A method for synthesizing a diketone hydrazone

Abstract

This invention provides a method for synthesizing methyl ethyl ketone (MEK) azide, which introduces a nonionic surfactant into the traditional hydrogen peroxide reaction system. The specific reaction system includes raw materials, a catalyst, an oxidant, and an auxiliary agent: the raw materials include MEK and ammonia, the oxidant is hydrogen peroxide, the catalyst is an amide compound, and the auxiliary agent is a nonionic surfactant. Preferably, disodium EDTA can also be introduced into the hydrogen peroxide. By introducing the auxiliary agent to modify the reaction system environment, the effective contact area between the reactants can be significantly increased, ensuring a more uniform and rapid synthesis reaction. It can also lower the reaction temperature for synthesizing MEK azide, reducing energy consumption while improving reaction efficiency and the yield of MEK azide.

Description

Technical Field

[0001] This invention belongs to the field of chemical synthesis technology, and mainly relates to a method for synthesizing butanone and hydrazine hydrate. Background Technology

[0002] Ketone azides are an intermediate in the preparation of hydrazine hydrate. Hydrazine hydrate and the corresponding ketone are obtained through the hydrolysis of ketrazine azides. Hydrazine hydrate, also known as hydrated hydrazine, is a colorless, oily liquid with a faint ammonia odor. It is a widely used chemical raw material and an important chemical product. In the pharmaceutical industry, it is commonly used in the production of anti-tuberculosis and anti-diabetic drugs; in pesticide synthesis, it is used to produce herbicides, plant growth regulators, and insecticides and fungicides; in the chemical industry, it is used to produce various foaming agents and cleaning agents for boilers or reaction vessels; high-concentration hydrazine hydrate is mainly used in the military industry for the production of rocket fuel and energetic materials.

[0003] There are four main industrial production methods for hydrazine hydrate: the Raschig process, the urea process, the ketazine process, and the hydrogen peroxide process. The Raschig process uses sodium hypochlorite (obtained by passing chlorine gas through a supersaturated sodium hydroxide solution) as an oxidant to oxidize ammonia and obtain a low-concentration hydrazine hydrate solution. This method has a low product yield (65%, based on sodium hypochlorite) and high energy consumption, and has been phased out. The urea process uses urea as a nitrogen source, reacting with sodium hypochlorite to produce hydrazine hydrate, with a yield of approximately 70% (based on sodium hypochlorite). This method is energy-intensive and produces a large amount of ammonia nitrogen byproducts. The ketazine process is a modified Raschig process, proposed and applied industrially by Bayer AG in Germany. It involves introducing acetone during the reaction of ammonia and sodium hypochlorite to form a more stable acetone-azo intermediate, which is then separated and hydrolyzed to obtain the hydrazine hydrate product. This method has a high hydrazine hydrate yield (90%, based on sodium hypochlorite), but requires the recycling of large amounts of ammonia during production, resulting in high energy consumption. Furthermore, all three methods mentioned above require the use of strong alkalis such as sodium hydroxide and chlorine, which not only causes equipment corrosion but also produces large amounts of waste brine. Currently, the domestic industrial production of hydrazine hydrate mainly uses the urea method and the ketone azide method.

[0004] The hydrogen peroxide process uses hydrogen peroxide instead of sodium hypochlorite as the oxidant, amide as the catalyst, ammonium ketone as the co-catalyst, and methyl ethyl ketone (MEK) and ammonia as raw materials. First, the intermediate MEK azide is synthesized, and then MEK azide is hydrolyzed at high temperature to produce hydrazine hydrate. This method avoids the use of highly corrosive chlorine gas and sodium hydroxide, and does not produce waste brine, making it a green and environmentally friendly production process. The production of hydrazine hydrate using the hydrogen peroxide process has gradually become recognized as the most promising technology in the industry and has been successfully applied abroad.

