Nghiên cứu ảnh hưởng của một số yếu tố công nghệ đến quá trình thuần hóa thuốc phóng một gốc pirocxilin bằng phương pháp phun dung dịch chất thuần hóa tt tiếng anh

1 MINISTRY OF EDUCATION AND TRAINING MINISTRY OF NATIONAL DEFENCE ACADEMY OF MILITARY SCIENCE AND TECHNOLOGY PHAM QUANG HIEU STUDY OF THE INFLUENCE OF TECHNOLOGICAL FACTORS ON PHLEGMATIZED PROCESS PYROXYLIN PROPELLANT BY SPRAYING PHLEGMATIZED SOLUTION Specialization: Chemical engineering Code: 952 03 01 SUMMARY OF DOCTORAL THESIS Hanoi - 2020 This thesis has been completed at: Academy of Military Science and Technology, Ministry of Defence Scientific supervisors: Dr Pham Van Toai Assoc Prof Dr Chu Chien Huu Reviewer 1: Dr Pham Manh Thao Military Technical Academy Reviewer 2: Assoc Prof Dr Vu Minh Thanh Academy of Military Science and Technology Reviewer 3: Dr Nguyen Phương Nga General Department of Defense Industry The thesis was defended in front of the Doctoral Evaluating Council at Academy level held at Academy of Military Science and Technology at 8:30 AM, date … month … , 2020 Công nghiệp Việt Nam The thesis is able to be found at: - The Library of Academy of Military Science and Technology; - Vietnam National Library INTRODUCTION The ugency of the thesis topic Domesticated pirocxilin propellant (phlegmatization propellant) is an energy-based one (cellulose nitrate- NC) In order to reduce the average combustion rate of the propellant particles and control the combustion process of the propellant (in the direction of the fire increases positively), a layer of domestication layer is absorbed outside the propellant particles The purpose of domestication is to increase the speed of the warhead due to the increase in the amount of stuffing propellant during the shot, as the same time maximum pressure of the propellant gas produced is maintained or reduced In the world, there are many published researches on the technology of producing pirocxilin propellants However, there is very little published research on domesticated pirocxilin propellants because it is a military field that most countries keep secret, only transfer when purchasing technology Domestically, the technology for producing some labels of pirocxilin has been transferred to Vietnam by foreign partners On the basis of technology transfer documents, Vietnam National Defense Industry has also successfully studied a number of common pirocxilin propellants and was put into equipment for the military However, technologies for producing domesticated pirocxilin propellants are very limited, there have been no intensive studies on the essence of domestication, technological factors affecting product quality The aims Clarify the influence of some technological factors on the domestication of pirocxilin propellants, set up the technology parameter of domesticization of pirocxilin propellant, apply to the production of domesticated pirocxilin propellant used for high-caliber bullets 23mm and 30mm navy The ranges Issues related to domestication technology; absorption, diffusion of domestication; determination of the depth of osmotic layer, concentration of domestication; experimental evaluation of gunner target of propellants The research method The thesis uses techniques of manufacturing semi-finished product of propellant, domesticating propellant, analyzing and evaluating chemical and physical characters, and shooting Raman and IR spectrums The scientific and practical meaning The research results of the thesis have scientific significance and have practical value in the military field, establishing the domestication technology process to produce lables of 5/7SFL and 6/7FL propellants The layout The thesis consists of 127 pages distributed as follows: beginning pages, chapter - overview, 30 pages; 2- experiment, 20 pages; chapter - results and discussion, 61 pages; page conclusion; the list of scientific works has published page and 96 references Chapter INTRODUCTION Overview of pirocxilin propellants, characteristics and roles of