Emulsion explosive containing single sensitizer and preparation method thereof

Abstract

The application relates to single-sensitizer-containing emulsion explosive and a preparation method thereof, and belongs to the technical field of emulsion explosive. The application provides a preparation method of single-sensitizer-containing emulsion explosive, which comprises the following steps: preparing a water phase, preparing an oil phase, mixing the water phase and the oil phase to prepare a preliminary emulsification product, and further homogenizing to obtain a water-in-oil emulsion. The application forms a stable water-in-oil emulsion system by preparing a stable water phase system and an oil phase system, further promotes the uniform dispersion and high efficiency of hollow glass microbeads, and improves the overall performance of the emulsion explosive.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of emulsion explosive, and relates to an emulsion explosive containing a single sensitizer and a preparation method thereof. BACKGROUND

[0002] Emulsion explosive is a kind of water-containing industrial explosive in the form of W / O (water-in-oil) emulsion prepared by using emulsion technology, in which microdroplets of an oxidizing agent salt solution are uniformly dispersed in a continuous medium of an oil phase containing porous substances such as dispersed bubbles or hollow glass beads, and the emulsion explosive is widely used in mining, civil engineering, building demolition and military fields, and can play an effective blasting role in various complex environments. A sensitizer is an important component for enhancing the explosive performance of emulsion explosive, which can improve the sensitivity of the emulsion explosive to external stimuli such as impact and friction, and further improve the explosive speed and energy release efficiency of the emulsion explosive. Traditional emulsion explosive generally uses one or more sensitizers, however, although the composite sensitizer can improve the sensitivity, there may be interactions between the multiple sensitizers, which leads to a decrease in the performance of some components, and even causes instability or unsafe conditions. SUMMARY

[0003] The purpose of the present application is to provide an emulsion explosive containing a single sensitizer and a preparation method thereof. The present application forms a stable water-in-oil emulsion system by preparing a stable water phase system and an oil phase system, further promotes the uniform dispersion and efficient action of hollow glass beads, and improves the overall performance of the emulsion explosive.

[0004] The purpose of the present application can be achieved by the following technical solutions:

[0005] A preparation method of an emulsion explosive containing a single sensitizer, the preparation method of the emulsion explosive comprising the following steps:

[0006] Step X1, the stirring speed is controlled to be constant, 1-ethyl-3-methyl imidazole bromide is added into a reaction kettle, and then stirring and heating are performed until the temperature reaches 70-80 DEG C; after the temperature reaches, stirring is performed for 1-3 min; ammonium nitrate, sodium nitrate, ethylene glycol and water are sequentially added, and stirring and heat preservation are performed until complete dissolution; while stirring, sodium dihydrogen phosphate solution is added dropwise to adjust the pH to 6.5-7.5, and the water phase is obtained after the stirring is completed;

[0007] Step X2, bio-based oil phase materials are added into another reaction kettle, and then stirring is performed at 60-70 DEG C until uniform; then, a compounded emulsifier is added, and stirring is performed for 10-20 min; then, calcium stearate and hydroxyethyl cellulose are added, and stirring is continuously performed for 15-25 min, and the oil phase is obtained;

[0008] Step X3, while stirring at 40℃, add the water phase to the oil phase at a constant speed, and start the high-speed mixer; continue stirring for 20-30min after the addition is completed to obtain a preliminary emulsified product;

[0009] Step X4, preheat the homogenizer to 40℃, and transfer the preliminary emulsified product to the homogenizer; homogenize to obtain a water-in-oil emulsion.

[0010] Step X5, at room temperature, add the hollow glass microspheres to the water-in-oil emulsion and stir for 10-20min to obtain the emulsion explosive.

[0011] Further, the mass ratio of 1-ethyl-3-methylimidazole bromide, ammonium nitrate, sodium nitrate, ethylene glycol and water in step X1 is 8-9:29-31:4.5-5.5:2-3:25-28; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.1-0.3mol / L.

[0012] Further, the mass ratio of the bio-based oil phase material, the composite emulsifier, calcium stearate and hydroxyethyl cellulose in step X2 is 20-22:0.6-1:0.22-0.24:0.02-0.04.

