Method for preparing butanone azine by electrolysis
The preparation of butanone nitrogen is solved by electrolytic method, and the problems of low product yield and high energy consumption in the existing hydrazine hydrate production process are achieved, and the efficient and environmentally friendly preparation of butanone nitrogen is achieved, reducing production costs.
Patent Information
- Application Number
- CN202210827232.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-07-13
- Publication Date
- 2025-08-12
- Estimated Expiration
- 2042-07-13
AI Technical Summary
The existing hydrazine hydrate production processes have problems such as low product yield, high energy consumption and high production costs, especially the ketone nitrogen-coated method and hydrogen peroxide method have shortcomings in ammonia recycling and energy consumption.
Butanone nitrogen is prepared by electrolytic method. By electrolyzing a mixture of ammonium chloride, ammonia water and butanone under specific conditions, electrolyzing is performed using anode such as titanium-plated ruthenium iridium oxide or platinum electrodes, and nickel plates or stainless steel electrodes to form a mixture of butanone nitrogen and ammonium chloride. After extraction and distillation, high-purity butanone nitrogen is obtained to achieve recycling of ammonium chloride.
The preparation of high-purity butanone nitrogen is achieved, which reduces production costs, avoids the use of catalysts and the generation of wastewater, and improves current efficiency and product yield.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of butanone azine preparation, and specifically relates to a method for preparing butanone azine by electrolysis. Background Art
[0002] Ketazine is an intermediate in the preparation of hydrazine hydrate, which can be obtained by hydrolysis. Hydrazine hydrate is an important chemical raw material and a widely used chemical product. It is a key raw material for the production of foaming agents, pesticides, pharmaceuticals, dyes, developers, and reducing agents. It is also used in the manufacture of high-purity metals and synthetic fibers, the separation of rare elements, the deoxygenation of large boiler feed water, and the production of rocket fuel and explosives.
[0003] As is well known, there are four main methods for producing hydrazine hydrate: the Rasching process, Bayer's ketazine process, the urea process, and PCUK's hydrogen peroxide process. The Rasching process uses sodium hypochlorite as an oxidant to oxidize ammonia to produce a dilute hydrazine hydrate solution. Sodium hypochlorite is produced by reacting excess sodium hydroxide with chlorine gas. This process has been phased out due to its low yield (approximately 65% based on NaClO) and high energy consumption.
[0004] Bayer's ketazine process is an improvement on the Raschig process. By adding a ketone, the generated hydrazine is rapidly converted to the ketazine, a highly antioxidant. The ketazine is then separated and hydrolyzed to form hydrazine. This process offers high product yields (over 90% based on NaClO), but it consumes significant energy when recycling large amounts of ammonia.
[0005] The urea process uses urea as a nitrogen source and sodium hypochlorite as an oxidant to synthesize hydrazine hydrate. This process avoids the recycling of large amounts of ammonia. However, due to the oxidative decomposition of hydrazine, it suffers from low product yields (approximately 70% based on NaClO), high energy consumption, and the emission of large amounts of ammoniacal nitrogen compounds during production. Consequently, it has been gradually replaced by the ketazine process.
[0006] The hydrogen peroxide method uses hydrogen peroxide instead of sodium hypochlorite as the oxidant, with nitrile or amide as catalyst, and sodium phosphate and ammonium carboxylate as co-catalysts. Butanone and ammonia react with hydrogen peroxide to form butanone azine, which is then hydrolyzed to form hydrazine. This method has the advantage of using only about one-fifth the amount of ammonia recycled compared to the ketazine method using sodium hypochlorite as the oxidant. It also eliminates the use of highly corrosive chlorine and sodium hydroxide, produces no highly corrosive oxides, and offers low energy consumption, making it an energy-saving and environmentally friendly green production process. However, the hydrogen peroxide method suffers from the disadvantage of high production costs.
