Multi-dimensional evaluation method for interaction of components of volatile explosives and powders

Abstract

The invention provides a multi-dimensional evaluation method for interaction of components of volatile explosives and powders. The method comprises the following steps: step 1, preparation of explosives and powders samples and single-component samples in the explosives and powders samples; 2, monitoring decomposition characteristic quantities of the explosive and powder samples and single-component samples in the explosive and powder samples; and step 3, evaluating the interaction of the components in the explosive and powder sample. According to the multi-dimensional evaluation method for the interaction of the components of the volatile explosives and powders provided by the invention, the sample is placed in the semi-closed sample pool for testing, so that the technical problem of blank of an evaluation method for the interaction of the components of the volatile explosives and powders in a formula is solved; meanwhile, an evaluation method for monitoring the interaction of the components of the explosives and powders by a thermal-mass spectrometry method is established, so that the dynamic real-time monitoring of the evaluation process can be realized; the interaction of the explosive and powder samples is evaluated from multiple dimensions of decomposition heat release, weightlessness and gas product decomposition, and the evaluation result is more reliable.

Description

Technical Field

[0001] The invention belongs to the technical field of safety assessment of explosives and pyrotechnics, relates to an evaluation method for explosive components, and specifically relates to a multi-dimensional evaluation method for the interaction of volatile explosive components. Background Art

[0002] Higher energy and stronger battlefield survivability are the core requirements for explosives in future wars. In order to meet the high-energy demand, new formulas in the explosives industry are emerging one after another. The evaluation of component interactions is one of the key parameters for the safety evaluation of new formulas. With the diversification of explosive materials, there are various charging forms such as liquid, solid-liquid mixed, and gel. Due to the volatilization of their own components, their stability also changes accordingly. The commonly used interaction evaluation methods currently include "pressure sensor method for vacuum stability test", "differential thermal analysis and differential scanning calorimetry for stability and compatibility" and "micro-calorimetry for stability and compatibility". In the actual specific application process of these methods, there are many problems such as single evaluation dimension, different evaluation standards and inapplicability to volatile sample components. Summary of the invention

[0003] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a multi-dimensional evaluation method for the interaction between volatile explosive components, so as to solve the technical problem of the lack of evaluation methods for the interaction between volatile explosive components in the prior art.

[0004] In order to solve the above technical problems, the present invention adopts the following technical solutions to achieve the above problems:

[0005] A multi-dimensional evaluation method for the interaction between volatile explosive components, the method comprising the following steps:

[0006] Step 1: Preparation of explosive samples and single-component samples in explosive samples:

[0007] The explosive sample and the single component sample in the explosive sample are weighed and placed in semi-closed sample cells respectively, so as to obtain a semi-closed sample cell containing the explosive sample and a semi-closed sample cell containing the single component sample in the explosive sample.

[0008] Step 2: Monitoring the decomposition characteristics of explosive samples and single-component samples in explosive samples:

[0009] The semi-closed sample cell containing the explosive sample obtained in step 1 and the semi-closed sample cell containing the single-component sample of the explosive sample are respectively placed in the synchronous thermal analyzer, and the nitrogen purge gas is turned on. First, a suitable heating rate and heating temperature range are selected to carry out the decomposition experiment, and the heat flow curve and the mass change curve of the sample over time during the heating decomposition process are recorded. Then, the mass spectrometer is turned on, and the scanning characteristic mass parameters of the mass spectrometer are set. The mass spectrometer is run to collect and monitor the characteristic mass spectrum signal corresponding to the mass number ion channel of the mass spectrometer over time in real time.

[0010] Step 3: Evaluation of the interaction between components in explosive samples:

[0011] The heat flow curve, mass change curve with time and the corresponding characteristic mass spectrum signal change curve with time of the explosive sample and the single component sample in the explosive sample obtained by real-time monitoring in the heating decomposition process in step 2 are taken as ΔT 1 =(T i1 -T 1 ) max , ΔT 2 =(T i2 -T 2 ) max , ΔT 3 =(T i3 -T 3 ) max , and take the maximum value ΔT by comparison max As an evaluation parameter for evaluating the interaction between components in explosive samples, if ΔT max ≤2℃, there is no interaction between the components in the explosive sample. If ΔT max >2℃, there is interaction between the components in the explosive sample.

