Application of an organic lead salt, its composition and preparation method

Abstract

The present invention discloses an application of an organic lead salt, a composition thereof and a preparation method thereof. The present invention provides a use of a compound I as a curing accelerator in the field of azide solid propellants. The curing accelerator of the present invention satisfies one or more of the following advantages: having excellent curing performance, maintaining good mechanical properties and combustion properties of the azide composite solid propellant.

Description

Technical Field

[0001] The invention relates to an application of an organic lead salt, a composition thereof and a preparation method thereof. Background Art

[0002] Composite solid propellant is a mixture of various chemical raw materials combined through strictly controlled chemical reactions. Its mechanical properties are determined by a combination of multiple factors. Composite solid propellant may have a long gelation time and curing time, or a high curing temperature, and sometimes even incomplete curing. Therefore, it is usually necessary to add a suitable curing catalyst to solve these problems. Commonly used catalysts include dibutyltin dilaurate, ferric acetone, triethanolamine, triethylamine, triphenylbismuth, etc. After the introduction of triphenyl bismuth, the process performance of the slurry and the mechanical properties of the grain were improved ([1] Wang Guojuan, Sheng Hongliang. Experimental study on curing catalyst of hydroxybutadiene propellant. Shanghai Aerospace, 1993(4):6-8; [2] Tian Dejin. Hydroxyl-terminated polybutadiene composite solid propellant. National University of Defense Technology Paper 52-5001; [3] Tang Hanyang, Study on the influence of styrene on the mechanical storage properties of propellants. Propulsion Technology. 1988(3); [4] Mei Nianhui. Application and performance study of foreign hydroxybutadiene propellants. 1981; [5] USP, 4925504.).

[0003] Usually, the metal organic compound triphenylbismuth (TPB) is used as a curing accelerator, and the propellant charge is cured at 50-60°C. When the propellant charge is cooled to room temperature, thermal stress, i.e., shrinkage stress, will be generated. Ethoxy triphenylbismuth curing catalyst can reduce the curing temperature to 35°C. (

[11] Liu Xunen, Tang Songqing, Chemical Propellants and Polymer Materials, 2004(2), 4-7.

[12] Liu Xunen, Miao Lin, Chen Li, et al. Synthesis and Application of TEPB. Journal of Beijing Institute of Technology, 1995(6):7).

[0004] Azide composite solid propellant is a new type of high-energy solid propellant, the main component of which is azide-containing (-N 3 ) is a prepolymer of adhesive, azide or nitrate plasticizer and high-energy and high-density oxidant. Since the heat of formation of azide adhesive is positive, this type of propellant has high energy, low mechanical sensitivity, good thermal stability and high burning rate. It can be used in high-energy propellants and low-signature propellants.

[0005] At present, the curing accelerator used in azide composite solid propellants is mainly triphenyl bismuth. Given the acidity of the azide propellant system, triphenyl bismuth will decompose during use to produce volatile components such as benzene, which will produce pores during the curing process and affect the mechanical properties and combustion performance of the grain. In addition, with the development of large-scale spacecraft, the demand for large-tonnage charges is increasing, and the difficulty of removing benzene is also increasing. The development of a new curing accelerator is a new technology with universal significance in the development of propellants.

[0006] We invented a new application of a class of organic lead salt compounds and successfully used them in azide composite solid propellant systems, maintaining good process performance and a low pressure index. Summary of the invention

[0007] The technical problem to be solved by the present invention is to overcome one or more of the defects of the existing azide solid propellants, namely, the single type of curing accelerator, the long curing time, the poor mechanical properties or the poor combustion performance of the azide solid propellants. Therefore, the present invention provides an application of an organic lead salt, a composition thereof and a preparation method thereof. The curing accelerator of the present invention satisfies one or more of the following advantages: having excellent curing performance, maintaining the good mechanical properties and combustion performance of the azide composite solid propellant.

[0008] The present invention solves the above technical problems through the following technical solutions.

[0009] The present invention provides a use of a compound I as a curing accelerator in the field of azide solid propellants;

[0010]

[0011] Wherein, R is H, amino, C 1－ C 4 Alkyl, C 1－ C 4 Alkoxy, C 2 -C 6 Alkenyl, C 6 -C 10 Aryl, one or more R 1 -1 Substituted C 1 -C 4 Alkyl or one or more R 1-2 Substituted C 2 -C 6 alkenyl;

[0012] Each R 1-1 are independently halogen;

[0013] Each R 1-2 and phenyl and phenyl substituted with methoxy.

