Evaluation method for temperature adaptability of energetic adhesive
By storing energy-containing adhesives at high and low temperatures in a constant temperature experimental box and measuring their performance parameters, the problem of lack of temperature adaptability evaluation methods in the prior art is solved, and a systematic evaluation and performance optimization of the temperature adaptability of energy-containing adhesives is achieved.
Patent Information
- Application Number
- CN202411911004.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-24
- Publication Date
- 2025-05-06
AI Technical Summary
There is a lack of effective temperature adaptability evaluation methods in the prior art, and it is difficult to evaluate the performance changes of energy-containing adhesives under high and low temperatures for a long time.
A method for evaluating the temperature adaptability of energy-containing adhesives is proposed. By setting different temperature conditions in a constant temperature experimental box, energy-containing adhesives are stored at high and low temperatures, and their performance parameters are measured, such as molecular weight, structure, decomposition temperature and viscosity.
This method can systematically evaluate the temperature adaptability of energy-containing adhesives, provide more comprehensive support for their design, synthesis and application, reduce test data errors, and reflect subtle changes in material performance parameters.
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Figure CN119935934A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of energetic materials, relates to an energetic adhesive, and in particular to a method for evaluating the temperature adaptability of an energetic adhesive. Background Art
[0002] Binders are important components of explosives such as propellants, solid propellants, polymer bonded explosives (PBX explosives), and are their matrix and skeleton. Only under its action can the other components of propellants, solid propellants, and PBX explosives be bonded together, so that they can maintain a certain geometric shape and good mechanical properties. In addition, it can also provide propellants, solid propellants, mixed explosives, etc. with carbon, hydrogen, oxygen and other elements required for combustion and explosion.
[0003] The properties of adhesives have an important influence on the various main properties of propellants, solid propellants, and PBX explosives (such as energy performance, mechanical properties, storage performance, combustion performance, etc.), and also determine their molding and processing technology. During processing, storage and use, due to the influence of physical, chemical, biological and other factors, the internal chemical composition and structure of the adhesive will change, resulting in material performance degradation and strength failure. Changes in the performance of the adhesive often affect its use and cause economic losses, and even affect the life and safety of the charge. Therefore, in the research process of energetic adhesives, environmental adaptability research is an important evaluation indicator. Summary of the invention
[0004] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a method for evaluating the temperature adaptability of an energetic adhesive, so as to solve the technical problem that there is no basis for evaluating the temperature adaptability of an energetic adhesive in the prior art.
[0005] In order to solve the above technical problems, the present invention adopts the following technical solutions to achieve the above problems:
[0006] A method for evaluating the temperature adaptability of an energetic adhesive, the method comprising the following steps:
[0007] Step 1, sample preparation:
[0008] Weigh the energetic adhesive and put it into a bottle, screw the bottle cap tightly and seal it with a sealing film.
[0009] Step 2: High and low temperature storage of samples:
[0010] The bottle containing the energetic adhesive is placed in the middle of the temperature field of the constant temperature test box and the storage experiment is started.
[0011] Step 3: Determination of performance parameters:
[0012] After reaching the set number of experimental days, the bottle containing the energetic adhesive is taken out and placed at room temperature to measure the performance parameters of the energetic adhesive after storage.
[0013] The present invention also has the following technical features:
[0014] The method for evaluating the temperature adaptability of the energetic adhesive comprises the following steps:
[0015] Step 1, sample preparation:
[0016] Weigh 1 g of energetic adhesive and place it in a 5 mL brown sample bottle. Tighten the cap of the sample bottle and seal it with a sealing film.
[0017] Step 2: High and low temperature storage of samples:
[0018] The temperature of the constant temperature test box is set. After the temperature stabilizes, the brown sample bottle containing the energetic adhesive is placed in the middle of the temperature field of the constant temperature test box to start the storage experiment.
[0019] Step 3: Determination of performance parameters:
[0020] After the set number of experimental days is reached, the brown sample bottle containing the energetic adhesive is taken out and placed at room temperature to measure the performance parameters of the energetic adhesive after storage.
