Synthesis method of alcamines polymer emulsifier for emulsion explosive
Alkyl amine polymeric emulsifiers were synthesized by combining the addition reaction of methyl acrylate and acetyl bromide with the esterification of polyisobutylene succinic anhydride and triethanolamine. This solved the problem of poor structural uniformity of emulsifier products and improved the storage stability and explosive performance of emulsion explosives.
Patent Information
- Application Number
- CN202510881423.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-27
- Publication Date
- 2025-11-04
AI Technical Summary
The existing emulsifier products have poor structural uniformity, resulting in poor storage stability of emulsion explosives, which affects production quality and application performance.
Methyl acrylate and acetyl bromide were subjected to a 1,4 addition reaction to generate N,N-dihydroxyethyl-3-aminopropionic acid methyl ester, which was then subjected to an esterification reaction with polyisobutylene succinic anhydride and triethanolamine to form an alcohol amine polymeric emulsifier, thereby controlling the structural uniformity of the product and improving its hydrophilicity and interfacial stability.
It has achieved efficient production of high-purity alkanolamine polymeric emulsifiers, improved emulsification ability and emulsification speed, enhanced the storage stability and detonation performance of emulsion explosives, and met safety standards.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of emulsifier synthesis, and particularly relates to a synthesis method of an alcohol amine high-molecular emulsifier for emulsion explosive. BACKGROUND
[0002] The storage stability of emulsion explosive is one of important characteristics of emulsion explosive, and directly affects the application performance of emulsion explosive.
[0003] As a key component determining the storage stability of emulsion explosive, the performance optimization of emulsifier has always been the focus of industry research. Among numerous emulsifiers, high-molecular emulsifiers exhibit significant advantages due to their unique steric hindrance effect and interfacial stability characteristics. Among them, the research on polyisobutylene succinic anhydride (PIBSA) derivative emulsifiers is the most in-depth. This type of compound constructs an amphiphilic high-molecular structure containing hydrophilic hydroxyl groups and lipophilic ester groups through the directional esterification of the anhydride groups of polyisobutylene succinic anhydride and polyhydric compounds. The polar groups in the molecule can form strong hydration, while the non-polar polyisobutylene segment provides a steric stabilization barrier. This synergistic effect endows the material with excellent interfacial adsorption capacity and long-term storage stability, providing an ideal colloidal protection effect for emulsion explosive systems.
[0004] It has been reported that polyisobutylene succinic anhydride derivative emulsifiers have good application effect in emulsion explosive, but the product of this type of emulsifier is relatively complex, and the product structure is relatively poor in singleness, which will have certain adverse effects on actual production and scientific research.
[0005] Therefore, it is particularly important for the development of emulsion explosive to develop an emulsifier with relatively simple product structure, excellent emulsifying performance, and excellent storage stability of the prepared emulsion explosive. The present application synthesizes a high-efficiency high-molecular alcohol amine emulsifier, explores the suitable process conditions, controls the relative simplicity of the product structure, and studies the influence of this type of emulsifier on the storage stability of emulsion explosive. SUMMARY
[0006] In order to solve the above problems, the present application aims to provide a synthesis method of alcohol amine high-molecular emulsifier for emulsion explosive, which can solve the problem of poor product singleness caused by the complex molecular configuration of polyol and polyol amine polyene-based high-molecular emulsifier, and control the quality fluctuations in industrial production. The new method can continuously and quickly produce high-quality alcohol amine high-molecular emulsifier, and the produced emulsifier has good emulsifying capacity, fast emulsion formation speed, and other characteristics, which is beneficial to the production and storage performance stability of explosive.
