Emulsion explosive containing single sensitizer and preparation method thereof

Abstract

The invention relates to an emulsion explosive containing a single sensitizer and a preparation method thereof, and belongs to the technical field of emulsion explosives. The invention provides a preparation method of an emulsion explosive containing a single sensitizer, which comprises the following steps: preparing a water phase, preparing an oil phase, mixing the water phase and the oil phase to prepare a primary emulsion product, and further homogenizing to obtain a water-in-oil emulsion. The uniform dispersion and high efficiency of the hollow glass beads are further promoted, and the overall performance of the emulsion explosive is improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of emulsion explosives, and relates to an emulsion explosive containing a single sensitizer and a preparation method thereof. Background Art

[0002] Emulsion explosive generally refers to a kind of water-in-oil (W / O) latex-shaped water-containing industrial explosive prepared by an emulsification technique, in which micro-droplets of an oxidizer salt aqueous solution are uniformly dispersed in an oil-phase continuous medium containing porous substances such as dispersed air bubbles or hollow glass microspheres, and is widely used in mine exploitation, civil engineering, building demolition, and military fields, etc., and can play an effective blasting role in various complex environments. A sensitizer is an important component to enhance the explosion performance of emulsion explosives, which can improve its sensitivity to external stimuli such as impact and friction, thereby enhancing the explosion velocity and energy release efficiency of the explosive. Traditional emulsion explosives generally use one or more sensitizers. However, although composite sensitizers can enhance the sensitivity, there may be interactions between multiple sensitizers, resulting in a decline in the performance of some components, and even leading to unstable or unsafe situations. Summary of the Invention

[0003] The purpose of the present invention is to provide an emulsion explosive containing a single sensitizer and a preparation method thereof. The present invention prepares a stable water-phase system and an oil-phase system, and synergistically forms a stable water-in-oil emulsion system, further promoting the uniform dispersion and efficient action of hollow glass microspheres, and improving the overall performance of the emulsion explosive.

[0004] The purpose of the present invention 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 comprises the following steps:

[0006] Step X1: Keep the stirring speed constant, add 1-ethyl-3-methylimidazolium bromide into the reaction kettle, stir and heat up to 70-80 °C, stir for 1-3 min after reaching the temperature, successively add ammonium nitrate, sodium nitrate, ethylene glycol and water, keep warm and stir until completely dissolved, adjust the pH to 6.5-7.5 by dropping a sodium dihydrogen phosphate solution while stirring, and obtain the water phase after the stirring ends;

[0007] Step X2: Add a bio-based oil-phase material into another reaction kettle, stir evenly at 60-70 °C, add a compound emulsifier and stir for 10-20 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 15-25 min to obtain the oil phase;

[0008] Step X3: Slowly add the aqueous phase to the oil phase while starting a high-speed stirrer and stirring at 40°C. After the addition is completed, continue stirring for 20 - 30 min to obtain a preliminary emulsified product;

[0009] Step X4: Preheat the homogenizer to 40°C, transfer the preliminary emulsified product to the homogenizer, and homogenize to obtain a water-in-oil emulsion;

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

[0011] Further, the mass ratio of 1-ethyl-3-methylimidazolium 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 prepared by compounding sodium dihydrogen phosphate and water, and the concentration is 0.1 - 0.3 mol / L.

[0012] Further, the mass ratio of the bio-based oil phase material, 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 includes the following steps:

[0014] Step Y1: Add natural vegetable oil and palladium-carbon catalyst to the hydrogenation reactor according to a mass ratio of 1:0.01, seal it, displace the air in the reactor with nitrogen 3 times, then displace it with hydrogen 3 times, introduce hydrogen, adjust the pressure in the reactor to 5 - 8 MPa, heat to 180 - 200°C, stir at a speed of 80 - 120 rpm for 3 - 4 h, then cool to room temperature, release the hydrogen pressure, filter and recover the palladium-carbon catalyst using a 0.22 μm 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 aqueous phase and the oil phase in Step X3 is 7.6 - 8.2:1.9 - 2.5, and the controlled addition means adding the aqueous phase to the oil phase at a speed of 1 - 2 L / min.

[0017] Further, the homogenization in Step X4 means homogenizing at a pressure of 120 - 130 MPa for 2 min, then standing for 2 min, and then homogenizing for another 2 min. After the homogenization is completed, cool to room temperature.