the constituents in the composition of pirocxilin propellants; some special pirocxilin propellants Introducing the purpose of birth, the main characteristics of domesticating pirocxilin propellants Theoretical foundations of domestication of propellants Application of Raman spectrum in assessing the domestication distribution domain in propellants The situation of foreign and domestic research on domesticated pirocxilin propellants Chapter OBJECTS AND RESEARCH METHOD 2.1 The objects The subjects of the study are pirocxilin propellant samples manufactured by the thesis in order to study domestication technology 2.2 Chemicals and equipments * Chemicals: NC has a nitrogen content 208÷209 ml NO/g manufactured by Factory Z, semi-finished propellant 5/7SFL and 6/7FL, xerezin is a saturated hydrocarbon with the formula CnH2n+2 with n= 35 55, made in Thái lan Industrial camphor (C10H16O) main content >95 %, made in India * Equipments: Synchronize the production line of single-base propellants of Factory Z, domestication equipment with pilot scale and industrial scale, spectrometer equipment of Labram HR Evolution, gas chromatography equipment of Clarus 680, infrared spectrum measuring equipment of Perkin Elmer spectrum 400 2.3 Research method and using technique 2.3.1 Identify the characteristics of propellants: Use current analytical method of measurement being applied in the military field 2.3.2 The method of domestication of propellants 2.3.3 The method of creating a Raman calibration spectrometer 2.3.4 The method of creating propellant samples in Ramam spectrum measurement Figure 2.9 Create propellant samples for measuring and analyzing Raman spectrum 2.3.5 Method of determining hydrogen bonding in a domesticated layer 2.3.6 Determine the muzzle pressure in the shot Chapter RESULT AND DICUSSION 3.1 The effect of temperature on domestication 3.1.1 The effect of temperature on the uniformity of the products Table Resuts of after domestication of propellants at different temperatures No TemperatureoC Result, camphor content in the positions, % Propellant particles are cover with a white layer, wet and swollen They stick into small pieces 25-35 vt1 vt2 vt3 vt4 0,69 1,29 1,00 1,56 40-50 50-60 65-75 75-85 Propellant particles keep the shape vt1 vt2 vt3 vt4 1,43 1,44 1,48 1,46 Propellant particles keep the shape vt1 vt2 vt3 vt4 1,56 1,59 1,58 1,60 Propellant particles keep the shape, many camphor particles stick to propellants vt1 vt2 vt3 vt4 1,22 1,35 1,05 1,42 Propellant particles keep the shape, many camphor (Ca) particles stick to propellants vt1 vt2 vt3 vt4 1,12 0,94 1,19 1,33 Results shows that the domesticated temperature of 40-60oC gave uniform results of propellants 3.1.2 The effect of domesticated temperature on the total content and distribution of camphor in the product Table Analytical resuts of post-domestication of propellants at different temperatures Results Indicators M1 M2 M3 M4 M5 M6 M7 o Domesticated temperature, C 35 40 45 50 55 60 70 Camphor (Ca) content of input, % ,7 Volatile mineral content, % 1,31 1,30 1,40 1,20 1,29 1,37 1,12 Camphor content in product, % 1,20 1,33 1,42 1,48 1,57 1,45 1,28 35 oC 55 oC 70 oC 15 Camphor content % Camphor content , % 1,6 1,5 1,4 1,3 1,2 1,1 10 45 oC 60 oC 35 40 45 50 55 60 65 70 75 10 20 30 40 50 60 70 Domesticated layer depth, µm Figure The influence of temperature on the camphor content distribution Domesticated temperature oC Figure Dependence on camphor content on domesticated temperature The result has determined a suitable domestication temperature at 55±2 oC 3.2 Effect of concentration of domestication solution to domestication Table 3 Condition and analysis results of post-domestication of propellants at different concentrations of domesticated solutions Results Indicators M13 M14 M15 M16 M17 M18 Camphor/alcohol ratio,% 1/1 1/1,5 1/2 1/2,5 1/3 1/4 Concentration of Phl-solution, % 50 40 33,3 28,5 25 20 Volume of Phl-solution, g 102 127,5 153 178,5 204 255 Total spraying time, s 204 255 306 357 