[0014] In one embodiment, in R, the C 1－ C 4 Alkyl, with one or more R 1-1 Substituted C 1 -C 4 C in the alkyl group 1 -C 4 The alkyl group may independently be methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl or tert-butyl, preferably methyl.

[0015] In one embodiment, in R, the C 1－ C 4 The alkoxy group may be methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, isobutoxy or tert-butoxy, preferably methoxy.

[0016] In one embodiment, in R, the C 2 -C 6 The alkenyl group may be vinyl, n-propenyl or isopropenyl, preferably vinyl.

[0017] In one embodiment, in R, the C 6 -C 10 The aryl group may be phenyl or naphthyl, preferably phenyl.

[0018] In one scenario, R 1-1 In the above, the halogen may be fluorine, chlorine, bromine or iodine, preferably fluorine.

[0019] In one embodiment, R is H or is replaced by one or more R 1-2 Substituted C 2 -C 6 Alkenyl, the R 1-2 is independently phenyl substituted with methoxy.

[0020] In a certain embodiment, R is H, methoxy, phenyl, methyl, vinyl, 2-p-methoxyphenylvinyl, amino or trifluoromethyl; preferably H or 2-p-methoxyphenylvinyl; more preferably 2-p-methoxyphenylvinyl.

[0021] In a certain embodiment, the compound I is any of the following structures:

[0022]

[0023]

[0024] Preferably

[0025] The present invention provides an azide solid propellant, the raw materials of which include the following components in parts by mass: 7.5 to 13.5 parts of azide rubber, 0.5 to 0.9 parts of triisocyanate (TDI), 0.04 to 0.06 parts of compound I, 4.2 to 7.8 parts of nitrate ester, 1.4 to 2.6 parts of plasticizer, 15 to 19 parts of fuel and 56 to 66 parts of oxidant;

[0026] Wherein, the definition of compound I is as described above.

[0027] In a certain embodiment, the nitrate ester is conventional in the art, preferably 2,2-dinitropropanol formal and / or 2,2-dinitropropanol acetal; more preferably, an equal mass mixture of 2,2-dinitropropanol formal and 2,2-dinitropropanol acetal.

[0028] In a certain embodiment, the mass fraction of the nitrate ester may be 4.2 to 7.8 parts, preferably 6 parts.

[0029] In a certain embodiment, the plasticizer is conventional in the art, and preferably dioctyl sebacate.

[0030] In a certain embodiment, the mass fraction of the plasticizer may be 1.4 to 2.6 parts, preferably 2 parts.

[0031] In a certain embodiment, the fuel is conventional in the art, preferably aluminum powder.

[0032] In a certain embodiment, the mass fraction of the fuel may be 15 to 19 parts, preferably 17 parts.

[0033] In a certain embodiment, the oxidant is conventional in the art, preferably ammonium perchlorate.

[0034] In a certain embodiment, the weight fraction of the oxidant may be 56 to 66 parts, preferably 61 parts.

[0035] In a certain embodiment, the mass fraction of the azide rubber may be 7.5 to 13.5 parts, preferably 10.5 parts.

[0036] In a certain embodiment, the mass fraction of the diisocyanate may be 0.5 to 0.9 parts, preferably 0.7 parts.

[0037] In a certain embodiment, the mass fraction of the compound I may be 0.04 to 0.06 parts, preferably 0.05 parts.

[0038] In one embodiment, the azide solid propellant is prepared by the following method: mixing the raw materials, vacuum degassing, and solidifying.

[0039] In a certain embodiment, the raw materials of the azide solid propellant are composed of the following components in parts by mass: 10.5 parts of azide rubber, 0.7 parts of diisocyanate, 0.05 parts of compound I, 6 parts of nitrate ester, 2 parts of dioctyl sebacate, 17 parts of aluminum powder, and 61 parts of ammonium perchlorate;

[0040] Wherein, the nitrate ester is a mixture of 2,2-dinitropropanol formal and 2,2-dinitropropanol acetal in equal mass;

[0041] The compound I is

[0042]

[0043] Preferably

[0044]

[0045] The present invention provides a method for preparing a compound I, comprising the following steps: in water, reacting a compound I-1 with a lead salt in a continuous flow reactor as shown below to obtain the compound I;

[0046]

[0047] Wherein, R is defined as above; and compound I is defined as above.

