CN110907496A - Experimental device and test method for inducing explosive auto-explosion of sulfide ore - Google Patents
Experimental device and test method for inducing explosive auto-explosion of sulfide ore Download PDFInfo
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Abstract
The invention relates to an experimental device and a test method for inducing explosive auto-explosion of sulfide ores, which comprises a constant temperature calorimetric box and a data terminal, and is characterized in that: the constant temperature calorimetric box is characterized in that an insulating heat-insulating cover plate is arranged at the opening of the upper part of the constant temperature calorimetric box in a covering mode, a reference pool and a sample pool are arranged in the constant temperature calorimetric box, heating elements are arranged inside the reference pool and the sample pool, a reference object heat flux sensor is arranged at the bottom of the reference pool, a gas detector is arranged on the upper part of the sample pool, a thermocouple A for monitoring the temperature of a sample and a thermocouple B for controlling the temperature of the sample are arranged on the lower part of the sample pool, a sample heat flux sensor is arranged at the bottom of the sample pool, the constant temperature calorimetric box, the heating elements, the gas detector, the reference object heat flux sensor, the sample heat flux sensor, the thermocouple A and the thermocouple B are electrically connected with a controller, the controller is electrically connected with a data terminal, and the influence of sulfide ore on.
Description
Technical Field
The invention relates to an experimental device and a test method for inducing explosive auto-explosion of sulfide ores.
Background
Sulfur is a basic chemical raw material, and sulfur-containing ore can be directly used for preparing sulfuric acid and sulfur. At present, the sulfur resource in China is mainly sulfide ore, and the mining area is already foundThe amount of sulfur ore reaches 800, about 50 hundred million tons. Sulphide ore is a generic name for iron sulphide minerals that can be used industrially, not by mineralogical name, including Pyrite (Pyrite, FeS)2) Marcasite, FeS2) And Pyrrhotite (Fe) x1-S), the 3 minerals have the same components and are closely symbiotic, but have different physical properties, and are collectively called sulfide ores.
The emulsion explosive is developed in the 70 th of the 20 th century in China, and through continuous improvement, the emulsion explosive has the advantages of reliable safety performance, good explosion performance, water resistance, low cost and the like. In 2005, the total output of the emulsion explosive in China exceeds that of the ammonium nitrate fuel oil (ANTNT) explosive, and the proportion of the emulsion explosive in the total output of the industrial explosive is increased year by year, so that the emulsion explosive becomes the leading product of the industrial explosive in China. The exploitation of sulphide ore mainly uses emulsion explosive to carry out blasting operation, when the emulsion explosive is directly contacted with sulphide ore, the main component ammonium nitrate in the emulsion explosive and FeS in the sulphide ore2Reaction takes place to form SO2Along with NO gas and other products, also give off a large amount of heat. If heat is accumulated in the blast hole, the temperature rise can lead the explosive to explode in advance, and casualty accidents are caused.
At present, the industrial development is rapid, the demand for sulfur ore resources is more and more increased, the deep mining of sulfide ore becomes a normal state, and meanwhile, the problem of thermal damage of deep mines is more serious. Therefore, in the blasting mining operation of the sulfide ores, the potential hazard of the sulfide ores inducing explosive self-explosion cannot be small. The research on whether the sulfide ores with different components can induce explosive spontaneous explosion is very important, and the method can provide data support and early warning for the exploitation of the sulfide ores and reduce the occurrence of spontaneous explosion casualty accidents.
Disclosure of Invention
The invention provides an experimental device and a test method for inducing explosive auto-explosion of sulfide ores.
The invention adopts the scheme that an experimental device for inducing explosive auto-explosion of sulfide ores comprises a constant temperature calorimetric box and a data terminal, wherein an insulating heat-preservation cover plate is covered at an opening at the upper part of the constant temperature calorimetric box, a reference pool and a sample pool are arranged in the constant temperature calorimetric box, heating elements are respectively arranged in the reference pool and the sample pool, a reference object heat flux sensor is arranged at the bottom of the reference pool, a reference object can be replaced according to the requirement in the middle of the reference pool, a gas detector is arranged at the upper part of the sample pool and is used for detecting gas generated after a reaction of the object to be detected, a thermocouple A for monitoring the temperature of a sample and a thermocouple B for controlling the temperature of the sample are arranged at the lower part of the sample pool, the sample heat flux sensor, the constant temperature calorimetric box, the heating elements, the gas detector, the reference object heat flux sensor, The thermocouple A and the thermocouple B are both electrically connected with the controller, the controller is electrically connected with the data terminal, and the reference substance heat flux sensor and the sample heat flux sensor are used for recording the heat passing through the reference substance and the sample.
Further, the heating element is an electric heating tube.
Further, the controller is a PLC, and the data terminal is a computer terminal.