[0012] in,

[0013] i represents a single component sample in the explosive sample.

[0014] T i1 It indicates the decomposition temperature corresponding to the maximum heat flow rate of a single component sample in a propellant and explosive sample during the heating process.

[0015] T i2 It indicates the decomposition temperature corresponding to the maximum weight loss rate of a single component sample in a pyrotechnic explosive sample during heating.

[0016] T i3 It indicates the decomposition temperature at which the concentration of the characteristic mass spectrometer signal of a single component sample in the explosive sample is maximum during the heating process.

[0017] T 1It indicates the decomposition temperature corresponding to the maximum heat flow rate of the explosive sample during the heating process.

[0018] T 2 It indicates the decomposition temperature corresponding to the maximum weight loss rate of the explosive sample during heating.

[0019] T 3 It indicates the decomposition temperature at which the concentration of the characteristic mass spectrometer signal of the explosive sample is maximum during the heating process.

[0020] ΔT 1 It represents the difference between the decomposition temperature corresponding to the maximum value of the heat flow rate of the single component sample in the explosive sample during the heating process and the decomposition temperature corresponding to the maximum value of the heat flow rate of the explosive sample during the heating process.

[0021] ΔT 2 It represents the difference between the decomposition temperature corresponding to the maximum weight loss rate of the single component sample in the explosive sample during the heating process and the decomposition temperature corresponding to the maximum weight loss rate of the explosive sample during the heating process.

[0022] ΔT 3 It represents the difference between the decomposition temperature at which the concentration of the characteristic mass spectrum signal of a single component sample in the explosive sample changes with time during the heating process and the decomposition temperature at which the concentration of the characteristic mass spectrum signal of the explosive sample changes with time during the heating process.

[0023] ΔT max = ΔT 1 , ΔT 2 and ΔT 3 The maximum value in .

[0024] The present invention also has the following technical features:

[0025] In step 1, the masses of the explosive sample and the single-component sample in the explosive sample in the semi-closed sample pool are both 1 to 5 mg.

[0026] In step 2, the nitrogen purge rate is between 25 mL / min and 100 mL / min; the heating rate is between 1 K / min and 20 K / min; and the temperature range is between 40° C. and 500° C.

[0027] Compared with the prior art, the present invention has the following technical effects:

[0028] (I) The multi-dimensional evaluation method for the interaction between volatile explosive components proposed in the present invention solves the technical problem of the lack of an evaluation method for the interaction between volatile explosive components in a formulation by placing the sample in a semi-closed sample cell for testing.

[0029] (II) The multi-dimensional evaluation method for the interaction between volatile explosive components proposed in the present invention has established a method for monitoring the interaction between explosive components using a thermal-mass spectrometry method, which can realize dynamic real-time monitoring of the evaluation process; the interaction between explosive samples is evaluated from multiple dimensions of decomposition heat release, weight loss and decomposition gas products, and the evaluation results are more reliable.

[0030] (III) The experimental samples used in the present invention are in the milligram level, the sample amount is small, and the experimental process is short and safe. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 Schematic diagram of the structure of the semi-closed sample pool.

[0032] Figure 2 Heat flow curves of DNTF-double base component (NC-NG) mixture, DNTF and double base component (NC-NG) during heating.

[0033] Figure 3 The curves showing the change of mass of DNTF-double base component (NC-NG) mixture, DNTF and double base component (NC-NG) with time during heating process.

[0034] Figure 4 The curves showing the change of characteristic mass spectrometry signals of the DNTF-double radical component (NC-NG) mixture, DNTF and double radical component (NC-NG) over time.

[0035] The meanings of the numbers in the figure are: 1-sample cell cover, 2-sample cell, 3-gasket.