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

[0019] Furthermore, the stirring speed during the stirring and heating in step X1 is 300 - 400 rpm, and the heating is carried out 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; the stirring speed in step X5 is 200 - 300 rpm.

[0020] Advantages of the present invention:

[0021] (1) When preparing the aqueous phase of the present invention, 1-ethyl-3-methylimidazolium bromide is introduced to form an ionic environment, which has good solubility for the components of the aqueous phase, is conducive to the uniform mixing of the components during the preparation of the aqueous phase, and forms a stable aqueous phase system.

[0022] (2) The present invention improves the saturation and stability of natural vegetable oil by hydrogenation treatment of natural vegetable oil, thereby improving the chemical stability and antioxidant property of the oil phase; on this basis, a composite emulsifier is added. Span 80 is used as a lipophilic emulsifier, and Tween 80 is used as a hydrophilic emulsifier. The synergistic effect of the two can effectively reduce the interfacial tension between oil and water and improve the emulsification stability; in addition, the long carbon chains of calcium stearate introduced in the present invention are intertwined with the oil phase molecules to form a physical cross-linked network. Hydroxyethyl cellulose forms fine particles or micelles by dispersing in the oil phase, and then forms a weakly cross-linked polymer network structure. The dual enhancement effect enables the oil phase to better resist shear force during emulsification, and the components synergistically promote the formation of a stable water-in-oil emulsion system when the oil and water phases are mixed.

[0023] (3) By preparing a stable water-in-oil emulsion system, the present invention further promotes the uniform dispersion and efficient action of hollow glass microspheres, and improves the overall performance of the emulsion explosive. Specific embodiments

[0024] To further illustrate the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following examples are used to describe in detail the specific embodiments, structures, features and effects according to the present invention.

[0025] Example 1

[0026] A preparation method of an emulsion explosive containing a single sensitizer. The preparation method of the emulsion explosive in this example includes the following steps:

[0027] Step X1: Keep the stirring speed constant. Add 1-ethyl-3-methylimidazolium bromide to the reaction kettle and stir and heat to 70 °C. After reaching the temperature, stir for 1 min. Then add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, and keep stirring until completely dissolved. While stirring, dropwise add sodium dihydrogen phosphate solution to adjust the pH to 6.5. After stirring ends, obtain the aqueous phase;

[0028] Step X2: Add the bio-based oil phase material into another reactor, stir evenly at 60°C, then add the compound emulsifier and stir for 10 min. Next, add calcium stearate and hydroxyethyl cellulose and continue to stir for 15 min to obtain the oil phase.

[0029] Step X3: Add the water phase to the oil phase at a controlled rate while starting a high-speed stirrer and stirring at 40°C. After the addition is completed, continue to stir for 20 min to obtain a preliminary emulsified product.

[0030] Step X4: Preheat the homogenizer to 40°C, transfer the preliminary emulsified product to the homogenizer, and homogenize to obtain a water-in-oil emulsion.

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

[0032] In step X1 of this example, the mass ratio of 1-ethyl-3-methylimidazolium bromide, ammonium nitrate, sodium nitrate, ethylene glycol, and water is 8:29:4.5:2:25; the sodium dihydrogen phosphate solution is prepared 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, 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 includes the following steps:

[0035] Step Y1: Add soybean oil and palladium-carbon catalyst into the hydrogenation reactor according to a mass ratio of 1:0.01, seal it, displace the air in the reactor with nitrogen 3 times, then displace it with hydrogen 3 times, and then introduce hydrogen. Adjust the pressure in the reactor 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 and recover the palladium-carbon catalyst using a 0.22 μm filter membrane, and collect the filtrate to obtain it.

[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 to the oil phase is 7.6:1.9, and the controlled rate means adding the water phase to the oil phase at a speed of 1 L / min.

[0038] Homogenization in step X4 of this example means homogenizing at a pressure of 120 MPa for 2 min, then standing for 2 min, and then homogenizing for another 2 min. After the homogenization is completed, cool to room temperature.

[0039] In this embodiment, the addition amount of hollow glass microspheres in step X5 accounts for 1 wt% of the total amount of the emulsion explosive.