[0005] In patent US6562311, acetamide-ammonium acetate was used as the catalytic system, butanone and ammonia were used as raw materials, and 70% hydrogen peroxide was used as the oxidant. The reaction was carried out at 50℃ for 7 hours, and the yield of butanone azide was 81.0%. Shen Jun et al. of East China University of Science and Technology (Study on the synthesis process of butanone azide, intermediate of hydrazine hydrate [J]. Fine Chemical Intermediates, 2008, 38(3):3) investigated the process conditions such as catalyst type, reaction temperature and reaction time. Finally, formamide was used as the catalyst, butanone and ammonia were used as raw materials, 27.5% hydrogen peroxide was used as the oxidant, and the reaction was carried out at 60℃ for 6 hours, and the yield of butanone azide was 83.5%. Similarly, Gu Chunsi et al. of East China University of Science and Technology (Study on the process of synthesizing butanone azide by hydrogen peroxide [J]. Chemical Reagents, 2018, 40(1):5) further optimized the above formamide catalytic reaction system, and the yield of butanone azide was increased to 87.0%.

[0006] In summary, in existing industrial production facilities, the yield of methyl ethyl ketone (MEK) in the synthesis of MEK is generally 80-87%, and product yield remains a major challenge restricting industrial production. Summary of the Invention

[0007] During the research, it was found that improvements to the existing technology for the synthesis of methyl ethyl ketone (MEK) azide mainly focus on the catalyst system, such as combining other co-catalyst components with amide catalysts to form improved catalyst systems. After in-depth research on the reaction system, the applicant believes that for the synthesis of MEK azide from MEK, due to the limited solubility of MEK in water, which further decreases with increasing temperature, and the insoluble MEK azide produced, the reaction system is a two-phase system including an oil phase and an aqueous phase. MEK and the product MEK azide are mainly in the oil phase; ammonia, the catalyst amide, and the oxidant hydrogen peroxide are all present in the aqueous phase. The synthesis reaction mainly occurs at the water-oil phase interface. However, in existing methyl ethyl ketone (MEK) azide synthesis processes, the reaction is mainly carried out under conditions of uniform mixing and the formation of a turbid liquid (or emulsion) through stirring. In this system, the contact area between the aqueous and oil phases is very limited, and the addition of hydrogen peroxide easily leads to localized, violent reactions. The heat released from the reaction generates high temperatures, causing the MEK and ammonia in the raw materials to volatilize and be lost, and the hydrogen peroxide to decompose, thus reducing the efficiency of the MEK azide synthesis reaction and the product yield. Based on the above understanding, the applicant proposes a novel approach to adjust the reaction system, providing a synthesis method that introduces a nonionic surfactant into the synthesis process.

[0008] To address the shortcomings of the prior art, the core objective of this invention is to provide a method for synthesizing methyl ethyl ketone (MEK). This method introduces a nonionic surfactant as an auxiliary agent to modulate the reaction system environment, which can significantly increase the effective contact area between reactants, ensuring a more uniform and rapid synthesis reaction. It can also reduce the reaction temperature for synthesizing MEK, thereby reducing energy consumption while improving reaction efficiency and the yield of MEK.

[0009] This invention is achieved through the following technical solution:

[0010] The reaction equation for synthesizing butanone azide from butanone is as follows:

[0011] 2CH3COC2H5+2NH3+H2O2→CH3(C2H5)C=NN=C(C2H5)CH3+4H2O

[0012] This invention provides a method for synthesizing butanone azo, which involves introducing a nonionic surfactant into the traditional hydrogen peroxide reaction system. The specific reaction system includes raw materials, a catalyst, an oxidant, and an auxiliary agent: the raw materials include butanone and ammonia, the oxidant is hydrogen peroxide, the catalyst is an amide compound, and the auxiliary agent is a nonionic surfactant. Preferably, disodium EDTA can also be introduced into the hydrogen peroxide as a stabilizer to reduce the natural decomposition of hydrogen peroxide.