A method of determining whether a sulphide ore will induce auto-detonation of an explosive, comprising the steps of:
(1) collecting sulfide ore powder in a mine blast hole, drying the sulfide ore by using a vacuum drying oven, and then grinding the sulfide ore to be less than 100 microns by adopting a manual grinding mode; (2) selecting an explosive used in the mine blasting operation, and adding ground sulfide ore powder into the explosive, wherein the mass of the sulfide ore powder accounts for 5-20% of the total mass; the mixing process is carried out in an environment below 25 ℃, and the mixture is slowly stirred; when a test sample is manufactured, the total mass is more than 100g, the sulfide ore powder is added into the explosive in batches to ensure that the sample is uniformly mixed, and the test is carried out in time after the mixing is finished; (3) weighing 0.1-1 g of sample into a sample cell of a testing device for testing; (4) setting test parameters through a data terminal, wherein the temperature rise rate control range is 0.1-2K/min, and the temperature range is 25-300 ℃; (5) weighing explosives with the same mass into a sample cell of a testing device for testing, and setting the same parameters as those in the step (4) for testing; (6) the data terminal records the heat flux parameter and the gas parameter in the two constant temperature calorimeters to generate a numberAccording to the report, the influence of the sulfide ore on the explosive is judged according to the data report, and the judgment is based on whether SO is detected in the whole test process2And NO gas, and differences in heat flux parameters of the sulphide ore powder to the explosive mixture and explosive throughout the test.
Compared with the prior art, the invention has the following beneficial effects: the device has the advantages of simple structure, reasonable design and convenient operation and use, and can judge the influence of the sulfide ore on the explosive through the heat flux difference of the reference substance and the test sample and the gas generated in the test process, predict the self-explosion danger of the explosive in the sulfide mine, realize the judgment of the influence of the sulfide ore with different components on different types of explosives, and provide guidance for the prevention of the self-explosion accidents of the sulfide mine.
Drawings
The invention is further described with reference to the following figures.
FIG. 1 is a schematic structural view of the apparatus;
FIG. 2 is a graph showing the results of data on a mixture of sulfide ore powder and explosive in this example;
FIG. 3 is a graph of data results for explosives in this example;
FIG. 4 is a graph comparing experimental data of a mixture of sulphide ore and emulsion explosive.
In the figure: 1-insulating heat preservation cover plate; 2-constant temperature calorimetric box; 3-a reference cell; 4-a gas detector; 5-a sample cell device; 6-heating element in reference cell; 7-heating elements within the sample cell; 8-a thermocouple; 9-reference heat flux sensor; 10-sample heat flux sensor; 11-a controller; 12-data terminal.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
As shown in figure 1, the experimental device for inducing explosive spontaneous explosion of sulphide ore comprises a constant temperature calorimetric box and a data terminal, wherein an insulating heat-preservation cover plate is covered at an opening at the upper part of the constant temperature calorimetric box, a reference pool and a sample pool are arranged in the constant temperature calorimetric box, heating elements are arranged in the reference pool and the sample pool, a reference object heat flux sensor is arranged at the bottom of the reference pool, a reference object can be replaced in the middle of the reference pool as required, a gas detector is arranged at the upper part of the sample pool and used for detecting gas generated after reaction of an object to be detected, thermocouples are arranged at the lower part of the sample pool and comprise two thermocouples A for monitoring the temperature of the sample and two thermocouples B for controlling the temperature of the sample, the sample heat flux sensor is arranged at the bottom of the sample pool, the constant temperature calorimetric box, the heating elements, the gas detector, the reference, The device monitors gas generated in the testing process by controlling the temperature of a testing environment, the heating rate and the proportion of the sulfide ore, compares the heat fluxes of the reference object and the sample, and judges whether the sulfide ore can induce the explosive to generate the spontaneous explosion accident or not.
In this embodiment, the data terminal may set test parameters, such as a test temperature, a temperature range, a temperature rise rate, and the like, and control the constant temperature calorimeter through the controller. The data report generated by the data terminal mainly comprises whether SO is generated in the test process2And NO gas, the difference in thermal flux between the reference cell and the sample cell. The gas detector is used for detecting SO2And a gas detector for NO gas, and other gas detection devices can be replaced according to different requirements.
In this embodiment, the heating element is an electric heating tube.
In this embodiment, the controller is a PLC, and the data terminal is a computer terminal.