[0040] In step X1 of this embodiment, the stirring speed during stirring and heating is 300 rpm, and the heating is carried out at a heating rate of 5 °C / min; the stirring speed in step X2 is 200 rpm; the stirring speed in step X3 is 2000 rpm; the stirring speed in step X5 is 200 rpm.

[0041] Example 2

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

[0043] Step X1: Keep the stirring speed constant, add 1-ethyl-3-methylimidazolium bromide into the reaction kettle and stir to heat up to 80 °C. After reaching the temperature, stir for 3 min, then add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, keep stirring and warming until completely dissolved, and adjust the pH to 7.5 by dropwise adding sodium dihydrogen phosphate solution while stirring. After the stirring ends, obtain the aqueous phase;

[0044] Step X2: Add the bio-based oil phase material into another reaction kettle, stir evenly at 70 °C, add the compound emulsifier and stir for 20 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 25 min to obtain the oil phase;

[0045] Step X3: Add the aqueous phase to the oil phase at a controlled speed while starting the high-speed stirrer and stir at 40 °C. After the addition ends, continue to stir for 30 min to obtain the preliminary emulsified product;

[0046] Step X4: Preheat the homogenizer to 40 °C, transfer the preliminary emulsified product to the homogenizer, and homogenize to obtain the water-in-oil emulsion;

[0047] Step X5: At room temperature, add the hollow glass microspheres to the water-in-oil emulsion and stir for 20 min to obtain the emulsion explosive.

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

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

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

[0051] Step Y1: Add soybean oil and palladium-carbon catalyst into the hydrogenation reactor according to a mass ratio of 1:0.01, seal it, displace the air in the reactor with nitrogen 3 times, then displace it with hydrogen 3 times, and then introduce hydrogen. Adjust the pressure in the reactor to 8 MPa, heat it to 200 °C, stir at a speed of 120 rpm for 4 h, then cool it to room temperature, release the hydrogen pressure, filter and recover the palladium-carbon catalyst using a 0.22 μm filter membrane, and collect the filtrate to obtain the product.

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

[0053] In this example, the mass ratio of the aqueous phase to the oil phase in step X3 is 8.2:2.5. Controlling the speed means adding the aqueous phase to the oil phase at a speed of 2 L / min.

[0054] In this example, homogenization in step X4 means homogenizing at a pressure of 130 MPa for 2 min, then standing for 2 min, and then homogenizing for another 2 min. After homogenization, cool it to room temperature.

[0055] In this example, the addition amount of hollow glass microspheres in step X5 accounts for 3 wt% of the total amount of emulsion explosive.

[0056] In step X1 of this example, the stirring speed during stirring and heating is 400 rpm, and the heating rate is 5 °C / min; the stirring speed in step X2 is 300 rpm; the stirring speed in step X3 is 3000 rpm; the stirring speed in step X5 is 300 rpm.

[0057] Example 3

[0058] A preparation method of an emulsion explosive containing a single sensitizer. The preparation method of the emulsion explosive in this example includes the following steps:

[0059] Step X1: Keep the stirring speed constant, add 1-ethyl-3-methylimidazolium bromide into the reaction kettle, stir and heat it to 75 °C, stir for 2 min after reaching the temperature, add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, keep stirring and heating until completely dissolved, and adjust the pH to 7 by dropwise adding sodium dihydrogen phosphate solution while stirring. After stirring, obtain the aqueous phase;

[0060] Step X2: Add the bio-based oil phase material into another reaction kettle, stir evenly at 65 °C, add the compound emulsifier and stir for 15 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 20 min to obtain the oil phase;

[0061] Step X3: Add the aqueous phase to the oil phase at a controlled speed while starting a high-speed stirrer and stirring at 40 °C. After the addition is completed, continue to stir for 25 min to obtain a preliminary emulsified product;

[0062] Step X4: Preheat the homogenizer to 40°C, transfer the preliminary emulsion product to the homogenizer, and homogenize to obtain a water-in-oil emulsion;

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

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

[0065] In this Example, the mass ratio of the bio-based oil phase material, composite emulsifier, calcium stearate, and hydroxyethyl cellulose in Step X2 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 includes the following steps:

[0067] Step Y1: Add soybean oil and palladium-carbon catalyst to the hydrogenation reactor according to a mass ratio of 1:0.01, seal it, displace the air in the reactor with nitrogen 3 times, then displace it with hydrogen 3 times, introduce hydrogen, adjust the pressure in the reactor to 6.5 MPa, heat to 190°C, stir at a speed of 100 rpm for 3.5 h, then cool to room temperature, release the hydrogen pressure, filter and recover the palladium-carbon catalyst using a 0.22 μm filter membrane, and collect the filtrate to obtain it.