[0013] Specifically, the present invention provides a method for synthesizing butanone azohydramine, the method comprising the following steps:

[0014] (1) Mix methyl ethyl ketone, ammonia, catalyst and nonionic surfactant evenly to form the first material stream;

[0015] (2) Under reaction conditions, an oxidant is introduced into the first feed stream and the reaction is carried out;

[0016] (3) After the reaction in step (2) is completed, an organic solvent is added for separation and extraction. After standing and layering, the upper layer is an organic phase (containing unreacted methyl ethyl ketone and the product methyl ethyl ketone azo).

[0017] In the above-mentioned method for synthesizing butanone, as some specific embodiments, the mass concentration of ammonia water is generally 20% to 30%, preferably 25% to 28%.

[0018] In the above-mentioned method for synthesizing butanone azo, as some specific embodiments, the catalyst is an amide compound, specifically selected from at least one of formamide, acetamide, propionamide, and dimethylformamide, preferably formamide.

[0019] In the above-mentioned method for synthesizing butanone azo, as some specific embodiments, the nonionic surfactant is fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine and polyether, etc., specifically selected from one or more of the Brij series polyoxyethylene lauryl ether (Brij-30), polyethylene glycol hexadecyl ether (Brig-56) and polyoxyethylene ether (Brij-58), preferably polyoxyethylene lauryl ether (Brij-30).

[0020] In the above-mentioned method for synthesizing butanone azo, as some specific embodiments, the reaction conditions in step (2) are as follows: the reaction temperature is 20-50℃, preferably 30-40℃; the reaction time is 1-5h.

[0021] In the above method for synthesizing butanone azo, as some specific embodiments, the oxidant in step (2) is a hydrogen peroxide solution, preferably a hydrogen peroxide solution containing disodium EDTA; the concentration of the hydrogen peroxide solution is 27.5wt% to 30wt%; the content of disodium EDTA in the hydrogen peroxide solution containing disodium EDTA is 0.1 to 1.0 g / mol of hydrogen peroxide, preferably 0.3 to 0.5 g / mol.

[0022] In the above-mentioned method for synthesizing butanone, as some specific implementation methods, the oxidant in step (2) is introduced by slow addition, specifically by dripping, and the addition can be completed within 1 to 2 hours.

[0023] In the above-mentioned method for synthesizing butanone azo, as some specific embodiments, the amount of nonionic surfactant used is 10% to 50% of the mass of butanone.

[0024] In the above-mentioned method for synthesizing butanone azo, as some specific embodiments, the separation solvent in step (3) is an organic solvent, specifically one or more of cyclohexane, n-hexane, toluene, and xylene, preferably xylene.

[0025] In the above-mentioned method for synthesizing butanone, as some specific embodiments, the molar ratio of butanone to hydrogen peroxide is 3 to 6:1.

[0026] In the above-mentioned method for synthesizing butanone, as some specific embodiments, the molar ratio of ammonia to hydrogen peroxide is 2 to 4:1.

[0027] In the above-mentioned method for synthesizing butanone, as some specific embodiments, the molar ratio of formamide to hydrogen peroxide is 2 to 4:1.

[0028] Compared with the prior art, the method for synthesizing butanone azohydramine provided by the present invention has one or more or all of the following advantages:

[0029] 1. This invention provides a novel method for the synthesis of butanone (MEK) azohydride. By introducing a nonionic surfactant into the reaction system, the aqueous phase, composed of ammonia and formamide, is encapsulated by nonionic surfactant molecules within the MEK oil phase, forming nanoscale droplets. The certain solubility of MEK in water allows it to also act as a co-surfactant in this system, making the entire water-in-oil system more stable. Unlike the traditional hydrogen peroxide method where the reaction solution separates into oil and water, the water-in-oil reaction system in this invention is macroscopically a clear and transparent solution. The introduced hydrogen peroxide then uniformly enters the aqueous droplets and reacts, greatly increasing the reaction contact area and reducing side reactions, thereby improving the efficiency and yield of the product synthesis.