[0013] Further, the preparation method of the bio-based oil phase material in step X2 comprises the following steps:

[0014] Step Y1, add natural plant oil and palladium-carbon catalyst to the hydrogenation reactor according to a mass ratio of 1:0.01, seal, replace the air in the reactor with nitrogen for 3 times, and then replace it with hydrogen for 3 times, then introduce hydrogen, adjust the pressure in the reactor to 5-8MPa, heat to 180-200℃, and then stir at a speed of 80-120rpm for 3-4h, then cool to room temperature, release the hydrogen pressure, filter the recovered palladium-carbon catalyst with a 0.22μm filter membrane, and collect the filtrate.

[0015] Further, the composite emulsifier in step X2 is composed of Span 80 and Tween 80 according to a mass ratio of 2.8-3.2:6.7-7.1.

[0016] Further, the mass ratio of the water phase and the oil phase in step X3 is 7.6-8.2:1.9-2.5, and the constant speed refers to adding the water phase to the oil phase at a speed of 1-2L / min.

[0017] Further, the homogenization in step X4 is to homogenize under a pressure of 120-130MPa for 2min, stand for 2min, then homogenize for another 2min, and cool to room temperature after the homogenization is completed.

[0018] Further, the addition amount of the hollow glass microspheres in step X5 accounts for 1-3wt% of the total amount of the emulsion explosive.

[0019] Further, the stirring speed in the stirring and temperature rising of step X1 is 300-400 rpm, and the temperature rising is at a temperature rising rate of 5℃ / min; the stirring speed in step X2 is 200-300 rpm; the stirring speed in step X3 is 2000-3000 rpm; and the stirring speed in step X5 is 200-300 rpm.

[0020] The beneficial effects of the present application are:

[0021] (1) The present application introduces 1-ethyl-3-methyl imidazole bromide to form an ionic environment during the preparation of the aqueous phase, which has good solubility for the components of the aqueous phase, and is conducive to the uniform mixing of the components during the preparation of the aqueous phase, forming a stable aqueous phase system.

[0022] (2) The present application improves the saturation and stability of natural plant oil by hydrogenation treatment, thereby improving the chemical stability and oxidation resistance of the oil phase; on this basis, a composite emulsifier is added, Span 80 as a lipophilic emulsifier and Tween 80 as a hydrophilic emulsifier, the synergistic effect of the two can effectively reduce the oil-water interfacial tension and improve the emulsion stability; in addition, the long carbon chain of the calcium stearate introduced in the present application is intertwined with the oil phase molecules to form a physical crosslinking network, and the hydroxyethyl cellulose forms a weak crosslinked polymer network structure by dispersing in the oil phase to form a small particle or micelle, thereby the double enhancement effect makes the oil phase better resist shear force during the emulsification process, and the components synergistically promote the mixing of the water and oil phases to form a stable water-in-oil emulsion system.

[0023] (3) The present application further promotes the uniform dispersion and efficient action of the hollow glass microspheres by preparing a stable water-in-oil emulsion system, thereby improving the overall performance of the emulsion explosive. DETAILED DESCRIPTION

[0024] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined invention purpose, the specific embodiments, structures, features and effects according to the present application are described in detail as follows in combination with the examples.

[0025] Example 1

[0026] A preparation method of an emulsion explosive containing a single sensitizer, the preparation method of the emulsion explosive of the present embodiment comprises the following steps:

[0027] Step X1: the stirring speed is controlled to be constant, 1-ethyl-3-methyl imidazole bromide is added into the reaction kettle, and then the temperature is raised to 70℃, after reaching the temperature, stirring for 1 min, then ammonium nitrate, sodium nitrate, ethylene glycol and water are added in sequence, and the temperature is kept constant and stirred until completely dissolved, while adding sodium dihydrogen phosphate solution dropwise to adjust the pH to 6.5, and then the stirring is stopped to obtain the aqueous phase;

[0028] Step X2, add the bio-based oil phase material into another reaction kettle, stir uniformly at 60°C, then add the compound emulsifier and stir for 10 min, and then add calcium stearate and hydroxyethyl cellulose, continue to stir for 15 min, to obtain an oil phase;

[0029] Step X3, add the water phase into the oil phase at a controlled speed while starting a high-speed blender to stir at 40°C, continue to stir for 20 min after the addition is completed, to obtain a preliminary emulsified product;

[0030] Step X4, preheat the homogenizer to 40°C, and then transfer the preliminary emulsified product into the homogenizer, to obtain a water-in-oil emulsion by homogenization.