408 510 Spraying time time, s 40,8 63,7 76,5 89,2 102 127,5 Volatile mineral content, 1,30 1,35 1,41 1,32 1,29 1,30 Camphor content inthe product,% 1,36 1,50 1,54 1,45 1,40 1,32 LN content, % 1,55 1,5 1,45 R² = 0,9895 1,4 1,35 1,3 20 25 30 35 40 45 50 Concentration of domesticated solution, % Figure Changes in camphor content in the product when the concentration of the domesticated solution is changed The thesis determines the best condition for the domestication process to take place when the concentration of domestication solution is about 33,3÷35 % 3.3 The influence of a number of technical factors on domestication 3.3.1 Influence of spraying pressure domestication solution during domestication Conducting domestication with a concentration of domestication solution is 33,3 % (camphor/alcohol ratio = 1/2), domestication temperature o 55±2 C, camphor content 1,7 % compared to semi-finished propellants Table Selecting the spraying pressure for domestication solution Pressure, No Results Remarks kg/cm2 Mist spraying is weak, irregular, Not suitable 0,8 with droplets There is a misting stream, which Not suitable 1,2 does not cover all the inner faces There is a misting stream, which 1,5 Suitable does not cover all the inner faces Fine mist spray, which is 2,0 dispersed, even and covered Suitable enough inside the equipment Fine mist spray, which is 2,5 dispersed, even and covered Suitable enough inside the equipment Thus, for the domestication, the necessary pressure must be a minimum of 2.0 kg/cm2 to cover the entire moving surface (corresponding to the width of the inner faces of domesticated equipment) of a domestication batch including kg of propellants Table Selecting solution sparaying pressure for domestication Results, camphor content, % No Pressure, Remarks kg/cm2 The process of domestication takes place normally 2,0 Suitable vt1 vt2 vt3 vt4 1,51 1,57 1,54 1,50 The process of domestication takes place normally Suitable, 2,5 even vt1 vt2 vt3 vt4 1,58 1,55 1,57 1,55 Agglutinate products as blocks Uneven 3,0 vt1 vt2 vt3 vt4 domestication 1,32 1,48 1,61 1,26 Agglutinate products as blocks Uneven 3,5 vt1 vt2 vt3 vt4 domestication 1,59 1,38 0,97 1,16 The result of determining the pressure for spraying the best domesticated solution is in the range of 2.0 2.5 kg/cm22for the 0.2 mm nozzle; then the thesis chooses spray pressure of 2.5 kg/cm to ensure more even in camphor content of the product and suitable time for the spraying of domesticated solution 3.3.2 Determine the optimum tang mix speed during domestication In a domestication eqquipment, the propellant needs to move at the arc corresponding to the o'clock and o'clock angles, the two edges of this position fit together at an angle of 120° This process needs to take place continuously during the domestication to ensure the uniformity of the product Table Select the rotation speed of the equipment before and after spraying the domestication solution Speed, rpm No Results Remarks The propellant rotates slowly, can not reach the position of the corner Unsuitable of o'clock, ranging from 4.30 o'clock - o'clock The propellant rotates slowly, can not reach the position of the corner Unsuitable 10 of o'clock, ranging from o'clock – 6.30 o'clock The propellant rotates steadily, can reach the position of the corner of Not 15 o'clock, ranging from o'clock – suitable 6.30 o'clock The propellant rotates steadily, can reach the position of the corner of Suitable 17 o'clock, ranging from o'clock – o'clock The propellant rotates steadily, can reach over the position of the corner Unsuitable 20 of o'clock, ranging from o'clock – o'clock Table Select the rotation speed of the equipment during spraying the domestication solution Speed, rpm No Results Remarks The propellant rotates steadily, can not Need to reach the position of the corner of increase 17 o'clock, ranging from o'clock – speed o'clock The propellant rotates steadily, can reach 20 the position of the corner of o'clock, Suitable ranging from o'clock – o'clock The propellant rotates steadily, can reach the 25 position of the corner of o'clock, ranging Suitable from o'clock – o'clock There is a phenomenon of shaking the equipmen, the propellant Unsuitable 30 block movement is up in the corner of o'clock – o'clock The result of choosing the domesticated equipment's rotation speed in the sprays of solution is 20 rpm, the rotation speed of the domesticated equipment before and after each spraying of the domesticated solution is 17 rpm for the batch of kg/batch capacity 3.3.3 Effect of camphor fluid supply regime on the domestication 3.3.3.1 Select the mode of supply of the domesticated solution Table Selecting the mode of supplying and spraying domesticated solution Rotation Mode of No Time speed, Results supply rpm Spraying -Spray: 290s 20 The domesticated equipment once -Rotate: 70 17 moves unsteadily, the product with many propellants sticked into blocks Spraying -Spray 1: 145s 20 The domesticated equipment twice -Rotate 12 17 moves unsteadily, the -Spray 2: 145s 20 product with many -Rotate: 70 17 propellants sticked into blocks -Spray 1: 97s 20 The domesticated process is -Rotate 12 17 normal, propellants move Spraying -Spray 2: 97s 20 steadily, but many 3 times -Rotate: 12 17 propellants are sticked -Spray 3: 96s 20 together -Rotate: 70 17 -Spray1: 73s 20 The domesticated process -Rotate 12 17 takes place steadily, -Spray 2: 73s 20 propellants move steadily Spraying -Rotate:12 17 Camphor content, % 4 times -Spray 3: 73s 20 vt1 vt2 vt3 vt4 - Rotate: 12 17 -Spray 4: 71s 20 1,55 1,57 1,54 1,56 - Rotate: 70 17 Results for domestication of pirocxilin propellant, the number of times the solution made are times in accordance with technology requirements, ensuring uniformity of product quality, resulting in the total time for a domestication process is about 120÷125 minutes excluding the time to prepare and disassemble materials 60 Ca content, % Depth of domlayer, µm 3.3.3.2 Influence of material supply to the depth and distribution of camphor content 15 40 10 20 1s 2nd 20 3rd 4th 40 Number of spray Domestication layer depth, µm Figure Dependence of the depth of Figure The distribution ofndcamphor rd domestication layer on the number of sprays of concentration at the 1st spraying; spraying; domesticated solution spraying and 4th spraying The thesis proposes a domestication technology regime on pilot scale as shown in following Table 3.9: Table Domestication technology of single-base propellants on pilot scale Amount of Rotation No Sequence of stages substance Time speed, rpm added Domestiacation temperature: 55±2 oC, pressure 2,5kg/cm2 Camphor content of 1,3÷1,8 % compared with semi-finished propellant Supply of propellant 3,0 kg 2 Supply of graphite 1,0 g Turning heat, preliminary graphite 35-40 17 1/4 Phl4 1st solution spray 56 76 s 20 solution Rotate 12 17 nd 1/4 Phl6 solution spray 56 76 s 20 solution Rotate 12 17 rd 1/4 Phl8 solution spray 56 76 s 20 solution Rotate 12 17 1/4 Phlsolution 10 4th solution spray 58 78 s 20 2,0 g graphite 11 Rotate 75 17 + At camphor content of 1.3% compared with 3.0 kg of semifinished propellants, the concentration of domestication solution is 33.3%, the weight of domesticated solution is 117 g, the spray time is 56 s, the total time of spraying domesticated solutions for the whole cycle is 224 s 11 From the results of the calibration curve of the peak ratio of I652/I850 compared with the concentration of camphor/NC standard samples by % of mass, this dependency is obtained as follows: I 652 / I 850  0,077 C   0, 4827 (3.5) Where [C] is concentration of camphor in comparison with NC by weight,% 3.5.2 The study determines the distribution and concentration of camphor according to the depth of domesticated layer 3.5.2.1 For 6/7FL propellants Raman spectra at different point positions on 6/7FL propellant samples (with camphor content of 1.15%) as shown in Figure 3.15 below: a) b) c) d) e) f) g) h) Figure 15 Raman spectrum images at depths: μm –a); μm-b); 10 μmc); 15 