[0036] The specific contents of the present invention are further explained in detail below in conjunction with embodiments. DETAILED DESCRIPTION

[0037] It should be noted that the devices and raw materials used in the present invention, unless otherwise specified, are all devices and raw materials known in the prior art.

[0038] This embodiment provides a multi-dimensional evaluation method for the interaction between volatile explosive and fire powder components. The method comprises the following steps: placing semi-closed sample cells containing explosive and fire powder samples and single-component samples in the explosive and fire powder samples into a synchronous thermal analyzer for testing. The decomposition heat release and weight loss rate of the explosive and fire powder samples and the single-component samples in the explosive and fire powder samples are studied from the perspectives of heat release and weight loss by using a synchronous thermal analysis method. The decomposition products of the explosive and fire powder samples and the single-component samples in the explosive and fire powder samples are collected and analyzed by using a mass spectrometer. The interaction between the components in the explosive and fire powder samples is evaluated by the temperature changes corresponding to the maximum values ​​of heat release, weight loss and gas product concentration.

[0039] In accordance with the above technical scheme, specific embodiments of the present invention are given below. It should be noted that the present invention is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical scheme of this application fall within the protection scope of the present invention.

[0040] Example:

[0041] This embodiment provides a multi-dimensional evaluation method for the interaction between volatile explosive components, which includes the following steps:

[0042] Step 1: Preparation of explosive samples and single-component samples in explosive samples:

[0043] Weigh 1 mg of DNTF-double radical component (NC-NG) mixture, 1 mg DNTF and 1 mg double radical component (NC-NG) into a semi-closed sample cell to obtain a semi-closed sample cell containing a DNTF-double radical component (NC-NG) mixture, a semi-closed sample cell of DNTF and a semi-closed sample cell of double radical component (NC-NG).

[0044] The explosive sample used in this example is a DNTF-double base component (NC-NG) mixture.

[0045] The DNTF used in this embodiment is the DNTF (2,4-dinitromethylaniline) known in the art; the double-base component (NC-NG) adopts the double-base component known in the art, wherein NC is nitrocellulose and NG is glyceryl trinitrate; the semi-closed sample cell is a semi-closed sample cell known in the art suitable for placing volatile components, such as Figure 1 shown.

[0046] Step 2: Monitoring the decomposition characteristics of explosive samples and single-component samples in explosive samples:

[0047] The semi-closed sample cell containing the DNTF-double radical component (NC-NG) mixture obtained in step 1, the semi-closed sample cell of DNTF and the semi-closed sample cell of the double radical component (NC-NG) are placed in the synchronous thermal analyzer respectively, and the nitrogen purge gas is turned on. The nitrogen purge rate is set between 25 mL / min and 100 mL / min, the heating rate is between 1 K / min and 20 K / min, and the temperature range is between 40 ° C and 500 ° C. The decomposition experiment is carried out, and the heat flow curves and mass change curves of the DNTF-double radical component (NC-NG) mixture, DNTF and double radical component (NC-NG) during the heating decomposition process are recorded. The heat flow curves are as follows: Figure 2 The curve of mass changing with time is shown in Figure 3 shown.

[0048] Then open the mass spectrometer, set the scanning characteristic mass parameters of the mass spectra of the DNTF-double radical component (NC-NG) mixture, DNTF and double radical component (NC-NG) to 30, 44, 46, 68, 70 and 84 respectively, run the mass spectrometer, and collect and monitor the characteristic mass spectrometer signal corresponding to the mass number ion channel of the mass spectrometer over time in real time, such as Figure 4 shown.

[0049] Step 3: Evaluation of the interaction between components in explosive samples:

[0050] The heat flow curve, mass change curve with time, and corresponding characteristic mass spectrometry signal change curve with time of the DNTF-double-base component (NC-NG) mixture, DNTF and double-base component (NC-NG) obtained by real-time monitoring in the analysis step 2 during the heating decomposition process are taken. 1 =(T i1-DNTF -T i1-(DNTF-双基组分) ) max , ΔT 2 =(T i2-DNTF -T i2-(DNTF-双基组分) ) max , ΔT 3 =(T (i3-84)-DNTF -T (i3-84)-(DNTF-双基组分) ) max , and take the maximum value ΔT by comparison max As an evaluation parameter for evaluating the interaction between DNTF and the double radical component (NC-NG) in the DNTF-double radical component (NC-NG) mixture, if ΔT max ≤2℃, there is no interaction between DNTF and the double radical component (NC-NG) in the DNTF-double radical component (NC-NG) mixture. If ΔT max >2°C, there is interaction between DNTF and the double radical component (NC-NG) in the DNTF-double radical component (NC-NG) mixture.

