claim 1, wherein the process is characterized by, In step (1), the volume ratio of acetonitrile to water in the mixed solution of acetonitrile and water is 10:1-40:
1.
4. The process of claim 1, wherein the process is characterized by, In step (1), the reaction temperature in the first continuous stirred tank reactor is controlled at 10-30℃.
5. The process of claim 1, wherein the process is characterized by, In step (2), the acid used is selected from any one of formic acid, acetic acid, sulfamic acid, p-toluenesulfonic acid and benzoic acid.
6. The process of claim 1, wherein the process is characterized by, In step (2), the ratio of the amount of acid added to the molar amount of benzylamine is 0.03:1-0.1:
1.
7. The process of claim 1, wherein the process is characterized by, In step (2), the reaction temperature in the second continuous stirred tank reactor is controlled at 10-30℃.