[0021] In step 1, the energetic adhesive is solid or liquid. The liquid energetic adhesive is directly weighed into a brown sample bottle, and the solid energetic adhesive needs to be processed into a sheet with a thickness not greater than 1 mm and a size not greater than 2 mm×2 mm before being weighed into a brown sample bottle.
[0022] In step 2, the temperature settings of the constant temperature experimental box are -20°C, 0°C, 40°C and 75°C respectively.
[0023] In step three, the experimental measurement days of the energetic adhesive are 0 days, 1 day, 4 days, 7 days, 14 days, 21 days, 35 days, 49 days, 63 days, 90 days, and 120 days, respectively.
[0024] In step three, the energetic adhesive taken out from the constant temperature test chamber must be placed in the dark at room temperature for 24 hours before the performance parameter measurement experiment can be carried out, and the experiment must be completed within one week after taking out.
[0025] The energetic adhesives tested on different days must be taken out on the same day for subsequent experiments.
[0026] Compared with the prior art, the present invention has the following technical effects:
[0027] (I) The method for evaluating the temperature adaptability of energetic adhesives proposed in the present invention solves the problem of having no basis for evaluating the temperature adaptability of energetic adhesives under high and low temperature conditions for a long time.
[0028] (II) The present invention takes into account the storage and use environment of the material, and comprehensively evaluates the temperature adaptability of the energetic adhesive at multiple temperature points and multiple parameters within the range of -20°C to 75°C, providing more comprehensive support for the design, synthesis and application of the energetic adhesive.
[0029] (III) The present invention adopts a method of storing samples in reverse order and clarifies the detailed requirements for sample preparation and testing, thereby reducing test data errors, eliminating the influence of factors such as humidity and light, and reflecting subtle changes in material performance parameters more accurately and reliably. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 The infrared spectra of polyazide glycidyl ether adhesive after storage at different temperatures for 120 days.
[0031] Figure 2 The infrared spectra of nitrate-based oxetane adhesive after storage at different temperatures for 120 days.
[0032] The specific contents of the present invention are further explained in detail below in conjunction with embodiments. DETAILED DESCRIPTION
[0033] It should be noted that the raw materials in the present invention, unless otherwise specified, are all raw materials known in the prior art.
[0034] Light, oxygenated ozone, temperature, microorganisms, chemical media, etc. can all cause changes in polymers. Combined with the synthesis, storage and process temperature conditions of energetic adhesives, it can be inferred that temperature is the main influencing factor of energetic adhesive changes. When the temperature rises, thermal decomposition such as chain decomposition, random breakage and side group decomposition will occur, resulting in accelerated degradation of energetic adhesives. The effect of thermal energy can not only break molecular chains, but also cross-link molecular chains. Cross-linking generates chemical bonds between chains and increases molecular weight. Excessive cross-linking makes the material hard and brittle, and the performance decreases, affecting the mechanical properties and interface characteristics of the charge. However, energetic adhesives are currently characterized mainly by basic properties, such as molecular weight and molecular weight distribution, functionality, glass transition temperature, mechanical properties, density, viscosity and thermal decomposition characteristics, and lack a systematic and comprehensive temperature adaptability evaluation method. Therefore, establishing a temperature adaptability evaluation method for energetic adhesives and characterizing the temperature change behavior of energetic adhesives on a macro scale has important guiding significance for the synthesis, processing and application of energetic adhesives.
[0035] In the present invention, the energetic adhesive is stored in high and low temperature environments, and parameters such as molecular weight, structure, decomposition temperature and viscosity of the samples before and after storage are characterized, and the temperature adaptability of the energetic adhesive is evaluated based on the variation law of the parameters.
[0036] 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.
[0037] Embodiment 1:
[0038] This embodiment provides a method for evaluating the temperature adaptability of an energetic adhesive, the method comprising the following steps:
[0039] Step 1, sample preparation:
[0040] Weigh 1 g of the azide energetic adhesive sample and place it in a 5 mL brown sample bottle. Tighten the sample bottle cap and seal it with a sealing film. Repeat weighing 41 times.