[0048] In a certain embodiment, the lead salt may be lead acetate or lead nitrate; preferably lead nitrate.

[0049] In one embodiment, the molar volume ratio of the lead salt to the water may be 0.1 mol / L-1.5 mol / L, preferably 0.5 mol / L-1.0 mol / L, for example 1.0 mol / L.

[0050] In one embodiment, the molar ratio of the compound I-1 to the lead salt may be (2:0.9)-(2:1.1); preferably 2:1.

[0051] In a certain embodiment, the molar volume ratio of the compound I-1 to the water can be 0.1 mol / L-3 mol / L, preferably 1 mol / L-2.0 mol / L, for example 2.0 mol / L.

[0052] In a certain embodiment, the reaction temperature of the reaction may be 0°C to 100°C, preferably 50°C to 90°C, for example 50°C to 70°C.

[0053] In a certain embodiment, the stirring frequency of the continuous flow reactor is 5-40 Hz, preferably 10-25 Hz.

[0054] In one embodiment, the compound I-1 and / or the lead salt are respectively introduced into the continuous flow reactor through an injection pump.

[0055] In one embodiment, the flow rate of the compound I-1 and the lead salt entering the continuous flow reactor can be 10 mL / min-100 ml / min; preferably 25 mL / min-50 ml / min; for example 50 ml / min.

[0056] In a certain embodiment, the residence time of the reaction may be 5-25 min, such as 5-10 min.

[0057] In a certain embodiment, in the reaction, the molar volume ratio of the lead salt to the water can be 0.1 mol / L-1.5 mol / L; the molar ratio of the compound I-1 to the lead salt can be (2:0.9)-(2:1.1); the reaction temperature of the reaction can be 0°C to 100°C; the stirring frequency of the continuous flow reactor is 5-40 Hz; the flow rate of the compound I-1 and the lead salt entering the continuous flow reactor can be 10 mL / min-100 ml / min; the residence time of the reaction can be 5-25 min.

[0058] In a certain embodiment, after the reaction is completed, the following post-treatment steps may be further included: filtration, water washing, and drying.

[0059] Without violating the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.

[0060] The reagents and raw materials used in the present invention are commercially available.

[0061] The positive and progressive effects of the present invention are: the preparation method of the organic lead salt of the present invention has a high yield; the azide composite solid propellant of the present invention has a low curing temperature and a short curing time, good compatibility of the grain column, good process performance and good mechanical properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0062] Figure 1 This is the single crystal spectrum of compound PB1.

[0063] Figure 2 This is the single crystal spectrum of compound PB1. DETAILED DESCRIPTION

[0064] The present invention is further described below by way of examples, but the present invention is not limited to the scope of the examples. The experimental methods in the following examples without specifying specific conditions are carried out according to conventional methods and conditions, or selected according to the product specifications.

[0065] Example 1 Preparation of organic lead salt compounds

[0066] PB1: 8-Hydroxyquinoline Lead

[0067] Prepare 8-hydroxyquinoline sodium aqueous solution and lead nitrate aqueous solution.

[0068] 1) Process temperature screening

[0069] The initial molar ratio of 8-hydroxyquinoline sodium: lead salt is 2:1, the concentration of lead salt is 0.5 mol / L, the flow rate of 8-hydroxyquinoline sodium is 25 mL / min, the flow rate of lead salt is 25 mL / min, and they enter the continuous flow reactor (500 ml) through the injection pump, the residence time is 10 min, and the stirring frequency is 25 Hz. The temperature is investigated under the conditions. After filtration, washing and drying, the product PB1 is obtained. The single crystal data is as follows Figure 1 and Figure 2 shown.

[0070] Table 1 Process temperature screening

[0071] serial number Temperature(℃) Yield (%) Pb element content (%) 1 30 75 41.9 2 50 86 42.1 3 70 85 41.9 4 90 86 42.0

[0072] Qualified products with lead content can be obtained at different temperatures. Combined with the yield data and energy consumption, 50°C was selected as the optimal temperature for the following research.