[0007] The technical scheme of the present application is as follows: A synthesis method of alcohol amine high-molecular emulsifier for emulsion explosive, the method comprising the following steps: S1: methyl acrylate and acetyl bromide react to obtain 3-bromine methyl propionate, and then react with diethanolamine to obtain N,N-dihydroxyethyl-3-amino methyl propionate: (methyl acrylate and acetyl bromide can be reacted by 1,4 addition to obtain 3-bromine methyl propionate in high yield, and then reacted with glycol amine to obtain N,N-dihydroxyethyl-3-amino methyl propionate with high purity and single structure, M 丙烯酸甲酯 : M 乙酰溴 = 1:1.1~1.3, M 二乙醇胺 : M 丙烯酸甲酯 =1.05:1); S2: N,N-dihydroxyethyl-3-amino methyl propionate reacts with polyisobutylene succinic anhydride by esterification to prepare polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-amino methyl propionate. (The molecule of N,N-dihydroxyethyl-3-amino methyl propionate contains two hydroxyl groups which can react with the anhydride bond of polyisobutylene succinic anhydride to prepare a product with relatively single structure, M 聚异丁烯丁二酸酐 : M ,N-二羟乙基-3-氨基丙酸甲酯 =2:1); S3: polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-amino methyl propionate reacts with triethanolamine by esterification to prepare an alcohol amine type polymer emulsifier. (Polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-amino methyl propionate contains two carboxyl groups, and triethanolamine contains hydroxyl groups which can react with the carboxyl groups and active H, M 聚异丁烯丁二酸酐-N,N-二羟乙基-3-氨基丙酸甲酯 : M 三乙醇胺 =1:2, and the appearance of the emulsifier is brownish yellow viscous liquid. Preferably, in the step S1, methyl acrylate is dissolved in methanol, hydroquinone is added, stirring at room temperature, acetyl bromide is added dropwise, after the reaction is completed, ethylene glycol amine is added dropwise under nitrogen protection, and N,N-dihydroxyethyl-3-amino methyl propionate is obtained after extraction with diethyl ether; Further preferably, in the step S1, methyl acrylate is dissolved in methanol, and a polymerization inhibitor hydroquinone is added to prevent the polymerization of methyl acrylate during the reaction, thereby affecting the yield, and then acetyl bromide is added and reacted at room temperature for 1~2h, M 丙烯酸甲酯 : M alcohol solvent: M 乙酰溴 =1: (5~10): (1.1~1.3), the amount of the polymerization inhibitor hydroquinone is 0.2%~0.5% of the total mass of the reaction system, ethylene glycol amine is added dropwise under nitrogen protection, M 二乙醇胺 : M 丙烯酸甲酯 =1.05:1, and reacted at 25-45℃ for 4-6 hours.
[0008] Preferably, in the step S2, the polyisobutylene succinic anhydride is dissolved in xylene, and N,N-dihydroxyethyl-3-aminopropanamide methyl ester is added dropwise under nitrogen protection, and an esterification reaction is carried out, after the reaction is completed, xylene is removed by rotary evaporation under reduced pressure, then petroleum ether is added, and saturated brine is used for multiple extractions, the organic phase is collected, and petroleum ether is removed by rotary evaporation under reduced pressure to obtain polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropanamide methyl ester. Further preferably, in the step S2, the solid-liquid ratio of the polyisobutylene succinic anhydride to xylene is 3:1, and the esterification reaction condition is 130-145°C for 2-4 hours. 聚异丁烯丁二酸酐 : M ,N-二羟乙基-3-氨基丙酸甲酯 =2:1, and the esterification reaction condition is 130-145°C for 2-4 hours. Preferably, in the step S3, the polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropanamide methyl ester is dissolved in xylene, and triethanolamine is added dropwise under nitrogen protection, and an esterification reaction is carried out, after the reaction is completed, xylene is removed by rotary evaporation under reduced pressure, then appropriate petroleum ether is added, and saturated brine is used for multiple extractions, the organic phase is collected, and petroleum ether is removed by rotary evaporation under reduced pressure to obtain the alcohol amine high molecular emulsifier.