[0041] In this embodiment, the azide energetic binder refers to a polyazide glycidyl ether binder known in the art.
[0042] The polyazide glycidyl ether adhesive used in this embodiment is a liquid sample. The number average molecular weight and dispersion coefficient of the initial sample of the polyazide glycidyl ether adhesive in this embodiment are the number average molecular weight and dispersion coefficient of the sample with serial number 0d; the viscosity value of the initial sample of the polyazide glycidyl ether adhesive is the viscosity value of the sample with serial number 0d.
[0043] Step 2: High and low temperature storage of samples:
[0044] The temperatures of the constant temperature experiment box were set at -20°C, 0°C, 40°C and 75°C, respectively. After the temperature of the constant temperature experiment box was stable, the first portion of the prepared polyazide glycidyl ether adhesive was placed in the middle of the temperature field of the constant temperature experiment box, and the time before placement was marked as 120 days; on the 31st day from the beginning of the experiment, the second portion of the polyazide glycidyl ether adhesive was placed, and the time was marked as 90 days; and so on, the polyazide glycidyl ether adhesive was placed within the designed date and the corresponding date was marked, and the storage experiment was started to ensure that the polyazide glycidyl ether adhesives of different experimental measurement days were taken out on the same day.
[0045] Step 3: Determination of performance parameters:
[0046] The experimental measurement days were set to 0 days, 1 day, 4 days, 7 days, 14 days, 21 days, 35 days, 49 days, 63 days, 90 days, and 120 days, respectively. After the set experimental days were reached, the brown sample bottle containing the azide energetic adhesive was taken out, and the stored polyazido glycidyl ether adhesive was tested after being placed in the dark at room temperature for 24 hours. The structure, molecular weight and distribution of each polyazido glycidyl ether adhesive were tested by infrared spectroscopy and gel chromatography, and the viscosity value of the polyazido glycidyl ether adhesive was tested by a viscometer.
[0047] Step 4: Temperature adaptability evaluation:
[0048] The performance parameter measurement data were processed, and the adaptability of the polyazide glycidyl ether adhesive under the temperature condition was evaluated according to the characteristics or rules of the spectrum changes, and compared with the initial sample (sample numbered 0d). Figure 1 , as shown in Table 1 and Table 2.
[0049] from Figure 1 It can be seen that the infrared spectra of the polyazide glycidyl ether adhesives stored at different temperatures did not change significantly, indicating that no new chemical bonds were generated in the azide energetic adhesive during the storage process.
[0050] Table 1 Molecular weight and molecular weight distribution changes of polyazide glycidyl ether adhesives
[0051]
[0052] It can be seen from Table 1 that the number average molecular weight and molecular weight distribution of the polyazide glycidyl ether adhesive stored at different temperatures did not change significantly, indicating that during the storage process, the chain structure did not undergo obvious breakage or cross-linking.
[0053] Table 2 Viscosity changes of polyazide glycidyl ether adhesives (Pa·s)
[0054] -20℃ 0℃ 40℃ 75℃ 0d 4.83 4.84 4.85 4.85 1d 4.96 4.91 4.75 4.76 4d 5.05 5.03 4.80 4.84 7d 5.15 5.01 4.89 4.82 14d 5.18 5.02 4.86 4.89 21d 5.15 5.06 4.79 4.90 35d 5.18 5.08 4.87 5.02 49d 4.91 4.84 4.94 5.05 63d 5.19 5.14 4.98 5.17 90d 5.27 5.11 5.20 5.45 120d 5.44 5.21 5.36 5.89
[0055] It can be seen from Table 2 that when the polyazide glycidyl ether adhesive is stored at different ambient temperatures, the viscosity gradually increases with the increase of storage days, but the change is not large; when stored at 75°C, the viscosity change trend is most obvious with the increase of storage days; when stored at low temperature, the viscosity of the sample tends to increase within one week, and the lower the temperature, the more obvious the change trend.