[0073] 2) Reactant concentration screening

[0074] The optimal temperature for the temperature selection is 50°C, the initial molar ratio of 8-hydroxyquinoline sodium: lead salt is 2:1, the flow rate of 8-hydroxyquinoline sodium is 25mL / min, the flow rate of lead salt is 25mL / min, the residence time is 10min, and the stirring frequency is 25Hz. After filtration, washing and drying, the product PB1 is obtained, and its single crystal data is the same as "1) Process temperature screening" in Example 1.

[0075] Table 2 Process concentration screening

[0076]

[0077]

[0078] As the concentration increases, the reaction yield increases accordingly. Considering the solubility of the lead salt, the maximum concentration is selected at 1.0 mol / L.

[0079] 3) Screening of residence time in continuous flow reactor

[0080] The temperature was 50°C, the initial molar ratio of 8-hydroxyquinoline sodium: lead salt was 2:1, the concentration of lead salt was 1.0 mol / L, and the stirring frequency was 25 Hz. After filtration, washing and drying, the product PB1 was obtained, and its single crystal data was the same as that in "1) Process Temperature Screening" in Example 1.

[0081] Table 3 Residence time screening

[0082]

[0083] The shortened residence time had little effect on the reaction yield. Considering the production efficiency, a residence time of 5 min was selected for subsequent research.

[0084] 4) Screening of stirring frequency

[0085] The temperature is 50°C, the initial molar ratio of 8-hydroxyquinoline sodium: lead salt is 2:1, the concentration of lead salt is 1.0 mol / L, the flow rate of 8-hydroxyquinoline sodium is 50 ml / min, and the flow rate of lead salt is 50 ml / min. After filtration, washing and drying, the product PB1 is obtained, and its single crystal data is the same as "1) Process temperature screening" in Example 1.

[0086] Table 4 Stirring frequency screening

[0087]

[0088] Based on the above research, the continuous flow synthesis process of lead salt catalyst is as follows: the initial molar ratio of 8-hydroxyquinoline sodium: lead salt is 2:1, the reaction temperature is 50°C, the concentration of lead salt is 1 mol / L, the flow rate of 8-hydroxyquinoline sodium is 50 ml / min, the flow rate of lead salt is 50 ml / min, the stirring frequency is 25 Hz, and the organic lead salt catalyst is obtained with a yield of >90%.

[0089] PB2: 2-methoxy-8-hydroxyquinoline lead

[0090] Prepare 2-methoxy-8-hydroxyquinoline sodium aqueous solution and lead nitrate aqueous solution. 2-methoxy-8-hydroxyquinoline sodium: lead salt molar ratio = 2:1, reaction temperature 50 ° C, lead salt concentration 1 mol / L, 2-methoxy-8-hydroxyquinoline sodium flow rate 50ml / min, lead salt flow rate 50ml / min, residence time 5min, stirring frequency 25Hz. After filtering, washing, drying, 2-methoxy-8-hydroxyquinoline lead salt compound is obtained with a yield of 90%.

[0091] PB3: 2-phenyl-8-hydroxyquinoline lead

[0092] Prepare 2-phenyl-8-hydroxyquinoline sodium aqueous solution and lead nitrate aqueous solution. 2-phenyl-8-hydroxyquinoline sodium: lead salt molar ratio = 2:1, reaction temperature 50 ° C, lead salt concentration 1 mol / L, 2-phenyl-8-hydroxyquinoline sodium flow rate 50ml / min, lead salt flow rate 50ml / min, residence time 5min, stirring frequency 25Hz. After filtering, washing, drying, 2-phenyl-8-hydroxyquinoline lead salt compound is obtained with a yield of 95%.

[0093] PB4: 2-methyl-8-hydroxyquinoline lead

[0094] Prepare 2-methyl-8-hydroxyquinoline sodium aqueous solution and lead nitrate aqueous solution. 2-methyl-8-hydroxyquinoline sodium: lead salt molar ratio = 2:1, reaction temperature 50 ° C, lead salt concentration 1 mol / L, 2-methyl-8-hydroxyquinoline sodium flow rate 50ml / min, lead salt flow rate 50ml / min, residence time 5min, stirring frequency 25Hz. After filtering, washing, drying, 2-methyl-8-hydroxyquinoline lead salt compound is obtained with a yield of 95%.