[0009] Further preferably, in the step S3, M 聚异丁烯丁二酸酐-N,N-二羟乙基-3-氨基丙酸甲酯 : M 三乙醇胺 =1:2, and the esterification reaction condition is 120-145°C for 3-5 hours.
[0010] Compared with the prior art, the present application has the following beneficial effects: 1. Innovation of the reaction: the synthesis of the intermediate I is generally that diethanolamine and methyl acrylate are reacted by Michael addition to synthesize N,N-dihydroxyethyl-3-aminopropanamide methyl ester, but there are still problems of more by-products and lower yield, the present application adopts methyl acrylate and acetyl bromide to carry out 1,4 addition to obtain 3-bromine propionic acid methyl ester, and then reacts with diethanolamine to generate N,N-dihydroxyethyl-3-aminopropanamide methyl ester (intermediate I), which can efficiently obtain high-purity target product, avoid multiple substitution by-products, and ensure that the intermediate I is a single linear structure.
[0011] 2. Control of molecular configuration: it is found through experimental condition screening that when the intermediate I and the polyisobutylene succinic anhydride (PIBSA) are reacted by esterification at a molar ratio of 2:1, the reaction can efficiently generate polyisobutylene succinic anhydride-intermediate I (intermediate II). The anhydride groups of PIBSA and the two hydroxyl groups of the intermediate I are oriented and esterified to form symmetrical ester bond connection (two molecules of the intermediate I are connected to each molecule of PIBSA), avoid branched structure, and ensure that the product is a linear polymer (structural singularity >95%).
[0012] 3. Improve structural selectivity: there is a problem of structural selectivity in the reaction of the carboxylic acid group in intermediate II with TEA, the application obtains the best process conditions through the selection of reaction temperature and reaction time, and through the control of the conditions, relatively stable products can be obtained.
[0013] 4. Optimize hydrophilic-lipophilic balance: the long-chain polyisobutylene of PIBSA provides a strong hydrophobic end, the hydroxyl and ester groups of intermediate I enhance the hydrophilicity, form a clear amphiphilic structure, and improve the emulsification efficiency.
[0014] 5. Enhance hydrophilicity and stabilize colloidal interface: intermediate II is esterified with triethanolamine at a molar ratio of 1:2 to introduce additional hydroxyl groups to generate the final product of alcohol amine polymer emulsifier. The esterification of the three hydroxyl groups of triethanolamine with the carboxyl groups of intermediate II significantly increases the density of polar groups in the molecule, strengthens the hydration capacity, and improves the emulsion speed. The flexible segment of triethanolamine cooperates with the rigid chain of PIBSA to form a dense interface adsorption layer, inhibits the coalescence of oil phase droplets, and improves the storage stability of emulsion explosive. BRIEF DESCRIPTION OF DRAWINGS
[0015] Figure 1 The process flow chart of the application. DETAILED DESCRIPTION The technical solutions in the embodiments of the application will be described clearly and completely below with specific embodiments of the application. The embodiments are only a part of the embodiments of the application, not all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative work are within the protection scope of the application.
[0016] In the context of the present specification, any matter or item not mentioned, except for the explicitly stated content, is directly used with the technology known in the art. Moreover, any embodiment described in the present patent can be freely combined with one or more other embodiments described in the present patent, and the technical solutions or technical ideas formed thereby are considered as part of the original disclosure or original description of the present application, and should not be considered as new content not disclosed in the present patent, unless the combination is considered as obviously unreasonable by those skilled in the art.
[0017] The data points disclosed in the present application not only include the specifically disclosed numerical points, but also include the endpoints of the numerical ranges. The ranges formed by any combination of these data points should be considered as the disclosed or described ranges of the present application, whether or not these numerical points are disclosed one by one in the present text.