[0007] In order to further reduce the production costs of hydrazine hydrate and ketazine, it is necessary to improve the production process of butanone azine. Summary of the Invention
[0008] The present invention aims to provide a method for preparing butanone azide by electrolysis. In this method, ammonium chloride can be recycled, thereby achieving atom economy, and no catalyst is required, resulting in simple subsequent separation and treatment, thereby reducing production costs.
[0009] The method for preparing butanone azide by electrolysis according to the present invention comprises the following steps:
[0010] (1) Place a mixture of ammonium chloride, ammonia water and butanone in an electrolytic cell and stir it, then connect the power supply for electrolysis;
[0011] (2) When the electrolysis threshold is reached, the electrolysis is stopped. At this time, a mixture of butanone azine and ammonium chloride is obtained in the electrolytic cell, which is then post-treated to prepare high-purity butanone azine.
[0012] in:
[0013] The anode used in the electrolysis in step (1) is one of a titanium-plated ruthenium-iridium oxide electrode or a platinum electrode; the cathode is one of a nickel plate or a stainless steel electrode; preferably, the anode is a titanium-plated ruthenium-iridium oxide electrode (this electrode is a commercially available product) and the cathode is a nickel plate; more preferably, the anode is a platinum electrode and the cathode is a stainless steel electrode.
[0014] During the electrolysis in step (1), one of ammonia, oxygen, nitrogen or helium is introduced, preferably ammonia is introduced, and the electrolysis pressure is controlled to be 0-0.2 MPa, the electrolysis temperature is 35-65°C, the current intensity is 0.5-5 A, and the current density is 50-500 A / m 2 , voltage is 1.2~5V, and electrode spacing is 2~15mm.
[0015] During the stirring process in step (1), the stirring speed is controlled to be 50~700r / min; stirring is always accompanied during the electrolysis process.
[0016] In step (1), the mass concentration of the ammonium chloride solution is 25-40%, the mass concentration of the ammonia water is 5-28%, and the molar ratio of the ammonia water, ammonium chloride and butanone is 1:0.8-1.2:0.8-1.4.
[0017] The electrolysis is stopped when the electrolysis threshold is reached in step (2). The limit of the electrolysis reaction is based on the butanone content. When the butanone content no longer decreases, it is determined to be the electrolysis threshold of the reaction.
[0018] Due to the volatility of butanone, gas chromatography was used for testing. The gas chromatography conditions were as follows: column temperature: 60°C, vaporization temperature: 200°C, detector: hydrogen flame ionization detector, injection volume: 0.5 μL. The gas chromatograph vaporizes the injected sample, separates it through the chromatographic column, and finally reaches the detector. The instrument automatically plots the electrical signal versus time and integrates it. The percentage of the peak area to the total peak area represents the concentration.
[0019] In step (2), when the electrolysis threshold is reached, the reaction is terminated, and a mixture of ammonium chloride and butanone azide remains in the electrolytic cell. Although butanone azide is water-soluble, according to the principle of "like dissolves like," butanone azide is more soluble in butanone. Therefore, butanone is used as the extractant and is added to the reaction system for extraction. After extraction, standing, and liquid separation, a homogeneous solution of butanone and butanone azide is obtained, and finally, refined butanone azide is obtained through distillation.
[0020] The ammonium chloride obtained after liquid separation in step (2) is recycled as an electrolysis raw material.
[0021] Wherein: the standing temperature is room temperature, the time is 1 hour; the distillation temperature is 110-120℃.
[0022] The equation involved in the electrolysis of ammonium chloride in an electrolytic cell is:
[0023] Anode: 2Cl - -2e - → Cl2↑;
[0024] Cathode: 2H + +2e - → H2↑.
[0025] The method for preparing butanone azine by electrolysis according to the present invention involves the following reaction equation:
[0026] Cl2+2NH3·H2O → NH4ClO+NH4Cl+H2O;
[0027] .