[0068] In this Example, the composite emulsifier in Step X2 is composed of Span 80 and Tween 80 according to a mass ratio of 3:6.9.

[0069] In this Example, the mass ratio of the water phase to the oil phase in Step X3 is 7.9:2.2. Controlling the speed means adding the water phase to the oil phase at a speed of 1.5 L / min.

[0070] Homogenization in Step X4 of this Example means homogenizing at a pressure of 125 MPa for 2 min, then standing for 2 min, and then homogenizing for another 2 min. After the homogenization is completed, cool to room temperature.

[0071] In this Example, the addition amount of the hollow glass microspheres in Step X5 accounts for 2 wt% of the total amount of the emulsion explosive.

[0072] In Step X1 of this Example, the stirring speed during stirring and heating is 350 rpm, and the heating rate is 5°C / min; the stirring speed in Step X2 is 250 rpm; the stirring speed in Step X3 is 2500 rpm; 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 this example comprises the following steps:

[0075] Step X1: Keeping the stirring speed constant, add 1-ethyl-3-methylimidazolium bromide into the reaction kettle, then stir and heat up to 72 °C. After reaching the temperature, stir for 3 min. Then add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, keep warm and stir until completely dissolved. While stirring, add sodium dihydrogen phosphate solution dropwise to adjust the pH to 6.8. After the stirring ends, obtain the aqueous phase;

[0076] Step X2: Add the bio-based oil phase material into another reaction kettle, stir evenly at 62 °C, then add the compound emulsifier and stir for 18 min. Then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 22 min to obtain the oil phase;

[0077] Step X3: Add the aqueous phase into the oil phase at a controlled speed while starting the high-speed stirrer and stirring at 40 °C. After the addition ends, continue to stir for 28 min to obtain the preliminary emulsified product;

[0078] Step X4: Preheat the homogenizer to 40 °C, transfer the preliminary emulsified product to the homogenizer, and homogenize to obtain the water-in-oil emulsion;

[0079] Step X5: At room temperature, add hollow glass microspheres into the water-in-oil emulsion and stir for 18 min to obtain the emulsion explosive.

[0080] In step X1 of this example, the mass ratio of 1-ethyl-3-methylimidazolium 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 prepared by compounding sodium dihydrogen phosphate and water, and the concentration is 0.15 mol / L.

[0081] 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 20.5:0.7:0.22:0.02.

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

[0083] Step Y1: Add soybean oil and palladium-carbon catalyst into the hydrogenation reaction kettle according to the mass ratio of 1:0.01, seal it, displace the air in the kettle with nitrogen 3 times, then displace it with hydrogen 3 times, then introduce hydrogen, adjust the pressure in the kettle to 6 MPa, heat up to 185 °C, stir at a speed of 110 rpm for 3.2 h, then cool to room temperature, release the hydrogen pressure, use a 0.22 μm filter membrane to filter and recover the palladium-carbon catalyst, and collect the filtrate to obtain it.

[0084] In this embodiment, the composite emulsifier in step X2 is composed of Span 80 and Tween 80 in a mass ratio of 2.9:6.8.

[0085] In this embodiment, the mass ratio of the aqueous phase to the oil phase in step X3 is 7.8:2.1. Controlling the speed means adding the aqueous phase to the oil phase at a speed of 1.2 L / min.

[0086] In this embodiment, the homogenization in step X4 is to homogenize at 120 MPa for 2 min, then let it stand for 2 min, and then homogenize for another 2 min. After the homogenization is completed, it is cooled to room temperature.

[0087] In this embodiment, the addition amount of hollow glass microspheres in step X5 accounts for 1.5 wt% of the total amount of emulsion explosive.