[0018] Example 1 S1 86.1 g of methyl acrylate (1 mol), 160.0 g of methanol (5 mol), 0.5 g of hydroquinone were added to a reaction bottle, stirred at room temperature, and 124.2 g of acetyl bromide (1.1 mol) was added dropwise to the reaction bottle with a dropping funnel, reacted at room temperature for 1 h, and then 80.93 g of ethylene glycol amine (1.05 mol) was slowly added dropwise under nitrogen protection, the temperature was controlled at 45°C, the reaction time was 6 h, after the reaction was completed, the product was extracted with 100 mL of ether, and the extract was separated by a separatory funnel. The organic phase was collected and dried with anhydrous sodium sulfate, and the impurities were filtered off. Finally, the ether was removed by a rotary evaporator to obtain the N,N-dihydroxyethyl-3-aminopropionic acid methyl ester product with a yield of 96%.
[0019] S2 400 g of polyisobutylene succinic anhydride was accurately weighed and dissolved in 160 mL of xylene with stirring. Under nitrogen protection, 51.815 g of N,N-dihydroxyethyl-3-aminopropionic acid methyl ester was added dropwise, and the reaction temperature was controlled within 125°C, and the reaction time was 2 h. After the reaction was completed, the xylene was removed by rotary evaporation under reduced pressure, and 200 mL of petroleum ether was added for extraction to extract the product.
[0020] After phase separation, the organic phase was collected. Finally, the petroleum ether was removed by a rotary evaporator to obtain the polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropionic acid methyl ester product.
[0021] S3 251.8 g of polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropionic acid methyl ester was accurately weighed and dissolved in 80 mL of xylene with stirring. Under nitrogen protection, 74.6 g of triethanolamine was added dropwise, the reaction temperature was controlled at 120°C, and the reaction time was 2 h. After the reaction was completed, the xylene was removed by rotary evaporation under reduced pressure, and 200 mL of petroleum ether was added for extraction. The organic phase was collected and dried, and finally the petroleum ether was removed by rotary evaporation to obtain the alcohol amine polymer emulsifier product with a purity of 90.16%.
[0022] Example 2 S1 86.1 g of methyl acrylate (1 mol), 160.0 g of methanol (5 mol), 0.5 g of hydroquinone were added to a reaction bottle, stirred at room temperature, and 124.2 g of acetyl bromide (1.1 mol) was added dropwise to the reaction bottle with a dropping funnel, reacted at room temperature for 1 h, and then 80.93 g of ethylene glycol amine (1.05 mol) was slowly added dropwise under nitrogen protection, the temperature was controlled at 45°C, the reaction time was 6 h, after the reaction was completed, the product was extracted with 100 mL of ether, and the extract was separated by a separatory funnel. The organic phase was collected and dried with anhydrous sodium sulfate, and the impurities were filtered off. Finally, the ether was removed by a rotary evaporator to obtain the N,N-dihydroxyethyl-3-aminopropionic acid methyl ester product with a yield of 96%.
[0023] S2 Accurately weigh 400 g of polyisobutylene succinic anhydride into 160 mL of xylene, keep stirring. Under the protection of nitrogen, add 51.815 g of N,N-dihydroxyethyl-3- aminopropanamide drop by drop, control the reaction temperature within 120°C, and the reaction time is 4 h. After the reaction is completed, remove the xylene by rotary evaporation under reduced pressure, and add 200 mL of petroleum ether for extraction. Collect the organic phase after phase separation. Finally, remove the petroleum ether by rotary evaporation to obtain the polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3- aminopropanamide product.
[0024] Use saturated brine for multiple extractions, and collect the organic phase after phase separation. Finally, remove the petroleum ether by rotary evaporation to obtain the polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropanamide product.
[0025] S3 Accurately weigh 251.8 g of polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3- aminopropanamide into 80 mL of xylene, keep stirring. Under the protection of nitrogen, add 74.6 g of triethanolamine drop by drop, control the reaction temperature at 130°C, and the reaction time is 4 h. After the reaction is completed, remove the xylene by rotary evaporation under reduced pressure, and add 200 mL of petroleum ether, use saturated brine for multiple extractions. Collect the organic phase and dry, finally remove the petroleum ether by rotary evaporation to obtain the alcohol amine polymer emulsifier product, with a purity of 94.06%.