[0051] Table 1 Decomposition characteristic parameters of DNTF-dual base component (NC-NG) mixture and its components (unit: °C)

[0052] <![CDATA[T i1 ]]> <![CDATA[T i2 ]]> <![CDATA[T i3-30 ]]> <![CDATA[T i3-44 ]]> <![CDATA[T i3-46 ]]> <![CDATA[T i3-68 ]]> <![CDATA[T i3-70 ]]> <![CDATA[T i3-84 ]]> DNTF 281.1 274.5 275.2 276.2 276.4 276.8 277.4 294.0 Double base components 206.1 193.7 153.1 151.9 150.3 - - - DNTF-Dual Base Component 204.7 192.2 191.3 202.4 190.1 192.9 190.4 197.4

[0053] in,

[0054] i represents a single component sample in a DNTF-dual base component (NC-NG) mixture.

[0055] T i1-DNTF It indicates the decomposition temperature corresponding to the maximum heat flow rate of DNTF during the heating process.

[0056] T i2-DNTFIt indicates the decomposition temperature corresponding to the maximum weight loss rate of DNTF during heating.

[0057] T (i3-84)-DNTF It indicates the decomposition temperature at which the concentration of DNTF is maximum during the change of the characteristic mass spectrometry signal over time during the heating process.

[0058] T i1-(DNTF-双基组分) It represents the decomposition temperature corresponding to the maximum heat flow rate of the DNTF-double base component (NC-NG) mixture during heating.

[0059] T i2-(DNTF-双基组分) It indicates the decomposition temperature corresponding to the maximum weight loss rate of the DNTF-double base component (NC-NG) mixture during heating.

[0060] T (i3-84)-(DNTF-双基组分) It represents the decomposition temperature at which the concentration of the characteristic mass spectrometer signal of the DNTF-biradical component (NC-NG) mixture during heating changes with time.

[0061] ΔT 1 It represents the difference between the decomposition temperature corresponding to the maximum heat flow rate of DNTF during heating and the decomposition temperature corresponding to the maximum heat flow rate of the DNTF-double base component (NC-NG) mixture during heating.

[0062] ΔT 2 It represents the difference between the decomposition temperature corresponding to the maximum weight loss rate of DNTF during heating and the decomposition temperature corresponding to the maximum weight loss rate of the DNTF-double base component (NC-NG) mixture during heating.

[0063] ΔT 3 It represents the difference between the decomposition temperature of the characteristic mass spectrum signal of DNTF at the maximum concentration during the time-varying process during heating and the decomposition temperature of the characteristic mass spectrum signal of the DNTF-biradical component (NC-NG) mixture at the maximum concentration during the time-varying process during heating.

[0064] ΔT max = ΔT 1 , ΔT 2 and ΔT 3 The maximum value in .

[0065] As shown in Table 1, take ΔT 1 =(T i1-DNTF -T i1-(DNTF-双基组分) ) max =76.4℃, ΔT 2 =(T i2-DNTF -T i2-(DNTF-双基组分) ) max =82.3℃, ΔT 3=(T (i3-84)-DNTF -T (i3-84)-(DNTF-双基组分) ) max =96.6℃, and take the maximum value ΔT by comparison max =96.6°C as the interaction parameter for evaluating the components of the DNTF-biradical (NC-NG) mixture. ΔT max >2°C, there is interaction between the components of the DNTF-bibasic component mixture. The multi-dimensional evaluation method for the interaction between volatile explosive components proposed in the present invention solves the technical problem of the lack of an evaluation method for the interaction between volatile explosive components in a formulation by placing the sample in a semi-closed sample cell for testing.