μm-d); 35 μm-e); 45 μm-f); 55 μm-g); 60 μm-h) 12 Table 12 The results determine the ratios of peaks and concentrations of camphor/NC Camphor/NC content, % No Positions, μm Ratio I652/ I850 1,67 15,39 1,43 12,27 10 1,32 10,93 15 1,10 8,04 35 1,01 6,90 45 0,72 3,08 50 0,49 0,1 55 0,29 3.5.2.2 For 5/7SFL propellant Raman spectra at different point positions on the 5/7FL propellant sample (with camphor content in M28 propellant of 1,51%), which obtained spectral image as shown in Figure 3.17 below: a) b) c) d) e) f) 13 g) h) i) l) Figure 17 Raman spectrum at the point 0µm -a); 10µm -b); 20µm -c); 30µm d);55µm -e); 60µm -f); 80µm -g); 90µm -h); 95µm -i); 100µm -l) Table 13 The results determine the concentration of camphor / NC% according to the location of the depth of domestication layer Positions, μm Camphor/NC content, % No I652/ I850 ratio 1.95 19.01 10 1.03 7.10 20 0.93 5.79 30 0.89 5.31 40 0.88 5.14 50 0.89 5.31 60 0.84 4.58 70 0.85 4.83 80 0.75 3.45 10 90 0.60 1.46 11 100 0.48 0.2 Based on the results obtained in Table 3.14, the graph shows the dependence of camphor concentration (by mass,%) on the depth of domestication layer for the 5/7SFL propellant samples as shown in Figure 3.19 below: Ca content % 14 20 15 10 R² = 0.9986 0 20 40 60 80 100 20 15 10 Camphor content 1,39% 20 40 60 80 Ca content, % Depth of domestication layer, µm 20 15 10 Camphor content 20 40 60 80 100 120 140 Ca conent, % Ca content, % Depth of domestication layer X, µm Figure 19 The change in camphor/NC concentration, % in different depth positions Compared with the sample curve, the distribution curve of camphor content in the 5/7FL propellant samples follows the pattern curve, the diffusion process according to the diffusion volume of polime network, similar to the 6/7FL propellant samples From the results of the camphor concentration distribution obtained in 5/7SFL and 6/7FL propellant samples, the thesis found that there is an equilibrium concentration region in those samples For 6/7FL propellant samples in the depth of domestication layer from 15 ÷ 35 µm with camphor/NC content, balance is about 7.5% For 5/7SFL propellant samples in the depth range of 15ữ75 àm with camphor/NC content balanced by about 5.0% Raman spectroscopy results of the 5/7SFL propellant sample with camphor content in different products are shown in the following figures: 25 20 15 10 Camphor content 1,47% 20 40 60 80 100 Depth of domestication layer, µm Figure 3.20 The distribution of camphor content according to the depth of domestication layer in samples with different camphor content in different propellants Depth of domestication layer, µm The result of using the 5/7SFL M28 propellant samples to determine the absorption and diffusion of camphor solution according to the holes in the propellant particle The specific Raman spectrum is as follows: 15 a) c) b) d) Figure 3.21 Raman spectrum at locations along the edge of propellant particles: alocation20x0 µm; b- location 20x50 µm; c- location 20x90 µm; d- location 20x100 µm Results shows that the phenomenon of absorption and diffusion of camphor vertically or horizontally of 5/7SFL propellant particles are similar At distances beyond 100 µm along the edge of the 5/7SFL propellant particles, no camphor presence is observed In the domestication process, the domestication solution does not "creep" into the propellant through the 7-holes route available of the propellant particles This result also shows the difference between the method of domestication by spraying solution of the thesis compared with the method of domestication by immersion of other authors, which have differences in the structure of the domesticated layer The reason is determined by the time of contact between the propellant particles with domesticaed solution and having big differences According to the method of spraying domesticated solutions, the contact time is very small compared to the method of immersion in domesticated solutions 3.5.3 The change in combustion heat in domesticated