[0028] Compared with the prior art, the present invention has the following beneficial effects:
[0029] In the electrolytic method for preparing butanone azide, chloride ions in a raw material ammonium chloride solution are electrolyzed to generate chlorine gas and ammonia monohydrate, the chlorine gas and ammonia monohydrate react to generate ammonium chloride and ammonium hypochlorite, and the ammonium hypochlorite, ammonia monohydrate and butanone react to generate ammonium chloride and products. The generated ammonium chloride can be recycled, is environmentally friendly, produces no wastewater, realizes atom economy, does not require the addition of a catalyst, simplifies subsequent separation and treatment, and greatly reduces production costs. DETAILED DESCRIPTION
[0030] The present invention will be further described below with reference to the examples.
[0031] Example 1
[0032] The method for preparing butanone azide by electrolysis described in Example 1 comprises the following steps:
[0033] (1) Place a mixture of ammonium chloride, ammonia water and butanone in an electrolytic cell and stir it, then connect the power supply for electrolysis;
[0034] (2) When the electrolysis threshold is reached, the electrolysis is stopped. At this time, a mixture of butanone azine and ammonium chloride is obtained in the electrolytic cell, which is then post-treated to prepare high-purity butanone azine.
[0035] in:
[0036] The anode used in the electrolysis in step (1) is a titanium-plated ruthenium-iridium oxide electrode (this electrode is a commercially available product), and the cathode is a nickel plate.
[0037] During the electrolysis in step (1), ammonia gas was introduced, and the electrolysis pressure was controlled to be 0.15 MPa, the electrolysis temperature was 35°C, the current intensity was 1A, and the current density was 100A / m 2 , voltage is 2.5V, and electrode distance is 5mm.
[0038] During the stirring process in step (1), the stirring speed is controlled to be 300 r / min; stirring is always accompanied during the electrolysis process.
[0039] The electrolyte composition in step (1) is: 85 mL of 30% by mass ammonium chloride solution, 135 mL of 15% by mass ammonia solution, and 40 g of butanone.
[0040] The electrolysis is stopped when the electrolysis threshold is reached in step (2). The limit of the electrolysis reaction is based on the butanone content. When the butanone content no longer decreases, it is determined to be the electrolysis threshold of the reaction.
[0041] Due to the volatility of butanone, gas chromatography was used for testing. The gas chromatography conditions were as follows: column temperature: 60°C, vaporization temperature: 200°C, detector: hydrogen flame ionization detector, injection volume: 0.5 μL. The gas chromatograph vaporizes the injected sample, separates it through the chromatographic column, and finally reaches the detector. The instrument automatically plots the electrical signal versus time and integrates it. The percentage of the peak area to the total peak area represents the concentration.
[0042] In step (2), when the electrolysis threshold is reached, the reaction is terminated, and a mixture of ammonium chloride and butanone azide remains in the electrolytic cell. Although butanone azide is water-soluble, according to the principle of "like dissolves like," butanone azide is more soluble in butanone. Therefore, butanone is added to the reaction system as an extractant for extraction. After extraction, standing (standing temperature is room temperature, time is 1 hour), and liquid separation steps, a homogeneous solution of butanone and butanone azide is obtained. Finally, refined butanone azide is obtained by distillation (distillation temperature is 115°C).
[0043] The ammonium chloride obtained after liquid separation in step (2) is recycled as an electrolysis raw material.
[0044] The test process is:
[0045] After 1 h of reaction, a total of 2.42 g of butanone was consumed and 2.45 g of butanone azide was generated. The average current efficiency was 89.8%. After post-treatment, 2.23 g of the final product was obtained, with a total yield of 81.7%.
[0046] After 2 h of reaction, a total of 5.00 g of butanone was consumed and 5.07 g of butanone azide was generated. The average current efficiency was 92.9%. After post-treatment, 4.61 g was obtained, with a total yield of 84.4%.