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

[0089] Example 5

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

[0091] Step X1: Keep the stirring speed constant, add 1-ethyl-3-methylimidazolium bromide to the reaction kettle, stir and heat up to 78 °C, stir for 1 min after reaching the temperature, then add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, keep stirring and heating until completely dissolved, and adjust the pH to 7.2 by dropwise adding sodium dihydrogen phosphate solution while stirring. After the stirring is completed, an aqueous phase is obtained;

[0092] Step X2: Add the bio-based oil phase material to another reaction kettle, stir evenly at 68 °C, add the compound emulsifier and stir for 12 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 18 min to obtain an oil phase;

[0093] Step X3: Add the aqueous phase to the oil phase at a controlled speed while starting a high-speed stirrer and stirring at 40 °C. After the addition is completed, continue to stir for 22 min to obtain a preliminary emulsified product;

[0094] Step X4: Preheat the homogenizer to 40 °C, transfer the preliminary emulsified product to the homogenizer, and homogenize to obtain a water-in-oil emulsion;

[0095] Step X5: At room temperature, add hollow glass microspheres to the water-in-oil emulsion and stir for 12 min to obtain the emulsion explosive.

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

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

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

[0099] Step Y1: Add soybean oil and palladium-carbon catalyst into the hydrogenation reactor according to a mass ratio of 1:0.01, seal it, displace the air in the reactor with nitrogen 3 times, then displace it with hydrogen 3 times, then introduce hydrogen, adjust the pressure in the reactor to 7 MPa, heat to 195 °C, stir at a speed of 90 rpm for 3.8 h, then cool to room temperature, release the hydrogen pressure, filter and recover the palladium-carbon catalyst using a 0.22 μm filter membrane, and collect the filtrate to obtain it.

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

[0101] In this embodiment, the mass ratio of the water phase to the oil phase in step X3 is 9.1:2.4. Controlling the speed means adding the water phase to the oil phase at a speed of 1.7 L / min.

[0102] In this embodiment, homogenization in step X4 means homogenizing at a pressure of 130 MPa for 2 min, then standing for 2 min, and then homogenizing for another 2 min. After the homogenization is completed, cool to room temperature.

[0103] In this embodiment, the addition amount of hollow glass microspheres in step X5 accounts for 2 wt% of the total amount of emulsion explosive.

[0104] In step X1 of this embodiment, the stirring speed during stirring and heating is 320 rpm, and the heating is carried out at a heating rate of 5 °C / min; the stirring speed in step X2 is 220 rpm; the stirring speed in step X3 is 2200 rpm; the stirring speed in step X5 is 220 rpm.

[0105] Comparative Example 1

[0106] On the basis of Example 3, while keeping other conditions the same, step X1 is changed to the following steps:

[0107] Keep the stirring speed constant. After preheating the reaction kettle to 75°C, add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, keep warm and stir until completely dissolved, and adjust the pH to 7 by dropping sodium dihydrogen phosphate solution while stirring. After stirring ends, obtain the aqueous phase.

[0108] Comparative Example 2

[0109] On the basis of Example 3, while keeping other conditions the same, change Step X2 to the following steps:

[0110] Add soybean oil to another reaction kettle, stir evenly at 65°C, add the compound emulsifier and stir for 15 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 20 min to obtain the oil phase.

[0111] Comparative Example 3

[0112] On the basis of Example 3, while keeping other conditions the same, change Step X2 to the following steps:

[0113] Add the bio-based oil phase material to another reaction kettle, stir evenly at 65°C, add Span 80 and stir for 15 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir 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 is 21:0.8:0.23:0.03.

[0114] Comparative Example 4

[0115] On the basis of Example 3, while keeping other conditions the same, change Step X2 to the following steps:

[0116] Add the bio-based oil phase material to another reaction kettle, stir evenly at 65°C, add Tween 80 and stir for 15 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir 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 is 21:0.8:0.23:0.03.

[0117] Comparative Example 5

[0118] On the basis of Example 3, while keeping other conditions the same, change Step X2 to the following steps:

[0119] Add the bio-based oil phase material to another reaction kettle, stir evenly at 65°C, add the composite emulsifier and stir for 15 min, then add calcium stearate, and continue to stir 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 calcium stearate is 21:0.8:0.26.

[0120] Comparative Example 6

[0121] On the basis of Example 3, while keeping other conditions the same, change Step X2 to the following steps:

[0122] Add the bio-based oil phase material to another reactor, stir evenly at 65°C, add the composite emulsifier and stir for 15 min, then add hydroxyethyl cellulose and continue to stir 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 hydroxyethyl cellulose is 21:0.8:0.26.