[0031] Step X5, at room temperature, add the hollow glass microspheres into the water-in-oil emulsion, and stir for 10 min, to obtain the emulsion explosive.

[0032] In step X1 of this example, the mass ratio of 1-ethyl-3-methylimidazole bromide, ammonium nitrate, sodium nitrate, ethylene glycol and water is 8:29:4.5:2:25; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.1 mol / L.

[0033] In step X2 of this example, the mass ratio of the bio-based oil phase material, the compound emulsifier, calcium stearate and hydroxyethyl cellulose is 20:0.6:0.22:0.02.

[0034] The preparation method of the bio-based oil phase material in step X2 of this example comprises the following steps:

[0035] Step Y1, add soybean oil and palladium-carbon catalyst into a hydrogenation reaction kettle according to a mass ratio of 1:0.01, seal, replace the air in the kettle with nitrogen for 3 times, and then replace it with hydrogen for 3 times, then pass in hydrogen, adjust the pressure in the kettle to 5 MPa, heat to 180°C, stir at a speed of 80 rpm for 3 h, then cool to room temperature, release the hydrogen pressure, filter the recovered palladium-carbon catalyst using a 0.22 μm filter membrane, and collect the filtrate.

[0036] The compound emulsifier in step X2 of this example is composed of Span 80 and Tween 80 according to a mass ratio of 2.8:6.7.

[0037] In step X3 of this example, the mass ratio of the water phase and the oil phase is 7.6:1.9, and the controlled speed means that the water phase is added to the oil phase at a speed of 1 L / min.

[0038] In step X4 of this example, homogenization means that after homogenization at a pressure of 120 MPa for 2 min, stand for 2 min, then homogenize for another 2 min, and then cool to room temperature after homogenization is completed.

[0039] The hollow glass microbeads in step X5 of the embodiment are added in an amount of 1wt% of the total amount of the emulsion explosive.

[0040] The stirring speed in the stirring temperature rising in step X1 of the embodiment is 300rpm, and the temperature rising is at a temperature rising rate of 5℃ / min; the stirring speed in step X2 is 200rpm; the stirring speed in step X3 is 2000rpm; and the stirring speed in step X5 is 200rpm.

[0041] Embodiment 2

[0042] A preparation method of an emulsion explosive containing a single sensitizer, the preparation method of the emulsion explosive of the embodiment comprises the following steps:

[0043] In step X1, the stirring speed is controlled to be constant, 1-ethyl-3-methyl imidazole bromide is added into a reaction kettle, and then the stirring is raised to 80℃, 3min after reaching the temperature, ammonium nitrate, sodium nitrate, ethylene glycol and water are sequentially added, and the stirring is performed until complete dissolution, the stirring is performed while adding sodium dihydrogen phosphate solution dropwise to adjust the pH to 7.5, and the water phase is obtained after the stirring is completed;

[0044] In step X2, bio-based oil phase materials are added into another reaction kettle, and then stirred uniformly at 70℃, compound emulsifiers are added and stirred for 20min, calcium stearate and hydroxyethyl cellulose are added, and the stirring is continued for 25min, and the oil phase is obtained;

[0045] In step X3, the water phase is added into the oil phase at a controlled speed, and a high-speed blender is started to stir at 40℃, the stirring is continued for 30min after the addition is completed, and the preliminary emulsification product is obtained;

[0046] In step X4, a homogenizer is preheated to 40℃, and the preliminary emulsification product is transferred into the homogenizer, and the water-in-oil emulsion is obtained by homogenization;

[0047] In step X5, hollow glass microbeads are added into the water-in-oil emulsion at room temperature, and the stirring is performed for 20min, and the emulsion explosive is obtained.

[0048] In step X1 of the embodiment, the mass ratio of 1-ethyl-3-methyl imidazole bromide, ammonium nitrate, sodium nitrate, ethylene glycol and water is 9:31:5.5:3:28; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.3mol / L.

[0049] In step X2 of the embodiment, the mass ratio of bio-based oil phase materials, compound emulsifiers, calcium stearate and hydroxyethyl cellulose is 22:1:0.24:0.04.