[0047] After 10 hours of reaction, a total of 24.40 g of butanone was consumed and 24.76 g of butanone azide was generated. The average current efficiency was 90.8%. After post-treatment, 22.56 g was obtained, with a total yield of 82.7%.
[0048] After 17 hours of reaction, a total of 39.20 g of butanone was consumed and 39.70 g of butanone azide was generated. The average current efficiency was 85.6%. After post-treatment, 36.50 g was obtained, with a total yield of 78.7%.
[0049] After 20 hours of reaction, a total of 39.30 g of butanone was consumed and 39.80 g of butanone azide was produced, with an average current efficiency of 73.0%. After post-processing, 36.55 g was recovered, for an overall yield of 67.0%. The butanone content remained essentially unchanged, and electrolysis was stopped when the electrolysis threshold was reached.
[0050] Example 2
[0051] The method for preparing butanone azide by electrolysis described in Example 2 comprises the following steps:
[0052] (1) Place a mixture of ammonium chloride, ammonia water and butanone in an electrolytic cell and stir it, then connect the power supply for electrolysis;
[0053] (2) When the electrolysis threshold is reached, the electrolysis is stopped. At this time, a mixture of butanone azine and ammonium chloride is obtained in the electrolytic cell, which is then post-treated to prepare high-purity butanone azine.
[0054] in:
[0055] The anode used in the electrolysis in step (1) is a titanium-plated ruthenium-iridium oxide electrode (this electrode is a commercially available product), and the cathode is a stainless steel electrode.
[0056] During the electrolysis in step (1), nitrogen was introduced, and the electrolysis pressure was controlled to be 0.02 MPa, the electrolysis temperature was 40°C, the current intensity was 5A, and the current density was 500A / m 2 , voltage is 3.5V, and electrode distance is 10mm.
[0057] During the stirring process in step (1), the stirring speed is controlled to 400 r / min; stirring is always accompanied during the electrolysis process.
[0058] The electrolyte composition in step (1) is: 48.5 mL of 25% by mass ammonium chloride solution, 135 mL of 5% by mass ammonia solution, and 16.2 g of butanone.
[0059] The electrolysis is stopped when the electrolysis threshold is reached in step (2). The limit of the electrolysis reaction is based on the butanone content. When the butanone content no longer decreases, it is determined to be the electrolysis threshold of the reaction.
[0060] Due to the volatility of butanone, gas chromatography was used for testing. The gas chromatography conditions were as follows: column temperature: 60°C, vaporization temperature: 200°C, detector: hydrogen flame ionization detector, injection volume: 0.5 μL. The gas chromatograph vaporizes the injected sample, separates it through the chromatographic column, and finally reaches the detector. The instrument automatically plots the electrical signal versus time and integrates it. The percentage of the peak area to the total peak area represents the concentration.
[0061] In step (2), when the electrolysis threshold is reached, the reaction is terminated, and a mixture of ammonium chloride and butanone azide remains in the electrolytic cell. Although butanone azide is water-soluble, according to the principle of "like dissolves like," butanone azide is more soluble in butanone. Therefore, butanone is added to the reaction system as an extractant for extraction. After extraction, standing (standing temperature is room temperature, time is 1 hour), and liquid separation steps, a homogeneous solution of butanone and butanone azide is obtained. Finally, refined butanone azide is obtained by distillation (distillation temperature is 110°C).
[0062] The ammonium chloride obtained after liquid separation in step (2) is recycled as an electrolysis raw material.
[0063] The test process is:
[0064] After 0.5 h of reaction, a total of 4.80 g of butanone was consumed and 4.87 g of butanone azide was generated. The average current efficiency was 71.4%. After post-treatment, 4.46 g of the final product was obtained, with a total yield of 65.4%.
[0065] After 1 h of reaction, a total of 9.40 g of butanone was consumed and 9.53 g of butanone azide was produced. The average current efficiency was 69.9%. After post-treatment, 8.76 g of the final product was obtained, with a total yield of 64.2%.