A method of determining whether a sulphide ore will induce auto-detonation of an explosive, comprising the steps of:
(1) collecting sulfide ore powder in a mine blast hole, drying the sulfide ore by using a vacuum drying oven, and then grinding the sulfide ore powder to be less than 100 microns in a manual grinding mode, wherein the sulfide ore powder and explosive cannot be fully mixed due to the fact that the particle size of the sulfide ore powder is larger than 100 microns, and a test result is influenced; (2) selecting the explosive used in the mine blasting operation, and vulcanizing the ground materialAdding mineral powder into the explosive, wherein the mass of the sulfide ore powder accounts for 5-20% of the total mass, and the test effect is not obvious when the mass of the sulfide ore is too small or too large; the mixing process is carried out in an environment below 25 ℃, the mixture is slowly stirred, and the situation that the sulfide ore powder and the explosive react in advance due to overhigh temperature or too high stirring speed is prevented; when a test sample is manufactured, the total mass is more than 100g, the sulfide ore powder is added into the explosive in batches to ensure that the sample is uniformly mixed, and the test is carried out in time after the mixing is finished; (3) when the amount of the test sample is too small, the actual reaction process cannot be truly reflected, and when the amount of the test sample is too large, safety accidents are easy to happen. Weighing 0.1-1 g of sample into a sample cell of a testing device for testing; (4) the thermal decomposition temperature of the explosive is generally 200-300 ℃, the explosive still has the risk of auto-explosion under the condition of low temperature in the actual production, the test parameters are set through a data terminal, the temperature rise rate control range is 0.1-2K/min, the temperature range is 25-300 ℃, the whole reaction process can be better known through the lower temperature rise rate, and the detection efficiency can be improved through the higher temperature rise rate; (5) weighing explosives with the same mass into a sample cell of a testing device for testing, and setting the same parameters as those in the step (4) for testing; (6) the data terminal records heat flux parameters and gas parameters in the two constant temperature calorimeters to generate a data report, the data report judges the influence of the sulfide ores on the explosive according to whether SO is detected in the whole test process2And NO gas, and differences in heat flux parameters of the sulphide ore powder to the explosive mixture and explosive throughout the test.
In this embodiment, the constant temperature heating box is a self-made metal cylindrical box, and a heat insulating material is added between the box and the reference pool to reduce the internal heat loss; the data terminal is a computer, such as a Daire brand host computer, i3-9100 and a DDR 48G memory; the gas detector can be a portable multi-gas detector of the Chinese and Western brand, and the model is M327583; the heat flux sensor can be an HTT-1000 high temperature heat flow sensor; the controller can be Siemens brand programmable logic controller with model number of 6ES7214-1AD23-0XB 0; the thermocouple can be an anti-seismic and anti-corrosion thermocouple for a high-temperature furnace with a higher Hao standard, and the model is WRNN-330; the heating element can be a heating tube of an electric Teflon water electroplating heating tube with model number SL-55.
The specific implementation method for judging whether the sulfide ore can induce the explosive spontaneous explosion is given below, and comprises two test experiments, wherein the first test experiment is a test experiment for a mixture of the sulfide ore and the explosive, the second test experiment is an explosive test experiment, and whether the sulfide ore can induce the explosive spontaneous explosion is judged according to data measured by the two tests.
Sulfide ore and explosive mixture test experiment:
firstly, drying the sulphide ore for 24 hours in a vacuum drying oven at the temperature of 80 ℃, and then preparing the sulphide ore into sulphide ore powder with the particle size of less than 100 microns by adopting a manual crushing and grinding mode;
mixing the sulfide ore powder and the emulsion explosive at room temperature according to the proportion of 1:9, wherein the environmental temperature cannot be too high, so that the sulfide ore powder and the emulsion explosive are prevented from reacting in advance;
weighing 0.2g of sample by using an analytical balance, placing the sample into a sample cell, wherein a reference substance in a reference cell is Al2O3；
Then the constant temperature calorimetric box is sealed by an insulating heat-preserving cover plate, so that the heat exchange between the constant temperature calorimetric box and the outside is prevented;
setting test parameters at a data terminal, setting the temperature range to be 25-300 ℃, setting the heating rate to be 1K/min, and clicking to start testing when the difference between the heat flux of the reference object and the heat flux of the sample pool is 0;
the controller controls the heating element according to the parameters set by the data terminal and by combining the real-time temperature of the sample measured by the thermocouple; finally, transmitting the reference object heat flux, the sample pool heat flux data and the gas generation condition measured in the constant temperature calorimeters to a data terminal through a controller;
under the condition that the temperatures of the reference substance and the sample are kept the same, the data terminal maps the difference between the heat flux of the reference substance and the heat flux of the sample pool, the temperature is an abscissa, and the difference between the heat fluxes is an ordinate:
when the difference between the heat fluxes is zero, the reference substance and the sample receive the same heat flux, and the ordinate is zero; heat of reference substanceWhen the flux is larger than the heat flux of the sample pool, the sample is emitting heat at the moment, and the ordinate is larger than zero; when the heat flux of the reference substance is less than that of the sample pool, the sample is absorbing heat at the moment, and the ordinate is less than zero. The mixture of sulphide ore and explosive will react exothermically during the test and give off heat, and an upward exothermic peak appears in the figure, and the peak temperature represents the temperature at which the reaction exotherm is the greatest. FIG. 2 is a graph showing the results of data on the mixture of sulphide ore powder and explosive in this example, showing that the exothermic peak begins to change at 283.94 ℃ and the peak temperature is 283.83 ℃. Meanwhile, the gas detection device detects SO in the test process2And NO gas formation, which represents the reaction of the sulphide ore with the explosive.