[0050] The preparation method of the bio-based oil phase materials in step X2 of the embodiment comprises the following steps:

[0051] Step Y1, soybean oil and palladium-carbon catalyst were added into the hydrogenation reactor according to a mass ratio of 1:0.01, sealed, and the air in the reactor was replaced with nitrogen for 3 times, and then replaced with hydrogen for 3 times. After that, hydrogen was introduced, the pressure in the reactor was adjusted to 8 MPa, heated to 200 DEG C, and stirred at a speed of 120 rpm for 4 h. Then the reactor was cooled to room temperature, the hydrogen pressure was released, and the palladium-carbon catalyst was recovered by filtration with a 0.22 mu m filter membrane. The filtrate was collected, and the emulsion explosive was obtained.

[0052] The composite emulsifier in step X2 of the example was composed of Span 80 and Tween 80 according to a mass ratio of 3.2:7.1.

[0053] The mass ratio of the water phase and the oil phase in step X3 of the example was 8.2:2.5, and the speed control means that the water phase was added to the oil phase at a speed of 2 L / min.

[0054] The homogenization in step X4 of the example was that the homogenization was carried out at a pressure of 130 MPa for 2 min, then the reactor was cooled to room temperature for 2 min, and then the homogenization was carried out again for 2 min.

[0055] The hollow glass microspheres in step X5 of the example were added in an amount of 3 wt% of the total amount of the emulsion explosive.

[0056] In step X1 of the example, the stirring speed during temperature rising was 400 rpm, and the temperature rising was at a rate of 5 DEG C / min; in step X2, the stirring speed was 300 rpm; in step X3, the stirring speed was 3000 rpm; and in step X5, the stirring speed was 300 rpm.

[0057] Example 3

[0058] A preparation method of an emulsion explosive containing a single sensitizer, the preparation method of the emulsion explosive of the example comprises the following steps:

[0059] Step X1, the stirring speed was controlled to be constant, 1-ethyl-3-methyl imidazole bromide was added into the reactor, and then the temperature was raised to 75 DEG C. After reaching the temperature, the stirring was carried out for 2 min. Then ammonium nitrate, sodium nitrate, ethylene glycol and water were added in sequence, and the stirring was carried out until they were completely dissolved. While stirring, sodium dihydrogen phosphate solution was added dropwise to adjust the pH to 7. The water phase was obtained after the stirring was completed.

[0060] Step X2, the bio-based oil phase material was added into another reactor, and stirred uniformly at 65 DEG C. Then the composite emulsifier was added, and stirred for 15 min. Then calcium stearate and hydroxyethyl cellulose were added, and stirred for 20 min. The oil phase was obtained.

[0061] Step X3, the water phase was added into the oil phase at a constant speed, and a high-speed blender was started to stir at 40 DEG C. After the addition was completed, the stirring was continued for 25 min. The preliminary emulsification product was obtained.

[0062] Step X4, preheat the homogenizer to 40℃, transfer the primary emulsification product to the homogenizer, homogenize to obtain a water-in-oil emulsion;

[0063] Step X5, at room temperature, add hollow glass microspheres to the water-in-oil emulsion, stir for 15 min, to obtain the emulsion explosive.

[0064] The mass ratio of 1-ethyl-3-methylimidazole bromide, ammonium nitrate, sodium nitrate, ethylene glycol and water in step X1 of this example is 8.5:30:5:2.5:26.5; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.2 mol / L.

[0065] The mass ratio of bio-based oil phase material, composite emulsifier, calcium stearate and hydroxyethyl cellulose in step X2 of this example is 21:0.8:0.23:0.03.

[0066] The preparation method of the bio-based oil phase material in step X2 of this example comprises the following steps:

[0067] Step Y1, add soybean oil and palladium-carbon catalyst into the hydrogenation reaction kettle according to a mass ratio of 1:0.01, seal, replace the air in the kettle with nitrogen for 3 times, then replace it with hydrogen for 3 times, then pass in hydrogen, adjust the pressure in the kettle to 6.5 MPa, heat to 190℃, then stir at a speed of 100 rpm for 3.5 h, then cool to room temperature, release the hydrogen pressure, filter the recovered palladium-carbon catalyst using a 0.22 μm filter membrane, and collect the filtrate.

[0068] The composite emulsifier in step X2 of this example is composed of Span 80 and Tween 80 according to a mass ratio of 3:6.9.

[0069] The mass ratio of the water phase and the oil phase in step X3 of this example is 7.9:2.2, and the speed control means that the water phase is added to the oil phase at a speed of 1.5 L / min.

[0070] The homogenization in step X4 of this example is to homogenize under a pressure of 125 MPa for 2 min, then stand for 2 min, then homogenize for another 2 min, and then cool to room temperature after homogenization.