[0066] After 1.5 h of reaction, a total of 12.50 g of butanone was consumed and 12.67 g of butanone azide was generated. The average current efficiency was 61.9%. After post-treatment, 11.60 g was obtained, with a total yield of 56.7%.
[0067] After 2 hours of reaction, a total of 12.63 g of butanone was consumed, and 12.81 g of butanone azide was produced, with an average current efficiency of 47.0%. After post-processing, 11.80 g was recovered, for an overall yield of 43.3%. The butanone content remained essentially unchanged, and electrolysis was stopped when the electrolysis threshold was reached.
[0068] Example 3
[0069] The method for preparing butanone azide by electrolysis described in Example 3 comprises the following steps:
[0070] (1) Place a mixture of ammonium chloride, ammonia water and butanone in an electrolytic cell and stir it, then connect the power supply for electrolysis;
[0071] (2) When the electrolysis threshold is reached, the electrolysis is stopped. At this time, a mixture of butanone azine and ammonium chloride is obtained in the electrolytic cell, which is then post-treated to prepare high-purity butanone azine.
[0072] in:
[0073] The anode used in the electrolysis in step (1) is a platinum electrode, and the cathode is a stainless steel electrode.
[0074] During the electrolysis in step (1), oxygen was introduced, and the electrolysis pressure was controlled to be 0.2 MPa, the electrolysis temperature was 65°C, the current intensity was 0.5 A, and the current density was 50 A / m 2 , voltage is 1.7V, and electrode spacing is 15mm.
[0075] During the stirring process in step (1), the stirring speed is controlled to 700 r / min; stirring is always accompanied during the electrolysis process.
[0076] The electrolyte composition in step (1) is: 142 mL of 40% by mass ammonium chloride solution, 135 mL of 28% by mass ammonia solution, and 60.5 g of butanone.
[0077] The electrolysis is stopped when the electrolysis threshold is reached in step (2). The limit of the electrolysis reaction is based on the butanone content. When the butanone content no longer decreases, it is determined to be the electrolysis threshold of the reaction.
[0078] Due to the volatility of butanone, gas chromatography was used for testing. The gas chromatography conditions were as follows: column temperature: 60°C, vaporization temperature: 200°C, detector: hydrogen flame ionization detector, injection volume: 0.5 μL. The gas chromatograph vaporizes the injected sample, separates it through the chromatographic column, and finally reaches the detector. The instrument automatically plots the electrical signal versus time and integrates it. The percentage of the peak area to the total peak area represents the concentration.
[0079] In step (2), when the electrolysis threshold is reached, the reaction is terminated, and a mixture of ammonium chloride and butanone azide remains in the electrolytic cell. Although butanone azide is water-soluble, according to the principle of "like dissolves like," butanone azide is more soluble in butanone. Therefore, butanone is added to the reaction system as an extractant for extraction. After extraction, standing (standing temperature is room temperature, time is 1 hour), and liquid separation steps, a homogeneous solution of butanone and butanone azide is obtained. Finally, refined butanone azide is obtained by distillation (distillation temperature is 110-120°C).
[0080] The ammonium chloride obtained after liquid separation in step (2) is recycled as an electrolysis raw material.
[0081] The test process is:
[0082] After 1 h of reaction, a total of 1.20 g of butanone was consumed and 1.22 g of butanone azide was produced. The average current efficiency was 89.5%. After post-treatment, 1.10 g of the final product was obtained, with a total yield of 80.8%.
[0083] After 2 h of reaction, a total of 2.40 g of butanone was consumed and 2.43 g of butanone azide was generated. The average current efficiency was 89.1%. After post-treatment, 2.20 g was obtained, with a total yield of 80.6%.