Explosive testing experiments:
weighing 0.2g explosive by using an analytical balance, and placing the explosive into a sample cell, wherein a reference substance in a reference cell is Al2O3Sealing the constant temperature calorimetric box by using an insulating heat-preserving cover plate;
setting the same parameters as those of a test experiment of a mixture of the sulfide ore and the explosive at a data terminal, setting the temperature range to be 25-300 ℃, and setting the temperature rise rate to be 1K/min;
when the difference between the heat flux of the reference substance and the heat flux of the sample pool is 0, clicking to start testing;
the data terminal was plotted against the recorded data, FIG. 3 is a graph of the data results for explosives, showing that the explosive began to mutate at an exothermic peak of 289.54 deg.C, the peak temperature was 290.64 deg.C, and no SO was detected during the experiment2And NO gas.
Referring to FIG. 4, the results of two experiments are compared to find that the exothermic peak of the sample added with the sulfide ore powder is advanced by 5.71 ℃ and the peak temperature is reduced by 6.81 ℃. This shows that the sulphide ore does reduce the thermal stability of the explosive, increases the risk of explosive auto-explosion, and in actual production, the explosive cannot contact sulphide ore powder, and simultaneously ensures ventilation in the mine and prevents the temperature of the heat accumulation blast hole from rising. If the exothermic temperature and peak temperature of the two tests are not advanced, the sulfide ore can not induce explosive self-explosion.
The above-mentioned preferred embodiments, further illustrating the objects, technical solutions and advantages of the present invention, should be understood that the above-mentioned are only preferred embodiments of the present invention and should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The utility model provides an experimental apparatus for sulphide ore induces explosive auto-explosion, includes constant temperature calorimetric box, data terminal, its characterized in that: constant temperature calorimetric box upper portion opening part lid is equipped with insulating heat preservation apron, is provided with reference pond, sample cell in the constant temperature calorimetric box, and reference pond, sample cell inside all install heating element, and reference thing heat flux sensor is installed to reference pond bottom, a gas detector is installed on sample pond upper portion, and thermocouple A, the thermocouple B of a control sample temperature are installed to the sample pond lower part, and there is sample heat flux sensor sample pond bottom, constant temperature calorimetric box, heating element, gas detector, reference thing heat flux sensor, sample heat flux sensor, thermocouple A, thermocouple B all with controller electric connection, controller and data terminal electric connection.
2. An experimental apparatus for inducing explosive auto-explosion of sulphide ores according to claim 1, wherein: the heating element is an electric heating pipe.
3. An experimental apparatus for inducing explosive auto-explosion of sulphide ores according to claim 1, wherein: the controller is a PLC, and the data terminal is a computer terminal.
4. A method for determining whether a sulphide ore is capable of inducing explosive auto-detonation, using the experimental apparatus for inducing explosive auto-detonation of a sulphide ore according to claim 1, comprising the steps of:
(1) collecting sulfide ore powder in mine blast holes, drying the sulfide ore by using a vacuum drying oven, and then adopting a manual grinding methodGrinding the mixture to be less than 100 mu m; (2) selecting an explosive used in the mine blasting operation, and adding ground sulfide ore powder into the explosive, wherein the mass of the sulfide ore powder accounts for 5-20% of the total mass; the mixing process is controlled to be carried out in an environment below 25 ℃, and the mixture is slowly stirred to prevent the sulfide ores and the explosive from reacting in the mixing process; when a test sample is manufactured, the total mass is more than 100g, the sulfide ore powder is added into the explosive in batches to ensure that the sample is uniformly mixed, and the test is carried out in time after the mixing is finished; (3) weighing 0.1-1 g of sample into a sample cell of a testing device for testing; (4) setting test parameters through a data terminal, wherein the temperature rise rate control range is 0.1-2K/min, and the temperature range is 25-300 ℃; (5) weighing explosives with the same mass into a sample cell of a testing device for testing, and setting the same parameters as those in the step (4) for testing; (6) the data terminal records heat flux parameters and gas parameters in the two constant temperature calorimeters to generate a data report, the data report judges the influence of the sulfide ores on the explosive according to whether SO is detected in the whole test process2And NO gas, and differences in heat flux parameters of the sulphide ore powder to the explosive mixture and explosive throughout the test.
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