pirocxilin propellants 3.5.3.1 For 6/7FL propellant Qv  42,8mNC  112, 2mLN  203,8 (3.6) Table 14 The change of combustion heat according to the depth of domestication layer Positions, Camphor/NC mNC, % mLN, % Qv, kJ/kg No μm concentration, % 15,39 84,24 12,97 1947,2 12,27 86,59 10,62 2310,1 10 10,93 87,63 9,58 2472,2 15 8,04 89,98 7,23 2835,5 16 35 45 50 55 60 6,90 3,08 0,0 0,0 0,0 Combustion heat, kJ/kg 90,94 94,31 97,21 97,21 97,21 6,27 2,90 0,0 0,0 0,0 2984,2 3506,6 3956,8 3956,8 3956,8 4500 4000 3500 3000 2500 2000 1500 20 40 60 Depth of domestcation layer, μm Figure 22 The change in combustion heat at different depth positions The outermost layer has the lowest combustion heat and increases gradually with the depth of the domesticated layer In addition, the combustion heat in the layers without domestication is constant Within the depth of the domesticated layer (50 μm), the combustion heat increases to 203% Qv(c) ≤ X ≤ 50 μm Qv = (3.7) 3956,8 kJ/kg 50 < X ≤ 660 μm In which: Qv(c): function shows the change in combustion heat of the domesticaed propellant layer corresponding to the depth of the domesticated layer X (μm) in the propellant; 660 μm is the average burning thickness of 2e1 of the 6/7FL propellant samples 3.5.3.2 For 5/7SFL propellant Qv  42,8mNC  112, 2mLN  580,9 (3.8) Table 15 The change of combustion heat according to the depth of domestication layer Positions, Camphor/NC mNC, mLN, Qv, No μm concentration, % % % kJ/kg 19,01 79,23 15,06 1120,2 10 7,10 88,04 6,25 2485,8 20 5,79 89,13 5,16 2654,8 30 5,31 89,54 4,75 2717,8 40 5,14 89,68 4,61 2740,2 50 5,31 89,54 4,75 2717,8 60 4,58 90,16 4,13 2814,6 17 70 4,83 89,95 4,34 2781,3 80 3,45 91,15 3,14 2967,3 90 1,46 92,93 1,36 3244,4 100 0,20 94,10 0,19 3425,5 110 0,0 94,29 0,0 3454,7 Based on the results obtained in Table 3.16, the graph depicts the dependence of the combustion heat of the propellant layer on the depth of the domestication layer on 5/7SFL propellant sample as shown in Figure 3.23 below: Combustion heat, kJ/kg 10 11 12 4000 3500 3000 2500 2000 1500 1000 20 40 60 80 100 Depth of domestication layer, μm Figure 23 The change in combustion heat at different depth positions (3.9) Qv(c) ≤ X ≤ 100 μm Qv = 3454,71 kJ/kg 100 < X ≤ 513 μm In which: Qv(c): function shows the change in combustion heat of the domesticaed propellant layer corresponding to the depth of the domesticated layer X (μm) in the propellant; 513 μm is the average burning thickness of 2e1 of the 5/7SFL propellant samples 3.6 Effect of camphor content to burning speed coefficient u1, the role of hydrogen bond between camphor and NC 3.6.1 Effect of camphor content on the combustion rate of u1 for 5/7SFL propellant The formula for calculating the u1 value of single-based propellant according to its chemical composition is shown by the following formula: 0.175.104 ( N  6.37) (3.10) u1  0.04(220  T )  3h  h ' In which: u1 has dimension (dm/s)/(kg/dm2), N is the nitrogen content in the propellant, %; T - propellant test temperature, oC; h- volatile mineral content , %; h’- volatile organic content, % Table 16 Effect of camphor content to burning speed coefficient Sample names No Indicators M0 M31 M32 M33 M34 Camphor content, % 1,26 1,30 1,50 1,55 18 Measured burning speed coefficient u1, 0,0962 0,0787 0,7040 0,0676 0,0638 mm/(bar.s) Time reaches maximum pressure, 11,0 11,50 12,0 13,0 13,37 ms Burning speed coefficient u1 are 0,0960 0,0793 0,0747 0,0740 0,0726 calculated according to (3.10), mm/(bar.s) The diagram showing the dependence of the burning speed coefficient u1 on camphor content is shown in the following figure 3.24: Burning speed coefficient u1 mm/(bar.s) 0,1 0,095 0,09 0,085 0,08 0,075 0,07 0,065 0,06 Theory Calculate 0,00 1,26 1,30 1,50 1,55 Camphor content, % Figure 24 The change in the burning speed coefficient u1 according to camphor content The results compared with the sample of pre-domesticated propellants shows that, when camphor content changes, it also change the burning speed coefficient