[0071] The addition amount of hollow glass microspheres in step X5 of this example accounts for 2 wt% of the total amount of the emulsion explosive.

[0072] The stirring speed in the stirring and heating in step X1 of this example is 350 rpm, and the heating is at a heating rate of 5℃ / min; the stirring speed in step X2 is 250 rpm; the stirring speed in step X3 is 2500 rpm; and the stirring speed in step X5 is 250 rpm.

[0073] Example 4

[0074] A preparation method of an emulsion explosive containing a single sensitizer, the preparation method of the emulsion explosive in the embodiment comprises the following steps:

[0075] Step X1, the stirring speed is controlled unchanged, 1-ethyl-3-methyl imidazole bromide is added into the reaction kettle, and then stirring is performed to heat to 72℃, after reaching the temperature, stirring is performed for 3min, ammonium nitrate, sodium nitrate, ethylene glycol and water are sequentially added, and the stirring is performed to completely dissolve under insulation, while the stirring is performed to drop sodium dihydrogen phosphate solution to adjust pH to 6.8, and the stirring is ended to obtain the water phase;

[0076] Step X2, the bio-based oil phase material is added into another reaction kettle, and then stirring is performed at 62℃ until uniform, then the compound emulsifier is added and stirring is performed for 18min, then calcium stearate and hydroxyethyl cellulose are added, and stirring is continuously performed for 22min to obtain the oil phase;

[0077] Step X3, the water phase is controlled to be added into the oil phase, and a high-speed blender is started at the same time to stir at 40℃, after the addition is completed, stirring is continuously performed for 28min to obtain the preliminary emulsification product;

[0078] Step X4, the homogenizer is preheated to 40℃, and the preliminary emulsification product is transferred into the homogenizer, and then homogenization is performed to obtain the water-in-oil emulsion;

[0079] Step X5, at room temperature, the hollow glass microbeads are added into the water-in-oil emulsion, and then stirring is performed for 18min to obtain the emulsion explosive.

[0080] In step X1 of the embodiment, the mass ratio of 1-ethyl-3-methyl imidazole bromide, ammonium nitrate, sodium nitrate, ethylene glycol and water is 8.2:29.5:4.8:2.2:26; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.15mol / L.

[0081] In step X2 of the embodiment, the mass ratio of the bio-based oil phase material, the compound emulsifier, calcium stearate and hydroxyethyl cellulose is 20.5:0.7:0.22:0.02.

[0082] The preparation method of the bio-based oil phase material in step X2 of the embodiment comprises the following steps:

[0083] Step Y1, the soybean oil and the palladium-carbon catalyst are added into the hydrogenation reaction kettle according to the mass ratio of 1:0.01, the kettle is sealed, the air in the kettle is replaced with nitrogen for 3 times, then replaced with hydrogen for 3 times, hydrogen is introduced, the pressure in the kettle is adjusted to 6MPa, heating is performed to 185℃, then stirring is performed at 110rpm for 3.2h, then the hydrogen pressure is released, the palladium-carbon catalyst is filtered and recovered by using a 0.22μm filter membrane, and then the filtrate is collected.

[0084] The complex emulsifier in step X2 of the embodiment is composed of Span 80 and Tween 80 in a mass ratio of 2.9:6.8.

[0085] The mass ratio of the water phase and the oil phase in step X3 of the embodiment is 7.8:2.1, and the speed control means that the water phase is added to the oil phase at a speed of 1.2 L / min.

[0086] The homogenization in step X4 of the embodiment is that the homogenization is carried out at a pressure of 120 MPa for 2 min, then the homogenization product is left for 2 min, and then the homogenization is carried out again for 2 min, and after the homogenization is completed, the homogenization product is cooled to room temperature.

[0087] The addition amount of the hollow glass microbeads in step X5 of the embodiment accounts for 1.5 wt% of the total amount of the emulsion explosive.

[0088] In the stirring and temperature rising in step X1 of the embodiment, the stirring speed is 370 rpm, and the temperature rising is carried out at a temperature rising rate of 5 ℃ / min; in step X2, the stirring speed is 280 rpm; in step X3, the stirring speed is 2800 rpm; and in step X5, the stirring speed is 280 rpm.