Claims

1. A multi-dimensional evaluation method for the interaction between volatile explosive components, characterized in that: The method comprises the following steps: Step 1: Preparation of explosive samples and single-component samples in explosive samples: Weigh the explosive sample and the single component sample in the explosive sample and place them in semi-closed sample cells respectively, so as to obtain a semi-closed sample cell containing the explosive sample and a semi-closed sample cell containing the single component sample in the explosive sample; Step 2: Monitoring the decomposition characteristics of explosive samples and single-component samples in explosive samples: The semi-closed sample cell containing the explosive sample obtained in step 1 and the semi-closed sample cell containing the single-component sample of the explosive sample are respectively placed in a synchronous thermal analyzer, and the nitrogen purge gas is turned on. A suitable heating rate and heating temperature range are first selected to perform a decomposition experiment, and the heat flow curve and the mass change curve of the sample over time during the heating decomposition process are recorded. Then, the mass spectrometer is turned on, the scanning characteristic mass parameter of the mass spectrometer is set, and the mass spectrometer is run to collect and monitor the characteristic mass spectrum signal corresponding to the mass number ion channel of the mass spectrometer over time in real time; Step 3: Evaluation of the interaction between components in explosive samples: The heat flow curve, mass change curve with time and corresponding characteristic mass spectrum signal change curve with time of the explosive sample and the single component sample in the explosive sample obtained by real-time monitoring in the heating decomposition process in step 2 are taken as ΔT1=(T i1 -T1) max , ΔT2=(T i2 -T2) max , ΔT3=(T i3 -T3) max , and take the maximum value ΔT by comparison max As an evaluation parameter for evaluating the interaction between components in explosive samples, if ΔT max ≤2℃, there is no interaction between the components in the explosive sample. If ΔT max >2℃, there is interaction between the components in the explosive sample; in, i represents a single-component sample in the explosive sample; T i1 It indicates the decomposition temperature corresponding to the maximum value of heat flow rate of a single component sample in the explosive sample during heating; T i2 It indicates the decomposition temperature corresponding to the maximum weight loss rate of a single component sample in a pyrotechnic explosive sample during heating; T i3 It indicates the decomposition temperature at which the concentration of the characteristic mass spectrometer signal of a single component sample in the explosive sample is the maximum during the heating process; T1 represents the decomposition temperature corresponding to the maximum heat flow rate of the explosive sample during the heating process; T2 represents the decomposition temperature corresponding to the maximum weight loss rate of the explosive sample during heating; T3 represents the decomposition temperature at which the concentration of the characteristic mass spectrometer signal of the explosive sample is the highest during the heating process; ΔT1 represents the difference between the decomposition temperature corresponding to the maximum value of the heat flow rate of the single component sample in the explosive sample during the heating process and the decomposition temperature corresponding to the maximum value of the heat flow rate of the explosive sample during the heating process; ΔT2 represents the difference between the decomposition temperature corresponding to the maximum weight loss rate of the single component sample in the explosive sample during the heating process and the decomposition temperature corresponding to the maximum weight loss rate of the explosive sample during the heating process; ΔT3 represents the difference between the decomposition temperature at which the characteristic mass spectrum signal of the single component sample in the explosive sample changes with time during the heating process and the decomposition temperature at which the characteristic mass spectrum signal of the explosive sample changes with time during the heating process; ΔT max is the maximum value among ΔT1, ΔT2 and ΔT3.

2. The multi-dimensional evaluation method for the interaction between volatile explosive components as claimed in claim 1, characterized in that: In step 1, the masses of the explosive sample and the single-component sample in the explosive sample in the semi-closed sample pool are both 1 to 5 mg.

3. The multi-dimensional evaluation method for the interaction between volatile explosive components as claimed in claim 1, characterized in that: In step 2, the nitrogen purge rate is between 25 mL / min and 100 mL / min; the heating rate is between 1 K / min and 20 K / min; and the temperature range is between 40° C. and 500° C.

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