[0056] Figure 1The experimental results in Tables 1 and 2 show that, using the temperature adaptability evaluation method for energetic adhesives of the present invention, the molecular structure, molecular weight and viscosity of the polyazido glycidyl ether adhesive do not undergo significant changes after long-term storage under different temperature conditions, indicating that the polyazido glycidyl ether adhesive has good high and low temperature adaptability and superior performance, and the probability of molecular chain breakage or cross-linking due to temperature during storage and use is low.
[0057] Embodiment 2:
[0058] This embodiment provides a method for evaluating the temperature adaptability of an energetic binder. The method is basically the same as the method provided in Example 1, except that the azide energetic binder is replaced by a nitrate energetic binder. The method comprises the following steps:
[0059] Step 1, sample preparation:
[0060] Weigh 1 g of nitrate energetic adhesive sample and place it in a 5 mL brown sample bottle. Tighten the sample bottle cap and seal it with a sealing film. Repeat weighing 41 times.
[0061] In this embodiment, the nitrate energetic binder refers to a nitrate-based oxetane binder known in the art.
[0062] The nitrate-based oxetane adhesive used in this embodiment is a liquid sample. The nitrate-based oxetane adhesive used in this embodiment is a liquid sample. The number average molecular weight and dispersion coefficient of the initial sample of the nitrate-containing energetic adhesive in this embodiment are the number average molecular weight and dispersion coefficient of the sample with serial number 0d; the viscosity value of the initial sample of the nitrate-containing energetic adhesive is the viscosity value of the sample with serial number 0d.
[0063] Step 2: High and low temperature storage of samples:
[0064] The temperatures of the constant temperature test box were set at -20°C, 0°C, 40°C and 75°C, respectively. After the temperature of the constant temperature test box was stable, the first portion of the prepared nitrate-based oxetane adhesive was placed in the middle of the temperature field of the constant temperature test box, and the time before placement was marked as 120 days; on the 31st day from the beginning of the experiment, the second portion of the nitrate-based oxetane adhesive was placed, and the time was marked as 90 days; and so on, the nitrate-based energetic adhesive was placed within the designed date and the corresponding date was marked, and the storage experiment was started to ensure that the nitrate-based oxetane adhesives of different experimental measurement days were taken out on the same day.
[0065] Step 3: Determination of performance parameters:
[0066] The experimental measurement days were set to 0 days, 1 day, 4 days, 7 days, 14 days, 21 days, 35 days, 49 days, 63 days, 90 days, and 120 days, respectively. After the set experimental days were reached, the brown sample bottle containing the nitrate energetic adhesive was taken out, and the nitrate-based oxetane adhesive was tested after being placed in the dark at room temperature for 24 hours. The structure, molecular weight and distribution of each nitrate-based oxetane adhesive were tested by infrared spectroscopy and gel chromatography, and the viscosity value of the nitrate-based oxetane adhesive was tested by a viscometer.
[0067] Step 4: Temperature adaptability evaluation:
[0068] Process the performance parameter measurement data, evaluate the adaptability of the nitrate-based oxetane adhesive under the temperature condition according to the characteristics or rules of the spectrum change, and compare and analyze it with the initial sample (sample numbered 0d), such as Figure 2 , as shown in Table 3 and Table 4.
[0069] from Figure 2 It can be seen that the infrared spectra of the nitrate-based oxetane adhesives stored at different temperatures did not change significantly, indicating that no new chemical bonds were generated in the nitrate-based energetic adhesives during the storage process.
[0070] Table 3 Molecular weight and molecular weight distribution changes of nitrate-based oxetane adhesives
[0071]
[0072]
[0073] As can be seen from Table 3, the molecular weight and molecular weight distribution of the nitrate-based oxetane adhesive stored at different temperatures did not change significantly after long-term storage below 40°C. However, the molecular weight showed a downward trend after storage at 75°C for 21 days. After storage for 91 days, the molecular weight showed an obvious downward trend and the molecular weight distribution became wider, with molecular chain breakage.