[0095] PB5: 2-vinyl-8-hydroxyquinoline lead

[0096] Prepare an aqueous solution of 2-vinyl-8-hydroxyquinoline sodium and an aqueous solution of lead nitrate. The molar ratio of 2-vinyl-8-hydroxyquinoline sodium to lead salt is 2:1, the reaction temperature is 50°C, the concentration of the lead salt is 1 mol / L, the flow rate of 2-vinyl-8-hydroxyquinoline sodium is 50 ml / min, the flow rate of the lead salt is 50 ml / min, the residence time is 5 min, and the stirring frequency is 25 Hz. After filtering, washing with water, and drying, a 2-vinyl-8-hydroxyquinoline lead salt compound is obtained with a yield of 85%.

[0097] PB6: 2-p-methoxyphenylvinyl-8-hydroxyquinoline lead

[0098]

[0099] Prepare an aqueous solution of 2-p-methoxyphenylvinyl-8-hydroxyquinoline sodium and an aqueous solution of lead nitrate. The molar ratio of 2-p-methoxyphenylvinyl-8-hydroxyquinoline sodium to lead salt is 2:1, the reaction temperature is 50°C, the concentration of the lead salt is 1 mol / L, the flow rate of 2-p-methoxyphenylvinyl-8-hydroxyquinoline sodium is 50 ml / min, the flow rate of the lead salt is 50 ml / min, the residence time is 5 min, and the stirring frequency is 25 Hz. After filtering, washing with water, and drying, a 2-p-methoxyphenylvinyl-8-hydroxyquinoline lead salt compound is obtained with a yield of 65%.

[0100] PB7: 2-amino-8-hydroxyquinoline lead

[0101] Prepare 2-amino-8-hydroxyquinoline sodium aqueous solution and lead nitrate aqueous solution. 2-amino-8-hydroxyquinoline sodium: lead salt molar ratio = 2:1, reaction temperature 50 ° C, lead salt concentration 1 mol / L, 2-amino-8-hydroxyquinoline sodium flow rate 50ml / min, lead salt flow rate 50ml / min, residence time 5min, stirring frequency 25Hz. After filtering, washing, drying, 2-amino-8-hydroxyquinoline lead salt compound is obtained with a yield of 91%.

[0102] PB8: 2-Trifluoromethyl-8-hydroxyquinoline lead

[0103] Prepare 2-trifluoromethyl-8-hydroxyquinoline sodium aqueous solution and lead nitrate aqueous solution. 2-trifluoromethyl-8-hydroxyquinoline sodium: lead salt molar ratio = 2:1, reaction temperature 50 ° C, lead salt concentration 1 mol / L, 2-trifluoromethyl-8-hydroxyquinoline sodium flow rate 50ml / min, lead salt flow rate 50ml / min, residence time 5min, stirring frequency 25Hz. After filtering, washing, drying, 2-trifluoromethyl-8-hydroxyquinoline lead salt compound was obtained with a yield of 86%.

[0104] Example 2

[0105] The basic formula of the experiment is: polyurethane rubber (PBT) / triisocyanate (TDI) / curing accelerator (organic lead salt PB) / nitrate (A) / plasticizer (KZ) / aluminum powder (Al) / ammonium perchlorate (AP). The basic composition of the formula is shown in Table 5.

[0106] The nitrate ester (A) is a mixture of 2,2-dinitropropanol formal and 2,2-dinitropropanol acetal in equal amounts; and the plasticizer (KZ) is dioctyl sebacate.

[0107] Table 5 Main ingredients of basic formula

[0108] Components PBT TDI PB A KZ Al AP Mass fraction 10.5 0.7 0.05 6 2 17 61

[0109] Preparation of film samples: PBT, TDI, PB, A, KZ, Al and AP were mixed mechanically for 10 minutes (paste), degassed at 25°C vacuum (30 mmHg) for 3 hours, and then cured in ovens at 25°C and 35°C, and the appearance of the samples was observed and the samples were measured with a LX-A type Shore hardness tester (standard: GB / T531-1999 "Rubber pocket hardness tester indentation hardness test method"), and the Shore hardness of different curing times was determined according to the process requirements. When the Shore hardness was greater than 30HA, the system was considered to have been cured. The results are shown in Table 6.

[0110] Table 6 Fully cured data

[0111]

[0112] The data in Table 6 show that the lead salts we tested are basically better than triphenylbismuth (TPB) in curing time at both temperatures, among which PB1 and PB6 have very significant improvements.

[0113] Example 3

[0114] The engine charge was mixed using a 5L vertical mixer and the slurry was vacuum cast. The mechanical properties of the resulting drug column are shown in Table 7.