[0030] 2. The method for synthesizing butanone azo provided by the present invention has high reaction efficiency and can obtain the target product at a lower reaction temperature and a shorter reaction time. Compared with the usual reaction temperature (50-60℃) in the prior art, the reaction temperature is reduced by 20-30℃. Attached Figure Description

[0031] Figure 1 Comparison photos of the methyl ethyl ketone-ammonia-formamide reaction system (after standing) before and after the introduction of surfactant.

[0032] Figure 2 Comparison photos of the methyl ethyl ketone-ammonia-formamide reaction system (stirred) before and after the introduction of surfactant. Detailed Implementation

[0033] The specific embodiments of the present invention will be described in detail below. However, it should be noted that the scope of protection of the present invention is not limited to these specific embodiments, but is determined by the claims in the appendix.

[0034] All publications, patent applications, patents, and other references mentioned in this specification are incorporated herein by reference. Unless otherwise defined, all technical and scientific terms used in this specification have the meanings commonly understood by those skilled in the art. In case of conflict, the definitions in this specification shall prevail.

[0035] When this specification uses the prefixes “known to those skilled in the art,” “prior art,” or similar terms to derive materials, substances, methods, steps, apparatus, or components, the objects derived from such prefixes cover those commonly used in the art at the time of this application, but also include those that are not currently commonly used but will become generally recognized in the art as suitable for similar purposes.

[0036] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.

[0037] In this document, all numeric values ​​of parameters (e.g., quantity or condition) should be understood to be modified by the term “about” in all cases, regardless of whether “about” actually appears before the numeric value.

[0038] In the context of this instruction manual, all chemical reagents are available for purchase.

[0039] Unless otherwise specified, all percentages, parts, ratios, etc. mentioned in this instruction manual are based on weight, and the pressure is gauge pressure.

[0040] In the context of this specification, any two or more embodiments of the present invention can be arbitrarily combined, and the resulting technical solutions are part of the original disclosure of this specification and also fall within the protection scope of the present invention.

[0041] In the context of this specification, the yield of butanone azide is calculated using the following formula:

[0042]

[0043] Analysis method:

[0044] After the reaction was completed, a certain amount of xylene was added to the system to demulsify and extract the methyl ethyl ketone (MEK) azide. The mixture was allowed to stand and separate into layers. The upper oil phase consisted of the remaining MEK, the product MEK azide, and xylene, while the lower aqueous phase consisted of the remaining ammonia and formamide. The upper oil phase was chemically analyzed using an Agilent 7890A gas chromatograph (KB-5 capillary column, FID detector), and the mass of MEK azide was obtained by area normalization.

[0045] Figure 1 This is the macroscopic state of the butanone-ammonia-formamide reaction system solution when left to stand. Before the introduction of the surfactant, the entire system is divided into two layers: an upper oil phase consisting of butanone and a lower aqueous phase consisting of ammonia and formamide. After introducing a certain amount of Brij-30, the layering phenomenon disappears, forming a water-in-oil system, which appears as a transparent and homogeneous solution macroscopically.

[0046] Figure 2 This shows the macroscopic state of the butanone-ammonia-formamide reaction system solution during stirring. Before the introduction of the surfactant, the entire system was a turbid liquid (emulsion) and the solution was opaque; after introducing a certain amount of Brij-30 to form a water-in-oil system, the macroscopic state remained a transparent and homogeneous solution.

[0047] Example 1

[0048] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 200 mL of methyl ethyl ketone (MEK), 100 mL of 25 wt% ammonia, 50 mL of formamide, and 30 g of Brij-30. After stirring to form a clear, transparent water-in-oil reverse microemulsion, heat to 30°C. Once the temperature stabilizes, add 50 mL of 30 wt% hydrogen peroxide (containing 0.2 g of disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system over 1 hour. After the addition is complete, continue the reaction for another hour. After the reaction is complete, add 100 mL of xylene to the system to break the emulsion and extract the MEK azohydride. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azohydride was calculated to be 93.8%.