[0026] Example 3 S1 Add 86.1 g of methyl acrylate (1 mol), 160 g of methanol (5 mol), and 0.5 g of p- benzenediol into a reaction bottle, stir at room temperature, and add 124.2 g of acetyl bromide (1.1 mol) into the reaction bottle through a dropping funnel at room temperature, react for 2 h, then slowly add 80.93 g of ethylenediamine (1.05 mol) under the protection of nitrogen, control the temperature at 25°C, and the reaction time is 4 h. After the reaction is completed, extract the product with 100 mL of ether, and separate the extract through a separatory funnel. Collect the organic phase and dry with anhydrous sodium sulfate, and filter out the impurities. Finally, remove the ether by rotary evaporation to obtain the N,N-dihydroxyethyl-3- aminopropanamide product, with a yield of 94%.
[0027] S2 Accurately weigh 400 g of polyisobutylene succinic anhydride into 160 mL of xylene, keep stirring. Under the protection of nitrogen, add 51.815 g of N,N-dihydroxyethyl-3- aminopropanamide drop by drop, control the reaction temperature within 120°C, and the reaction time is 4 h. After the reaction is completed, remove the xylene by rotary evaporation under reduced pressure, and add 200 mL of petroleum ether for extraction. Collect the organic phase after phase separation. Finally, remove the petroleum ether by rotary evaporation to obtain the polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3- aminopropanamide product.
[0028] Use saturated brine for multiple extractions, and collect the organic phase after phase separation. Finally, remove the petroleum ether by rotary evaporation to obtain the polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropanamide product.
[0029] S3 accurately weigh 251.8 g of polyisobutylene succinic anhydride-N,N- dihydroxyethyl-3-aminopropionic acid methyl ester and dissolve in 80 mL of xylene, keep stirring uniform. Under the protection of nitrogen, add 74.6 g of triethanolamine drop by drop, control the reaction temperature at 135°C, and the reaction time is 5h. After the reaction is completed, remove the xylene under reduced pressure, and add 200 mL of petroleum ether, extract with saturated brine for several times. Collect the organic phase and dry, and finally remove the petroleum ether by rotary evaporation to obtain the alcohol amine polymer emulsifier product, with a purity of 83.15%.
[0030] Example 4 Based on Example 1, the specific optimization data of step S1 is as follows: Table 1: The separation yield of intermediate I after reaction for 4h at different temperatures under the protection of nitrogen. Other conditions are the same as Example 1. Considering comprehensively, the reaction temperature of 25-45°C is more appropriate.
[0031] Table 1: The separation yield of intermediate I at different temperatures
[0032] Based on Example 1, the specific optimization data of step S1 is as follows: Table 2: The separation yield of intermediate I after reaction for different times at 45°C under the protection of nitrogen. Other conditions are the same as Example 1. Considering comprehensively, the reaction time of 4-6h is more appropriate.
[0033] Table 2: The separation yield of intermediate I at different reaction times
[0034] Based on Example 1, the specific optimization data of step S1 is as follows: Table 3: The separation yield of intermediate I after reaction for 6h at 45°C with different contents of hydroquinone. Other conditions are the same as Example 1. The yield is low when the content of hydroquinone is less than 0.2%, and there is no obvious change when the content is higher than 0.5%, so the content of 0.2-0.5% is more appropriate.
[0035] Table 3: The separation yield of intermediate I with different contents of polymerization inhibitor
[0036] Example 5 Based on Example 2, the specific optimization data of step S2 is as follows: Table 4 data: nitrogen protection, under different temperatures, after 3h reaction, the acid value of intermediate II changes. From the results, with the reaction temperature is elevated, the acid value of intermediate II decreases accordingly, when the temperature is 145°C, the acid value of the product is basically unchanged. Other same as example 2. Comprehensive consideration, the reaction temperature of this experiment is 130-145°C more appropriate.