[0115] Table 7 Mechanical properties of propellants

[0116]

[0117] It can be seen from Table 7 that 0.05% PB6 increases the tensile strength of the propellant by 0.1 MPa.

[0118] Example 4

[0119] Using PB6 as a curing accelerator, the test engine charge was carried out using the formula composition in Table 5, a 25L vertical mixer was used for mixing, and the slurry was cast by vacuum casting. The resulting powder column was tested with a standard engine BSFΦ118: the propellant burning rate was 9mm / s (20℃, 6MPa), and the burning rate pressure index was 0.3 at a working pressure of 6-18MPa.

Claims

1. Use of compound I as a curing accelerator in the field of azide solid propellants; in, R is H, amino, C 1－ C 4 Alkyl, C 1－ C 4 Alkoxy, C 2 -C 6 Alkenyl, C 6 -C 10 Aryl, one or more R 1-1 Substituted C 1 -C 4 Alkyl or one or more R 1-2 Substituted C 2 -C 6 alkenyl; Each R 1-1 are independently halogen; Each R 1-2 and phenyl and phenyl substituted with methoxy.

2. The use according to claim 1, It is characterized in that It meets one or more of the following conditions: (1) In R, the C 1－ C 4 Alkyl, with one or more R 1-1 Substituted C 1 -C 4 C in the alkyl group 1 -C 4 Alkyl is independently methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl or tert-butyl; (2) In R, the C 1－ C 4 Alkoxy is methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, isobutoxy or tert-butoxy; (3) In R, the C 2 -C 6 Alkenyl is vinyl, n-propenyl or isopropenyl; (4) In R, the C 6 -C 10 Aryl is phenyl or naphthyl; (5)R 1-1 wherein the halogen is fluorine, chlorine, bromine or iodine.

3. The use according to claim 2, It is characterized in that It meets one or more of the following conditions: (1) In R, the C 1－ C 4 Alkyl, with one or more R 1-1 Substituted C 1 -C 4 C in the alkyl group 1 -C 4 Alkyl is independently methyl; (2) In R, the C 1－ C 4 Alkoxy is methoxy; (3) In R, the C 2 -C 6 Alkenyl is vinyl; (4) In R, the C 6 -C 10 Aryl is phenyl; (5)R 1-1 wherein the halogen is fluorine.

4. The use according to claim 1, It is characterized in that The R is H or one or more R 1-2 Substituted C 2 -C 6 Alkenyl, the R 1-2 is independently phenyl substituted with methoxy.

5. The use according to claim 1, It is characterized in that The R is H, methoxy, phenyl, methyl, vinyl, 2-p-methoxyphenylvinyl, amino or trifluoromethyl.

6. The use according to claim 5, It is characterized in that The R is H or 2-p-methoxyphenylvinyl.

7. The use according to claim 6, It is characterized in that The R is 2-p-methoxyphenylvinyl.

8. The use according to claim 1, It is characterized in that The compound I is any of the following structures:

9. The use according to claim 8, It is characterized in that The compound I is 10. An azide solid propellant, It is characterized in that The raw materials include the following components by mass: 7.5 to 13.5 parts of azide rubber, 0.5 to 0.9 parts of diisocyanate, 0.04 to 0.06 parts of compound I, 4.2 to 7.8 parts of nitrate, 1.4 to 2.6 parts of plasticizer, 15 to 19 parts of fuel and 56 to 66 parts of oxidant, Wherein, the definition of compound I is as described in any one of claims 1-9.

11. The azide solid propellant according to claim 10, It is characterized in that It meets one or more of the following conditions: (1) The nitrate ester is 2,2-dinitropropanol formal and / or 2,2-dinitropropanol acetal; (2) The mass fraction of the nitrate ester is 4.2 to 7.8 parts; (3) The plasticizer is dioctyl sebacate; (4) The mass fraction of the plasticizer is 1.4 to 2.6 parts; (5) The fuel is aluminum powder; (6) The mass fraction of the fuel is 15 to 19 parts; (7) The oxidant is ammonium perchlorate; (8) The mass fraction of the oxidant is 56 to 66 parts; (9) The mass fraction of the azide rubber is 7.5 to 13.5 parts; (10) The mass fraction of the diisocyanate is 0.5 to 0.9 parts; (11) The mass fraction of the compound I is 0.04 to 0.06 parts; (12) The azide solid propellant is prepared according to the following method: mixing the raw materials, vacuum degassing, and solidifying.