[0089] Embodiment 5

[0090] A preparation method of an emulsion explosive containing a single sensitizer, the preparation method of the emulsion explosive of the embodiment comprises the following steps:

[0091] In step X1, the stirring speed is controlled to be constant, 1-ethyl-3-methylimidazole bromide is added to a reaction kettle, and then the temperature is raised to 78℃ by stirring, 1 min after reaching the temperature, ammonium nitrate, sodium nitrate, ethylene glycol and water are sequentially added, and the mixture is stirred and kept at the temperature until completely dissolved, while the pH is adjusted to 7.2 by dropwise adding sodium dihydrogen phosphate solution, and then the water phase is obtained by stirring;

[0092] In step X2, the bio-based oil phase material is added to another reaction kettle, stirred uniformly at 68℃, then the complex emulsifier is added and stirred for 12 min, and then calcium stearate and hydroxyethyl cellulose are added and stirred for 18 min, to obtain the oil phase;

[0093] In step X3, the water phase is added to the oil phase at a speed of 1.2 L / min while a high-speed stirrer is started to stir at 40℃, and after the addition is completed, the stirring is continued for 22 min to obtain a preliminary emulsification product;

[0094] In step X4, a homogenizer is preheated to 40℃, and the preliminary emulsification product is transferred to the homogenizer, and then a water-in-oil emulsion is obtained by homogenization;

[0095] In step X5, the hollow glass microbeads are added to the water-in-oil emulsion at room temperature, and stirred for 12 min to obtain the emulsion explosive.

[0096] The mass ratio of 1-ethyl-3-methylimidazole bromide, ammonium nitrate, sodium nitrate, ethylene glycol and water in step X1 of the example is 8.8:30.5:5.2:2.7:27; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.25 mol / L.

[0097] The mass ratio of the bio-based oil phase material, the composite emulsifier, calcium stearate and hydroxyethyl cellulose in step X2 of the example is 21.5:0.9:0.24:0.04.

[0098] The preparation method of the bio-based oil phase material in step X2 of the example comprises the following steps:

[0099] In step Y1, soybean oil and palladium-carbon catalyst are added into a hydrogenation reactor according to a mass ratio of 1:0.01, sealed, the air in the reactor is replaced with nitrogen for 3 times, and then replaced with hydrogen for 3 times, then hydrogen is introduced, the pressure in the reactor is adjusted to 7 MPa, heated to 195 ℃, stirred at a speed of 90 rpm for 3.8 h, then cooled to room temperature, the hydrogen pressure is released, and the palladium-carbon catalyst is recovered by using a 0.22 μm filter membrane, and the filtrate is collected.

[0100] The composite emulsifier in step X2 of the example is composed of Span 80 and Tween 80 according to a mass ratio of 3.1:7.

[0101] The mass ratio of the water phase and the oil phase in step X3 of the example is 9.1:2.4, and the speed control means that the water phase is added to the oil phase at a speed of 1.7 L / min.

[0102] The homogenization in step X4 of the example means that after being homogenized at a pressure of 130 MPa for 2 min, it is left for 2 min, then homogenized again for 2 min, and then cooled to room temperature after homogenization.

[0103] The hollow glass microbeads in step X5 of the example account for 2 wt% of the total amount of the emulsion explosive.

[0104] The stirring speed in the stirring and temperature rising in step X1 of the example is 320 rpm, the temperature rising is at a rate of 5 ℃ / min, the stirring speed in step X2 is 220 rpm, the stirring speed in step X3 is 2200 rpm, and the stirring speed in step X5 is 220 rpm.

[0105] Comparative Example 1

[0106] On the basis of Example 3, other conditions remain unchanged, and step X1 is changed to the following steps:

[0107] The stirring speed was controlled unchanged, and the reaction kettle was preheated to 75°C. Then, ammonium nitrate, sodium nitrate, ethylene glycol and water were added in sequence, and the mixture was stirred and heated until completely dissolved. While stirring, sodium dihydrogen phosphate solution was added dropwise to adjust the pH to 7. The stirring was stopped to obtain the water phase.

[0108] Comparative Example 2

[0109] Based on Example 3, other conditions were kept unchanged, and step X2 was changed to the following step:

[0110] The soybean oil was added to another reaction kettle and stirred uniformly at 65°C. Then, the compound emulsifier was added and stirred for 15 min. Subsequently, calcium stearate and hydroxyethyl cellulose were added, and the mixture was continuously stirred for 20 min to obtain the oil phase.