[0049] Example 2

[0050] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 200 mL of methyl ethyl ketone (MEK), 100 mL of 25 wt% ammonia, 50 mL of formamide, and 40 g of Brij-56. After stirring to form a clear, transparent water-in-oil reverse microemulsion, heat to 30°C. Once the temperature stabilizes, add 50 mL of 30 wt% hydrogen peroxide (containing 0.2 g of disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system over 1 hour. After the addition is complete, continue the reaction for another hour. After the reaction is complete, add 100 mL of xylene to the system to break the emulsion and extract the MEK azohydride. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azohydride was calculated to be 89.3%.

[0051] Example 3

[0052] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 200 mL of methyl ethyl ketone (MEK), 100 mL of 25 wt% ammonia, 50 mL of formamide, and 50 g of Brij-58. After stirring to form a clear, transparent water-in-oil reverse microemulsion, heat to 30°C. Once the temperature stabilizes, add 50 mL of 30 wt% hydrogen peroxide (containing 0.2 g of disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system over 1 hour. After the addition is complete, continue the reaction for another hour. After the reaction is complete, add 100 mL of xylene to the system to break the emulsion and extract the MEK azohydride. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azohydride was calculated to be 85.9%.

[0053] Example 4

[0054] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 430 mL of methyl ethyl ketone (MEK), 270 mL of 25 wt% ammonia, 130 mL of formamide, and 50 g of Brij-30. After stirring to form a clear, transparent water-in-oil reverse microemulsion, heat to 30°C. Once the temperature stabilizes, add 80 mL of 30 wt% hydrogen peroxide (containing 0.2 g of disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system. The addition is completed over 1 hour, followed by another hour of reaction. After the reaction is complete, add 100 mL of xylene to the system to break the emulsion and extract the MEK azohydride. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azohydride was calculated to be 90.4%.

[0055] Example 5

[0056] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 110 mL of methyl ethyl ketone (MEK), 70 mL of 25 wt% ammonia, 30 mL of formamide, and 20 g of Brij-30. After stirring to form a clear, transparent water-in-oil reverse microemulsion, heat to 30°C. Once the temperature stabilizes, add 40 mL of 30 wt% hydrogen peroxide (containing 0.2 g of disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system over 1 hour. After the addition is complete, continue the reaction for another hour. After the reaction is complete, add 100 mL of xylene to the system to break the emulsion and extract the MEK azohydride. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azohydride was calculated to be 91.5%.

[0057] Comparative Example 1

[0058] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 200 mL of methyl ethyl ketone (MEK), 100 mL of 25 wt% ammonia, and 50 mL of formamide. Stir and heat to 30°C. After the temperature stabilizes, add 50 mL of 30 wt% hydrogen peroxide (containing 0.2 g disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system over 1 hour. After the addition is complete, continue the reaction for another hour. After the reaction is complete, add 100 mL of xylene to the system to extract the MEK azide. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azide was calculated to be 45.7%.

[0059] Comparative Example 2

[0060] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 200 mL of methyl ethyl ketone (MEK), 100 mL of 25 wt% ammonia, and 50 mL of formamide. Stir and heat to 60 °C. After the temperature stabilizes, add 50 mL of 30 wt% hydrogen peroxide (containing 0.2 g disodium EDTA) to the constant-pressure dropping funnel and slowly add it dropwise to the reaction system over 1 hour. After the addition is complete, continue the reaction for another 5 hours. After the reaction is complete, add 100 mL of xylene to the system to extract the MEK azide. Allow the mixture to stand and separate into layers. Analyze the upper oil phase using gas chromatography. The yield of MEK azide was calculated to be 83.2%.