[0037] Table 4 different temperature intermediate II acid value determination results
[0038] Based on example 2, step S2 specific optimization data: Table 5 data: nitrogen protection, under 135°C, after different time reaction, the acid value of intermediate II changes. Other same as example 5. From the results, with the reaction time is prolonged, the acid value of intermediate II decreases accordingly, but after 4h reaction, the acid value of the product is basically unchanged. Comprehensive consideration, the reaction time of this experiment is 2-4h more appropriate.
[0039] Table 5 different reaction time intermediate II acid value determination results
[0040] Based on example 2, step S2 specific optimization data: Table 6 data: under 135°C, after 4h reaction, the acid value of intermediate II changes with different solid-liquid ratio of polyisobutylene succinic anhydride and xylene. Other same as example 2. From the results, when the solid-liquid ratio of polyisobutylene succinic anhydride and xylene is 3:1, the acid value is the smallest, so the solid-liquid ratio of polyisobutylene succinic anhydride and xylene is 3:1 most appropriate.
[0041] Table 6 different solid-liquid ratio intermediate II acid value determination results
[0042] Example 6 Based on example 3, other same as example 2. S3 specific optimization data: Table 7 data: nitrogen protection, under different temperatures, after 4h reaction, the hydroxyl value of the final product changes. From the results, with the reaction temperature is elevated, the hydroxyl value of the final product increases accordingly, when the temperature is 145°C, the hydroxyl value of the product is basically unchanged. Comprehensive consideration, the reaction temperature of this experiment is 120-145°C more appropriate.
[0043] Table 7 different temperature final product hydroxyl value determination results
[0044] Table 8: The hydroxyl value of the final product was measured after different reaction time. The result showed that the hydroxyl value of the final product increased with the reaction time, but the hydroxyl value of the product did not change after 3h reaction. In summary, the reaction time of 3-5h was suitable.
[0045] Table 8: The hydroxyl value of the final product was measured after different reaction time. The result showed that the hydroxyl value of the final product increased with the reaction time, but the hydroxyl value of the product did not change after 3h reaction. In summary, the reaction time of 3-5h was suitable.
[0046] Example 1: Stability of the product, 1. Viscosity test The result of Table 9 showed that the viscosity of the final product was higher than that of T152 and the intermediates. The higher the viscosity of the emulsion, the better the emulsification effect.
[0047] Table 9: Viscosity of the emulsion matrix
[0048] 2. High-low temperature cycle test The result of Table 10 showed that the conductivity increased with the increase of the number of high-low temperature cycles. The conductivity of the final product was smaller than that of T152 and the intermediates, indicating that the stability of the emulsion matrix was better.
[0049] Table 10: Conductivity of the emulsion matrix solution after different high-low temperature cycles
[0050] 3. Detonation performance test The detonation velocity, brisance, work capacity and the distance of the detonation are the main performances of the emulsion explosive, and are also the common indicators for measuring the detonation performance of the emulsion explosive. As shown in Table 11, the performance of the final product was improved in various aspects compared with T152 and the intermediates.
[0051] Table 11: Detonation performance of the emulsion explosive
[0052] 4. Safety performance test The mechanical sensitivity and thermal sensitivity of the emulsion explosive prepared from T152 and a series of products were determined according to GB772A-97 and GB18095-2000. As shown in Table 12, the emulsion explosives prepared from the four emulsifiers met the safety standards.
[0053] Table 12: Conductivity of the emulsion matrix solution after different high-low temperature cycles
[0054] The technical solutions of the present application are explained by the above examples, but the present application is not limited to the above examples, i.e. it does not mean that the present application must rely on the above specific examples to be implemented. Any improvement made by the person skilled in the art on the basis of the present application, or equivalent replacement of the materials selected for the present application, etc. falls within the scope of protection of the patent.