[0074] Table 4 Viscosity changes of nitrate-based oxetane adhesives (PA·S)
[0075] -20℃ 0℃ 40℃ 75℃ 0d 34.2 34.6 34.6 34.9 1d 34.4 34.6 35.3 35.2 4d 34.8 34.2 34.6 35.4 7d 34.9 34.7 34.8 36.0 14d 34.8 34.2 34.8 36.4 21d 34.7 34.6 35.4 36.0 35d 34.5 34.7 34.8 36.2 49d 34.4 34.0 35.3 36.9 63d 34.5 34.4 35.0 35.1 91d 34.6 34.6 34.9 35.8 120d 35.3 35.4 36.2 33.6
[0076] It can be seen from Table 4 that after the nitrate energetic adhesive was stored at -20°C, 0°C and 40°C for 120 days, the viscosity increased, but the increase was very small; while when stored at 75°C, the viscosity first increased and then decreased.
[0077] Figure 2The experimental results in Tables 3 and 4 indicate that the nitrate-based oxetane adhesive has good room temperature and low temperature performance, but will degrade under high temperature for a long time. Long-term high temperature environment should be avoided during production, use and storage.
[0078] Examples 1 and 2 illustrate that the method for evaluating the temperature adaptability of energetic adhesives proposed in the present invention provides an evaluation basis for the temperature adaptability of different energetic adhesives under high and low temperature conditions for a long time.
Claims
1. A method for evaluating the temperature adaptability of an energetic adhesive, characterized in that: The method comprises the following steps: Step 1, sample preparation: Weigh the energetic adhesive and put it into a bottle, screw the bottle cap tightly and seal it with a sealing film; Step 2: High and low temperature storage of samples: The bottle containing the energetic adhesive was placed in the middle of the temperature field of the constant temperature test box and the storage experiment was started; Step 3: Determination of performance parameters: After reaching the set number of experimental days, the bottle containing the energetic adhesive is taken out and placed at room temperature to measure the performance parameters of the energetic adhesive after storage.
2. The method for evaluating the temperature adaptability of an energetic adhesive according to claim 1, wherein: The method specifically comprises the following steps: Step 1, sample preparation: Weigh 1 g of energetic adhesive and place it in a 5 mL brown sample bottle. Tighten the cap of the sample bottle and seal it with a sealing film. Step 2: High and low temperature storage of samples: Set the temperature of the constant temperature test box. After the temperature stabilizes, place the brown sample bottle containing the energetic adhesive in the middle of the temperature field of the constant temperature test box and start the storage experiment. Step 3: Determination of performance parameters: After the set number of experimental days is reached, the brown sample bottle containing the energetic adhesive is taken out and placed at room temperature to measure the performance parameters of the energetic adhesive after storage.
3. The method for evaluating the temperature adaptability of an energetic adhesive according to claim 1, wherein: In step 1, the energetic adhesive is solid or liquid. The liquid energetic adhesive is directly weighed into a brown sample bottle, and the solid energetic adhesive needs to be processed into a sheet with a thickness not greater than 1 mm and a size not greater than 2 mm×2 mm before being weighed into a brown sample bottle.
4. The method for evaluating the temperature adaptability of an energetic adhesive according to claim 1, wherein: In step 2, the temperature settings of the constant temperature experimental box are -20°C, 0°C, 40°C and 75°C respectively.
5. The method for evaluating the temperature adaptability of an energetic adhesive according to claim 1, wherein: In step three, the experimental measurement days of the energetic adhesive are 0 days, 1 day, 4 days, 7 days, 14 days, 21 days, 35 days, 49 days, 63 days, 90 days, and 120 days, respectively.
6. The method for evaluating the temperature adaptability of an energetic adhesive according to claim 1, wherein: In step three, the energetic adhesive taken out from the constant temperature test chamber must be placed in the dark at room temperature for 24 hours before the performance parameter measurement experiment can be carried out, and the experiment must be completed within one week after taking out.
7. The method for evaluating the temperature adaptability of an energetic adhesive according to claim 1, wherein: The energetic adhesives tested on different days must be taken out on the same day for subsequent experiments.