[0061] Comparative Example 3

[0062] To a reaction apparatus equipped with a magnetic stirrer, thermometer, reflux condenser, and constant-pressure dropping funnel, add 200 mL of methyl ethyl ketone (MEK), 100 mL of 25 wt% ammonia, 50 mL of formamide, and 30 g of cetyltrimethylammonium bromide (CTAB, a cationic surfactant). The mixture is stirred and heated to 30°C. After the temperature stabilizes, 50 mL of 30 wt% hydrogen peroxide (containing 0.2 g of disodium EDTA) is added to the constant-pressure dropping funnel and slowly added dropwise over 1 hour. The reaction continues for another hour after the addition is complete. After the reaction is finished, 100 mL of xylene is added to the system to break the emulsion and extract the MEK azohydride. The mixture is allowed to stand and separate into layers. The upper oil phase is analyzed by gas chromatography. The yield of MEK azohydride is calculated to be 62.1%.

[0063] The specific implementation of the present invention has been described in detail above, but it is only an example. The present invention is not limited to the specific implementation examples described above, and equivalent modifications to the microemulsion reaction system involved in the present invention are also within the protection scope of the present invention.

Claims

1. A method for synthesizing butanone azohydramine, the method comprising the following steps: (1) Mix methyl ethyl ketone, ammonia, catalyst and nonionic surfactant evenly to form a first feed stream; the nonionic surfactant is at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene alkylamine and polyether; the catalyst is an amide compound; the amount of nonionic surfactant is 10% to 50% of the mass of methyl ethyl ketone; (2) Under reaction conditions, an oxidant is introduced into the first feed stream and the reaction is carried out; the oxidant is a hydrogen peroxide solution; (3) After the reaction in step (2) is completed, an organic solvent is added for separation and extraction. The upper layer is obtained by standing and separating the layers.

2. The method for synthesizing butanone azide according to claim 1, characterized in that: The ammonia concentration is 20% to 30%.

3. The method for synthesizing butanone azide according to claim 1, characterized in that: The ammonia concentration is 25%–28%.

4. The method for synthesizing butanone azide according to claim 1, characterized in that: The catalyst is selected from at least one of formamide, acetamide, propionamide, and dimethylformamide.

5. The method for synthesizing butanone azide according to claim 1 or 4, characterized in that: The catalyst is formamide.

6. The method for synthesizing butanone azide according to claim 1, characterized in that: The nonionic surfactant is selected from one or more of polyoxyethylene lauryl ether, polyethylene glycol hexadecyl ether, and polyoxyethylene ether.

7. The method for synthesizing butanone azide according to claim 1, characterized in that: The nonionic surfactant is polyoxyethylene lauryl ether.

8. The method for synthesizing butanone azide according to claim 1, characterized in that: The reaction conditions in step (2) are as follows: the reaction temperature is 20-50℃ and the reaction time is 1-5h.

9. The method for synthesizing butanone azide according to claim 1, characterized in that: The reaction conditions in step (2) are as follows: the reaction temperature is 30-40℃ and the reaction time is 1-5h.

10. The method for synthesizing butanone azide according to claim 1, characterized in that: The oxidant in step (2) is a hydrogen peroxide solution containing disodium EDTA; the concentration of the hydrogen peroxide solution is 27.5% to 30%; the content of disodium EDTA in the hydrogen peroxide solution containing disodium EDTA is 0.1 to 1.0 g / mol of hydrogen peroxide.

11. The method for synthesizing butanone azide according to claim 10, characterized in that: The content of disodium EDTA in the hydrogen peroxide solution is 0.3–0.5 g / mol of hydrogen peroxide.

12. The method for synthesizing butanone azide according to claim 1, characterized in that: The separation solvent in step (3) is an organic solvent, which is one or more of cyclohexane, n-hexane, toluene, and xylene.

13. The method for synthesizing butanone azide according to claim 1, characterized in that: The separation solvent in step (3) is xylene.

14. The method for synthesizing butanone azide according to claim 1, characterized in that: The molar ratio of methyl ethyl ketone (MEK) to hydrogen peroxide is 3–5:

1.

15. The method for synthesizing butanone azide according to claim 1, characterized in that: The molar ratio of ammonia to hydrogen peroxide is 2 to 4:

1.

16. The method for synthesizing butanone azide according to claim 1, characterized in that: The molar ratio of formamide to hydrogen peroxide is 2 to 4:1.

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