of propellant particles Specifically, when the camphor content increases from to 1.55%, burning speed coefficient of u1 decreases by 33.68%; Thanks to this, the combustion time of the propellant to the time of maximum pressure is extended by 21.54% It is also because the time of maximum pressure is extended so that the warhead has moved a space about ∆l in the length L of the gun barrel, increasing the combustion chamber volume in balance with the gas pressure generated, due to that, the maximum peak pressure for a domesticated propellant is lower than a conventional propellant 3.6.2 The role of hydrogen bond between camphor and NC The thesis topic uses the IR spectrum to determine the spectrum of the free -OH functional group existing in the samples containing NC with different camphor content, the results are shown in the following figure 3.25: 19 -OH (free) Figure 25 IR spectrum of samples 1- 10%; 2- 20%; 3- 25%; 4- 30%; 540% camphor content compared with NC From the IR spectral graph as well as documents, in the range of 3570 3200 cm-1, it is characteristic of the peak of free –OH bond as well as hydrogen bond of this group, the peak type of this link has the form vertices being not pointed like other links for the test sample Even for the cellulose base sample in Figure 3.25, the peak of the free –OH bond is curved in the spectral range of 3300 3400 cm-1 Results shows that when the camphor content is greater than 25% (samples 3,4 and 5), the peak intensity of the free –O-H bond does not change, while at the content of 20% (sample 2) and 10% (sample 1) there is a change in the height of the peak This is because there is exists of a hydrogen bond between the hydroxyl and carbonyl functional groups =C=O, when the camphor content is greater than 25% (samples 3,4 and 5), the entire carbonyl group in camphor is linked completely saturated with hydroxyl group of NC; at camphor concentrations less than 25%, the amount of carbonyl functional group is still insufficient, not enough to create a saturated bond with the entire hydroxyl group in the NC, so the IR spectrum has been observed in the presence of the free -OH group of NC 3.7 Application of research results to the production of domesticated pirocxilin propellants on an industrial line and 23mm and 30 mm high-caliber naval bullets Table 17 Industrial domestication process for batch of 100 kg launcher Rotation Amount of Time, No Sequence of stages speed, substance added rpm Domesticated temperature: 55±2 oC, pressure 2,5 kg/cm2 Supply of propellant 100 kg 33 g (5/7SFL) Supply of graphite 100 g (6/7FL) Turning heat 35-40 24 20 10 1st solution spray Rotate 2nd solution spray Rotate 3rd solution spray Rotate 4nd solution spray 1/4 phl-solution 1/4 phl-solution 1/4 phl-solution 1/4 phl-solution 67 g (5/7SFL) 200 g (6/7FL) graphite 3,7 5,1 12 3,7 5,1 12 3,7 5,1 12 36 24 36 24 36 24 3,7 5,1 36 11 Rotate 75 24 12 Remove propellants 3.7.1 For 5/7SFL propellant Table 18 Results of creating 5/7SFL propellant No Indicators Requirements 5/7SFL-M1 5/7SFL-M2 Volatile mineral content,% 1,2 ± 0,3 1,33 1,16 Volatile organic content, % ≤ 0,8 0,69 0,59 DPA content, % 1,6 ± 0,4 1,47 1,46 Xerezin content, % 2,6 ± 0,6 2,27 2,41 Camphor content, % ≤ 1,8 1,26 1,72 Graphite content, % ≤ 0,1 0,1 0,10 Specific weight, g/cm3 ≥ 1,54 1,572 1,593 Chemical stability , h ≥ 60 68 Combustion heat, kJ/kg ≥ 3302 3305 3309 10 Combustion thickness 2e1, mm 0,50…0,58 0,534 0,513 11 Length, mm 3,0….4,0 3,6 3,4 Table 20 Test shot results of 5/7SFL-M1 propellant No Index Test conditions Requirements Results - Amount of stuffing ω= 78 g; 983+5-3 V0TB = 981,8 - The bullet is insulated at V0TB = Shoot the m/s m/s speed test a temperature of RV = 4,23 m/s (152)oC, not less than 48 RV  m/s; hours - Amount of stuffing ω= 78 g; PmTB ≤ 3017 PmTB= 2929 Shoot - The bullet is insulated at kG/cm kG/cm2 pressure a temperature of Pmmax ≤3170 Pmmax =2991 test kG/cm2 kG/cm2 (152)oC, not less than 48 hours 21 Table 21 The results of the 5/7SFL-M2 propellant