[0111] Comparative Example 3

[0112] Based on Example 3, other conditions were kept unchanged, and step X2 was changed to the following step:

[0113] The bio-based oil phase material was added to another reaction kettle and stirred uniformly at 65°C. Then, Span 80 was added and stirred for 15 min. Subsequently, calcium stearate and hydroxyethyl cellulose were added, and the mixture was continuously stirred for 20 min to obtain the oil phase. At this time, the mass ratio of the bio-based oil phase material, Span 80, calcium stearate and hydroxyethyl cellulose was 21:0.8:0.23:0.03.

[0114] Comparative Example 4

[0115] Based on Example 3, other conditions were kept unchanged, and step X2 was changed to the following step:

[0116] The bio-based oil phase material was added to another reaction kettle and stirred uniformly at 65°C. Then, Tween 80 was added and stirred for 15 min. Subsequently, calcium stearate and hydroxyethyl cellulose were added, and the mixture was continuously stirred for 20 min to obtain the oil phase. At this time, the mass ratio of the bio-based oil phase material, Tween 80, calcium stearate and hydroxyethyl cellulose was 21:0.8:0.23:0.03.

[0117] Comparative Example 5

[0118] Based on Example 3, other conditions were kept unchanged, and step X2 was changed to the following step:

[0119] The bio-based oil phase material was added to another reaction kettle and stirred uniformly at 65°C. Then, the compound emulsifier was added and stirred for 15 min. Subsequently, calcium stearate was added, and the mixture was continuously stirred for 20 min to obtain the oil phase. At this time, the mass ratio of the bio-based oil phase material, compound emulsifier and calcium stearate was 21:0.8:0.26.

[0120] Comparative Example 6

[0121] On the basis of Example 3, other conditions remain unchanged, step X2 is changed to the following steps:

[0122] Into another reaction kettle, the bio-based oil phase material was stirred uniformly at 65℃, then the composite emulsifier was added and stirred for 15 min, and then the hydroxyethyl cellulose was added and stirred for 20 min to obtain the oil phase; at this time, the mass ratio of the bio-based oil phase material, the composite emulsifier and the hydroxyethyl cellulose was 21:0.8:0.26.

[0123] Comparative Example 7

[0124] On the basis of Example 3, other conditions remain unchanged, the preparation method of the emulsion explosive is changed to the following steps:

[0125] Step X1, the stirring speed was controlled unchanged, 1-ethyl-3-methyl imidazole bromide was added into the reaction kettle, and then the stirring was heated to 75℃, after reaching the temperature, the stirring was carried out for 2 min, then the ammonium nitrate, sodium nitrate, ethylene glycol and water were added and stirred until completely dissolved, while the sodium dihydrogen phosphate solution was added dropwise to adjust the pH to 7, and then the stirring was stopped to obtain the water phase;

[0126] Step X2, into another reaction kettle, the bio-based oil phase material was stirred uniformly at 65℃, then the composite emulsifier was added and stirred for 15 min, and then the calcium stearate and the hydroxyethyl cellulose were added and stirred for 20 min to obtain the oil phase;

[0127] Step X3, the water phase was added into the oil phase at a controlled speed, and a high-speed blender was started to stir at 40℃, after the addition was completed, the stirring was continued for 25 min to obtain a water-in-oil emulsion;

[0128] Step X4, at room temperature, the hollow glass microspheres were added into the water-in-oil emulsion and stirred for 10-20 min to obtain the emulsion explosive.

[0129] Comparative Example 8

[0130] On the basis of Example 3, other conditions remain unchanged, the homogenization condition of step X4 was changed to homogenization at a pressure of 125 MPa for 4 min, and then cooled to room temperature.

[0131] The emulsion explosives prepared in Examples 1-3 and Comparative Examples 1-8 were used as samples, and their performances were tested according to GB18095-2000, and the test results are shown in Table 1.

[0132] Table 1 Test results of emulsion explosive performance

[0133] Briskness (mm) Detonation velocity (m / s) Example 1 16.2 5674 Example 2 16.2 5677 Example 3 16.3 5683 Example 4 16.1 5669 Example 5 16.1 5667 Comparative Example 1 15.7 5630 Comparative Example 2 15.2 5580 Comparative Example 3 15.4 5601 Comparative Example 4 15.3 5605 Comparative Example 5 15.6 5613 Comparative Example 6 15.5 5610 Comparative Example 7 15.9 5658 Comparative Example 8 16.0 5654

[0134] As shown in Table 1, the emulsion explosive containing a single sensitizer prepared by the present application has good sensitization effect when used, and the performance of the emulsion explosive is good.