[0084] After 10 hours of reaction, a total of 11.89 grams of butanone was consumed and 12.06 grams of butanone azide was produced. The average current efficiency was 88.4%. After post-treatment, 10.98 grams was obtained, with a total yield of 80.5%.
[0085] After 20 hours of reaction, a total of 24.10 g of butanone was consumed and 24.43 g of butanone azide was generated. The average current efficiency was 89.6%. After post-processing, 22.20 g was obtained, with a total yield of 81.4%.
[0086] After 51 hours of reaction, a total of 60.19 grams of butanone was consumed and 61.03 grams of butanone azide was produced. The average current efficiency was 87.7%. After post-treatment, 55.49 grams was obtained, with a total yield of 79.8%.
[0087] After 60 hours of reaction, a total of 60.28 g of butanone was consumed, and 61.11 g of butanone azide was produced, with an average current efficiency of 74.7%. After post-processing, 56.10 g was recovered, for an overall yield of 68.6%. The butanone content remained essentially unchanged, and electrolysis was stopped when the electrolysis threshold was reached.
[0088] Example 4
[0089] The method for preparing butanone azide by electrolysis described in this embodiment 4 comprises the following steps:
[0090] (1) Place a mixture of ammonium chloride, ammonia water and butanone in an electrolytic cell and stir it, then connect the power supply for electrolysis;
[0091] (2) When the electrolysis threshold is reached, the electrolysis is stopped. At this time, a mixture of butanone azine and ammonium chloride is obtained in the electrolytic cell, which is then post-treated to prepare high-purity butanone azine.
[0092] in:
[0093] The anode used in the electrolysis in step (1) is a platinum electrode (this electrode is a commercially available product), and the cathode is a nickel plate.
[0094] During the electrolysis in step (1), helium was introduced, and the electrolysis pressure was controlled to be 0.1 MPa, the electrolysis temperature was 50°C, the current intensity was 3A, and the current density was 300A / m 2 , voltage is 2.9V, and electrode distance is 2mm.
[0095] During the stirring process in step (1), the stirring speed is controlled to 50 r / min; stirring is always accompanied during the electrolysis process.
[0096] The electrolyte composition in step (1) is: 108 mL of 30% by mass ammonium chloride solution, 135 mL of 20% by mass ammonia solution, and 71.5 g of butanone.
[0097] The electrolysis is stopped when the electrolysis threshold is reached in step (2). The limit of the electrolysis reaction is based on the butanone content. When the butanone content no longer decreases, it is determined to be the electrolysis threshold of the reaction.
[0098] Due to the volatility of butanone, gas chromatography was used for testing. The gas chromatography conditions were as follows: column temperature: 60°C, vaporization temperature: 200°C, detector: hydrogen flame ionization detector, injection volume: 0.5 μL. The gas chromatograph vaporizes the injected sample, separates it through the chromatographic column, and finally reaches the detector. The instrument automatically plots the electrical signal versus time and integrates it. The percentage of the peak area to the total peak area represents the concentration.
[0099] In step (2), when the electrolysis threshold is reached, the reaction is terminated, and a mixture of ammonium chloride and butanone azide remains in the electrolytic cell. Although butanone azide is water-soluble, according to the principle of "like dissolves like," butanone azide is more soluble in butanone. Therefore, butanone is added to the reaction system as an extractant for extraction. After extraction, standing (standing temperature is room temperature, time is 1 hour), and liquid separation steps, a homogeneous solution of butanone and butanone azide is obtained. Finally, refined butanone azide is obtained by distillation (distillation temperature is 110-120°C).
[0100] The ammonium chloride obtained after liquid separation in step (2) is recycled as an electrolysis raw material.
[0101] The test process is:
[0102] After 1 h of reaction, a total of 6.84 g of butanone was consumed and 6.94 g of butanone azide was generated. The average current efficiency was 84.8%. After post-treatment, 6.32 g of the final product was obtained, with a total yield of 77.2%.