12. The azide solid propellant according to claim 11, It is characterized in that It meets one or more of the following conditions: (1) The nitrate ester is a mixture of 2,2-dinitropropanol formal and 2,2-dinitropropanol acetal in equal weight; (2) The mass fraction of the nitrate ester is 6 parts; (3) The mass fraction of the plasticizer is 2 parts; (4) The mass fraction of the fuel is 17 parts; (5) The mass fraction of the oxidant is 61 parts; (6) The mass fraction of the azide rubber is 10.5 parts; (7) The mass fraction of the diisocyanate is 0.7 parts; (8) The mass fraction of the compound I is 0.05 parts.

13. The azide solid propellant according to any one of claims 10 to 12, It is characterized in that The raw materials of the azide solid propellant are composed of the following components in parts by mass: 10.5 parts of azide rubber, 0.7 parts of diisocyanate, 0.05 parts of compound I, 6 parts of nitrate ester, 2 parts of dioctyl sebacate, 17 parts of aluminum powder, and 61 parts of ammonium perchlorate; Wherein, the nitrate ester is a mixture of 2,2-dinitropropanol formal and 2,2-dinitropropanol acetal in equal mass; The compound I is 14. The azide solid propellant according to claim 13, It is characterized in that The compound I is 15. A method for preparing compound I, It is characterized in that The method comprises the following steps: in water, reacting compound I-1 with lead salt in a continuous flow reactor to obtain compound I; Wherein, the definition of R is as described in any one of claims 1-9; the definition of compound I is as described in any one of claims 1-9.

16. The preparation method according to claim 15, It is characterized in that It meets one or more of the following conditions: (1) The lead salt is lead acetate or lead nitrate; (2) the molar volume ratio of the lead salt to the water is 0.1 mol / L-1.5 mol / L; (3) The molar ratio of the compound I-1 to the lead salt is (2:0.9)-(2:1.1); (4) The molar volume ratio of the compound I-1 to the water is 0.1 mol / L-3 mol / L; (5) The reaction temperature of the reaction is 0°C to 100°C; (6) The stirring frequency of the continuous flow reactor is 5-40 Hz; (7) The compound I-1 and the lead salt are respectively introduced into a continuous flow reactor through an injection pump; (8) The flow rate of the compound I-1 and / or the lead salt entering the continuous flow reactor is 10 mL / min-100 ml / min; (9) The residence time of the reaction is 5-25 min; (10) After the reaction is completed, the following post-treatment steps are also included: filtration, water washing, and drying.

17. The preparation method according to claim 16, It is characterized in that It meets one or more of the following conditions: (1) The lead salt is lead nitrate; (2) the molar volume ratio of the lead salt to the water is 0.5 mol / L-1.0 mol / L; (3) The molar ratio of the compound I-1 to the lead salt is 2:1; (4) The molar volume ratio of the compound I-1 to the water is 1 mol / L-2.0 mol / L; (5) The reaction temperature of the reaction is 50°C to 90°C; (6) The stirring frequency of the continuous flow reactor is 10 to 25 Hz; (7) The flow rate of the compound I-1 and / or the lead salt entering the continuous flow reactor is 25 mL / min-50 ml / min; (8) The residence time of the reaction is 5-10 min.

18. The preparation method according to claim 17, It is characterized in that It meets one or more of the following conditions: (1) The molar volume ratio of the lead salt to the water is 1.0 mol / L; (2) The molar volume ratio of the compound I-1 to the water is 2.0 mol / L; (3) The reaction temperature of the reaction is 50°C to 70°C; (4) The flow rate of the compound I-1 and / or the lead salt entering the continuous flow reactor is 50 ml / min.

19. The preparation method according to any one of claims 15 to 18, It is characterized in that The molar volume ratio of the lead salt to the water is 0.1 mol / L-1.5 mol / L; the molar ratio of the compound I-1 to the lead salt is (2:0.9)-(2:1.1); the reaction temperature of the reaction is 0°C to 100°C; the stirring frequency of the continuous flow reactor is 5-40 Hz; the flow rate of the compound I-1 and the lead salt entering the continuous flow reactor is 10 mL / min-100 ml / min; the residence time of the reaction is 5-25 min.

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