Claims
1. A method for synthesizing an alcoholamine-based polymeric emulsifier for emulsion explosives, characterized in that: The method includes the following steps: S1: Methyl acrylate and acetyl bromide undergo a 1,4 addition reaction to give methyl 3-bromopropionate, which then reacts with diethanolamine to generate N,N-dihydroxyethyl-3-aminopropionate methyl ester. S2: Methyl N,N-dihydroxyethyl-3-aminopropionate was prepared by esterification of polyisobutylene succinic anhydride with polyisobutylene succinic anhydride. S3: An alcohol amine polymeric emulsifier is prepared by esterification of polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropionate methyl ester with triethanolamine.
2. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 1, characterized in that, In step S1, methyl acrylate is used as a raw material, an alcohol solvent is added as a reaction solvent, a bisphenol polymerization inhibitor is added, the mixture is stirred at room temperature, acetyl bromide is added dropwise, diethanolamine is added dropwise under nitrogen protection, and after the reaction is complete, it is extracted with diethyl ether to obtain methyl N,N-dihydroxyethyl-3-aminopropionate.
3. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 2, characterized in that, In step S1, the alcohol solvent is methanol or ethanol, and the diphenol polymerization inhibitor is hydroquinone or 2-tert-butylhydroquinone. 丙烯酸甲酯 M alcohol solvents: M 乙酰溴 =1:(5~10):(1.1~1.3), the polymerization inhibitor dosage is 0.2%-0.5% of the total reaction mass, and ethylene glycolamine is added dropwise under nitrogen protection after the reaction, M 二乙醇胺 M 丙烯酸甲酯 =(1-2):1, preferably, M 二乙醇胺 M 丙烯酸甲酯 =1.05:
1.
4. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 2, characterized in that, In step S1, the reaction temperature is 25-45℃ and the reaction time is 4-6 hours.
5. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 1, characterized in that, In step S2, polyisobutylene succinic anhydride is dissolved in xylene, and N,N-dihydroxyethyl-3-aminopropionate methyl ester is added dropwise under nitrogen protection. After the reaction is completed, xylene is removed by rotary evaporation under reduced pressure. Then, petroleum ether is added, and the mixture is extracted multiple times with saturated brine. The organic phase is collected, and petroleum ether is removed by rotary evaporation under reduced pressure to obtain polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropionate methyl ester.
6. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 5, characterized in that, In step S2, the solid-liquid ratio of polyisobutylene succinic anhydride to xylene is (2.5-3.5):1, preferably 3:1; M 聚异丁烯丁二酸酐 M ,N-二羟乙基-3-氨基丙酸甲酯 =(1-3):1, preferably, M 聚异丁烯丁二酸酐 M ,N-二羟乙基-3-氨基丙酸甲酯 =2:
1.
7. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 6, characterized in that, In step S2, the esterification reaction conditions are 130-145℃ for 2-4 hours.
8. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 1, characterized in that, In step S3, polyisobutylene succinic anhydride-N,N-dihydroxyethyl-3-aminopropionate methyl ester is dissolved in xylene, and triethanolamine is added dropwise under nitrogen protection. After the reaction is completed, xylene is removed by rotary evaporation under reduced pressure. Then, petroleum ether is added, and the mixture is extracted multiple times with saturated brine. The organic phase is collected, and petroleum ether is removed by rotary evaporation under reduced pressure to obtain an alcoholamine polymeric emulsifier.
9. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 8, characterized in that, In step S3, M 聚异丁烯丁二酸酐-N,N-二羟乙基-3-氨基丙酸甲酯 M 三乙醇胺 =1:(1.5-3.5), preferably, the molar ratio is 1:
2.
10. The method for synthesizing an alcoholamine polymeric emulsifier for emulsion explosives according to claim 8, characterized in that, In step S3, the esterification reaction conditions are 120-145℃ for 3-5 hours.