[0123] Comparative Example 7

[0124] On the basis of Example 3, while keeping other conditions the same, change the preparation method of the emulsion explosive to the following steps:

[0125] Step X1: Keep the stirring speed unchanged, add 1-ethyl-3-methylimidazolium bromide to the reactor, stir and heat up to 75°C, stir for 2 min after reaching the temperature, add ammonium nitrate, sodium nitrate, ethylene glycol, and water in sequence, keep warm and stir until completely dissolved, adjust the pH to 7 by dropping sodium dihydrogen phosphate solution while stirring, and obtain the aqueous phase after stirring ends;

[0126] Step X2: Add the bio-based oil phase material to another reactor, stir evenly at 65°C, add the compound emulsifier and stir for 15 min, then add calcium stearate and hydroxyethyl cellulose, and continue to stir for 20 min to obtain the oil phase;

[0127] Step X3: Add the aqueous phase to the oil phase at a controlled speed while starting the high-speed stirrer and stirring at 40°C, continue to stir for 25 min after the addition ends to obtain the water-in-oil emulsion;

[0128] Step X4: At room temperature, add hollow glass microspheres to the water-in-oil emulsion and stir for 10 - 20 min to obtain the emulsion explosive.

[0129] Comparative Example 8

[0130] On the basis of Example 3, while keeping other conditions the same, change the homogenization conditions of Step X4 to homogenize at 125 MPa for 4 min, and cool to room temperature after homogenization ends.

[0131] Taking the emulsion explosives prepared in Examples 1 - 3 and Comparative Examples 1 - 8 as samples, test their performance according to GB18095 - 2000, and the test results are shown in Table 1 below.

[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 can be seen from Table 1, the emulsion explosive containing a single sensitizer prepared by the present invention has a good sensitization effect during use, and the performance of the emulsion explosive is good.

[0135] As described above, it is only the preferred embodiment of the present invention, and there is no limitation to the present invention in any form. Although the present invention has been disclosed as above with the preferred embodiment, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to equivalent embodiments by using the disclosed technical content within the scope of the technical solution of the present invention. However, as long as it does not depart from the content of the technical solution of the present invention, any indirect modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

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, control the stirring speed to be constant, add 1-ethyl-3-methylimidazolium bromide to the reaction kettle, stir and heat to 70-80°C, stir for 1-3 minutes after reaching the temperature, add ammonium nitrate, sodium nitrate, ethylene glycol and water in sequence, keep warm and stir until completely dissolved, add sodium dihydrogen phosphate solution dropwise while stirring to adjust the pH to 6.5-7.5, and complete stirring to obtain an aqueous phase; Step X2, add the bio-based oil phase material to another reaction kettle, stir evenly at 60-70° C., 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, adding the water phase to the oil phase at a controlled speed and stirring at 40° C. with a high-speed stirrer. After the addition is completed, stirring is continued for 20-30 minutes to obtain a preliminary emulsified product; Step X4, preheating a homogenizer to 40° C., transferring the preliminary emulsified product to the homogenizer, and homogenizing to obtain a water-in-oil emulsion; Step X5: Add hollow glass microspheres into the water-in-oil emulsion at room temperature and stir for 10-20 minutes to obtain the emulsion explosive.

2. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, characterized in that: In step X1, the mass ratio of 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; the sodium dihydrogen phosphate solution is obtained by compounding sodium dihydrogen phosphate and water, and the concentration is 0.1-0.3 mol / L.

3. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, characterized in that: The mass ratio of the bio-based oil phase material, composite 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, characterized in that: The method for preparing the bio-based oil phase material in step X2 comprises the following steps: Step Y1, adding natural vegetable oil and palladium carbon catalyst in a mass ratio of 1:0.01 to a hydrogenation reactor, sealing, replacing the air in the reactor with nitrogen 3 times, and then replacing it with hydrogen 3 times, introducing hydrogen, adjusting the pressure in the reactor to 5-8MPa, heating to 180-200°C, stirring at 80-120rpm for 3-4h, and then cooling to room temperature, releasing the hydrogen pressure, using a 0.22μm filter membrane to filter and recover the palladium carbon catalyst, and collecting the filtrate to obtain.

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

1.

6. The method for preparing an emulsion explosive containing a single sensitizer according to claim 1, characterized in that: 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.

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

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

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