[0135] The above merely describes the preferred embodiments of the present application, and is not intended to limit the present application in any form. Although the present application has been disclosed with the preferred embodiments as above, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical content to obtain equivalent embodiments with equivalent changes, as long as the changes or modifications do not deviate from the technical solution of the present application. Any indirect modifications, equivalent changes and modifications made to the above embodiments according to the technical essence of the present application still fall within the scope of the technical solution of the present application.

Claims

1. A method for preparing an emulsion explosive containing a single sensitizer, characterized in that: The preparation method of the emulsion explosive comprises the following steps: Step X1, controlling the stirring speed to remain unchanged, adding 1-ethyl-3-methylimidazolium bromide to the reactor, stirring, and heating to 70-80°C. After reaching the temperature, stirring for 1-3 minutes, adding ammonium nitrate, sodium nitrate, ethylene glycol, and water in sequence, and stirring at this temperature until completely dissolved. While stirring, sodium dihydrogen phosphate solution is added dropwise to adjust the pH to 6.5-7.

5. After stirring, an aqueous phase is obtained; the mass ratio of the 1-ethyl-3-methylimidazolium bromide, ammonium nitrate, sodium nitrate, ethylene glycol, and water is 8-9:29-31:4.5-5.5:2-3:25-28; Step X2: Add the bio-based oil phase material to another reaction kettle and stir evenly at 60-70° C., then add the compound emulsifier and stir for 10-20 minutes, then add calcium stearate and hydroxyethyl cellulose, and continue stirring for 15-25 minutes to obtain the oil phase; Step X3: Add the water phase to the oil phase at a controlled rate while stirring at 40° C. with a high-speed stirrer. Continue stirring for 20-30 minutes after the addition is complete to obtain a preliminary emulsified product. Step X4: preheat a homogenizer to 40° C., transfer the preliminary emulsified product into the homogenizer, and homogenize to obtain a water-in-oil emulsion; Step X5: Add hollow glass microspheres to the water-in-oil emulsion at room temperature and stir for 10-20 minutes to obtain an emulsion explosive; The method for preparing the bio-based oil phase material in step X2 comprises the following steps: Step Y1, natural vegetable oil and palladium carbon catalyst are added to the hydrogenation reactor in a mass ratio of 1:0.01, sealed, the air in the reactor is replaced with nitrogen 3 times, and then replaced with hydrogen 3 times, hydrogen is introduced, and the pressure in the reactor is adjusted to 5-8 MPa. After heating to 180-200 ° C, stirring at 80-120 rpm for 3-4 hours, the mixture is cooled to room temperature, the hydrogen pressure is released, and the palladium carbon catalyst is recovered by filtering with a 0.22 μm filter membrane, and the filtrate is collected.

2. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The sodium dihydrogen phosphate solution in step X1 is prepared by mixing sodium dihydrogen phosphate and water, and has a concentration of 0.1-0.3 mol / L.

3. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The mass ratio of the bio-based oil phase material, compound emulsifier, calcium stearate and hydroxyethyl cellulose in step X2 is 20-22:0.6-1:0.22-0.24:0.02-0.

04.

4. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The emulsifier prepared in step X2 is composed of Span 80 and Tween 80 in a mass ratio of 2.8-3.2:6.7-7.

1.

5. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The mass ratio of the water phase to the oil phase in step X3 is 7.6-8.2:1.9-2.5, and the rate control refers to adding the water phase to the oil phase at a rate of 1-2 L / min.

6. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The homogenization in step X4 is to homogenize at a pressure of 120-130 MPa for 2 minutes, then let it stand for 2 minutes, and then homogenize for another 2 minutes. After the homogenization is completed, it is cooled to room temperature.

7. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The amount of hollow glass microspheres added in step X5 accounts for 1-3 wt% of the total amount of emulsion explosive.

8. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, wherein: The stirring speed in the stirring and heating in step X1 is 300-400 rpm, and the heating is performed at a heating rate of 5°C / min; the stirring speed in step X2 is 200-300 rpm; the stirring speed in step X3 is 2000-3000 rpm; and the stirring speed in step X5 is 200-300 rpm.