[0103] After 2 h of reaction, a total of 13.66 g of butanone was consumed and 13.84 g of butanone azide was generated. The average current efficiency was 84.6%. After post-treatment, 12.60 g was obtained, with a total yield of 77.0%.
[0104] After 5 hours of reaction, a total of 33.29 grams of butanone was consumed and 33.75 grams of butanone azide was produced. The average current efficiency was 82.5%. After post-processing, 30.95 grams was obtained, with a total yield of 75.7%.
[0105] After 8 hours of reaction, a total of 52.30 g of butanone was consumed and 53.03 g of butanone azide was generated. The average current efficiency was 81.0%. After post-treatment, 48.79 g was obtained, with a total yield of 74.5%.
[0106] After 10 hours of reaction, a total of 52.41 g of butanone was consumed, and 53.14 g of butanone azide was produced, with an average current efficiency of 65.0%. After post-processing, 48.89 g was recovered, for an overall yield of 59.8%. The butanone content remained essentially unchanged, and electrolysis was stopped when the electrolysis threshold was reached.
Claims
1. A method for preparing butanone azide by electrolysis, characterized in that: It consists of the following steps: (1) Place a mixture of ammonium chloride, ammonia water and butanone in an electrolytic cell and stir it, then connect the power supply for electrolysis; (2) When the electrolysis threshold is reached, the electrolysis is stopped. At this time, a mixture of butanone azine and ammonium chloride is obtained in the electrolytic cell, which is then post-treated to prepare high-purity butanone azine; in: The anode used in the electrolysis in step (1) is one of a titanium-plated ruthenium-iridium oxide electrode or a platinum electrode; the cathode is one of a nickel plate or a stainless steel electrode; During the electrolysis in step (1), one of ammonia, oxygen, nitrogen or helium is introduced, and the electrolysis pressure is controlled to be 0-0.2 MPa, the electrolysis temperature is 35-65°C, the current intensity is 0.5-5 A, and the current density is 50-500 A / m 2 , voltage is 1.2~5V, electrode spacing is 2~15mm; During the stirring process in step (1), the stirring speed is controlled to be 50-700 r / min; stirring is always accompanied during the electrolysis process; In step (1), the mass concentration of the ammonium chloride solution is 25-40%, the mass concentration of the ammonia water is 5-28%, and the molar ratio of the ammonia water, ammonium chloride and butanone is 1:0.8-1.2:0.8-1.
4.
2. The method for preparing butanone azide by electrolysis according to claim 1, wherein: The anode used in the electrolysis in step (1) is a titanium-plated ruthenium-iridium oxide electrode, and the cathode is a nickel plate.
3. The method for preparing butanone azide by electrolysis according to claim 1, wherein: The anode used in the electrolysis in step (1) is a platinum electrode, and the cathode is a stainless steel electrode.
4. The method for preparing butanone azide by electrolysis according to claim 1, wherein: The electrolysis is stopped when the electrolysis threshold is reached in step (2). The limit of the electrolysis reaction is based on the butanone content. When the butanone content no longer decreases, it is determined to be the electrolysis threshold of the reaction. Since butanone is volatile, gas chromatography is used for testing. The gas chromatography detection conditions are as follows: column chamber temperature: 60°C, vaporization temperature: 200°C, detector: hydrogen flame ionization detector, injection volume: 0.5 μL.
5. The method for preparing butanone azide by electrolysis according to claim 1, wherein: In step (2), when the electrolysis threshold is reached, the reaction is terminated, and a mixture of ammonium chloride and butanone azide remains in the electrolytic cell. Butanone is added to the reaction system for extraction. After extraction, standing, and liquid separation steps, a homogeneous solution of butanone and butanone azide is obtained, and finally butanone azide is obtained by distillation.
6. The method for preparing butanone azide by electrolysis according to claim 5, characterized in that: The standing temperature is room temperature, the standing time is 1h; the distillation temperature is 110-120℃.