test Index Test conditions Requirements Results - Amount of stuffing ω= 79,25 g; V0TB = 983+5-3 V0TB = 982,1 Shoot the - The bullet is insulated at m/s m/s temperature of speed test a RV = 3,49 RV  m/s; m/s (152)oC, not less than 48 hours - Amount of stuffing ω= PmTB ≤ 3017 PmTB= 2788 79,25 g; Shoot kG/cm kG/cm2 pressure - The bullet is insulated at a Pmmax ≤3170 Pmmax =2843 test temperature of (152)oC, kG/cm2 kG/cm2 not less than 48 hours - Amount of stuffing ω= PmTB ≤ 3320 PmTB= 3004 79,25 g; Shoot kG/cm kG/cm2 pressure - The bullet is insulated at a Pmmax ≤3486 Pmmax =3030 test temperature of (402)oC, kG/cm2 kG/cm2 not less than 24 hours The results shows that the 5/SFL-M1 and 5/7SFL-M2 propellant samples have the same combustion heat value, the camphor content of the 5/7SFL-M2 propellant sample is much higher than the 5/7SFL-M1 one Results of shooting at 15oC for two propellant samples give the same muzzle velocity value, however the maximum average pressure value of the shooting group at 15oC for a 5/7SFL-M2 propellant sample is smaller than the 5/7SFL-M1 one So obviously camphor content has an influence on the radiation value of the propellant, especially on the maximum pressure value For 5/7SFL-M2 sample with camphor content of 1,72%, the peak having pressure shifted to the outside of the shell more than the 5/7SFL-M1 sample with camphor content of 1,26%, which obtain a smaller mean Pm pressure value With this result, the 5/7SFL propellant samples can be used as a propellant dose for 23mm bullets 3.7.2 For 6/7FL propellant Table 22 Results of creating 6/7FL propellants RequireNo Indicators 6/7FL-M1 6/7FL-M2 6/7FL-M3 ments Volatile mineral content, % 1,2 ± 0,3 1,18 0,95 1,24 Volatile organic content, % ≤ 0,8 0,59 0,30 0,54 DPA content, % 1,6 ± 0,4 1,74 1,47 1,52 Camphor content, % ≤ 1,8 1,03 1,15 1,71 Graphite content, % ≤ 0,3 0,12 0,1 0,11 Specific weight, g/cm3 ≥ 1,54 1,592 1,584 1,573 No 22 Chemical stability , h ≥ 60 61 65 Combustion heat, kJ/kg ≥ 3720 3786 3803 3721 Combustion thickness 2e1, mm 0,65…0,75 0,65 0,67 0,67 Length, mm 4,0….4,5 4,06 4,1 4,01 Table 3.24 Test shot results of 6/7FL-M1 propellant No Index Test conditions Requirements Results - Amount of stuffing ω= +15 V0TB = 890 -10 V0TB = 894,0 Shoot 114,0g; m/s the m/s - The bullet is insulated at a speed RV  m/s; RV = 1,85 m/s o temperature of (152) C, test not less than 48 hours - Amount of stuffing ω= PmTB ≤ 3200 PmTB= 3080 Shoot 114,0g; kG/cm2 kG/cm2 pressure - The bullet is insulated at a P ≤ 3500 Pmmax =3132 test temperature of (152)oC, mmax kG/cm2 kG/cm2 not less than 48 hours - Amount of stuffing ω= PmTB ≤ 3520 PmTB= 3279 Shoot 114,0g; kG/cm2 kG/cm2 pressure - The bullet is insulated at a P ≤ 3850 Pmmax =3473 test temperature of (402)oC, mmax kG/cm2 kG/cm2 not less than 24 hours Table 25 Test shot results of 6/7FL-M2 propellant No Index Test conditions Requirements Results - Amount of stuffing ω= V0TB = 890+15-10 V0TB = 896,9 Shoot 117,8 g; m/s the m/s - The bullet is insulated at a speed R = 0,7 m/s R  m/s; V V temperature of (152)oC, test not less than 48 hours - Amount of stuffing ω= PmTB ≤ 3200 PmTB= 3143 Shoot 117,8 g; kG/cm2 kG/cm2 pressure - The bullet is insulated at a P ≤ 3500 Pmmax =3173 test temperature of (152)oC, mmax kG/cm2 kG/cm2 not less than 48 hours With this result, both 6/7FL-M1 and 6/7FL-M2 propellant samples produced by the thesis can be used as propellant doses for 30mm naval bullets that meet the technical conditions [8] The results of the 30 mm muzzle pressure test using the 6/7FL propellant are shown in Figure 3.28: 10 23 Figure 28 Graph P(t) determines the muzzle pressure (Pđn) The results of mouth pressure measurement with piezo probe is 650 bar (663 kG/cm2) and 680 bar (693.6 kG/cm2), respectively CONCLUSION Outcomes: The thesis has pointed out a number of technological factors affecting the domestication process of single-base pirocxilin propellants based on quantitative as well as qualitative methods: domestication temperature 55±2oC, concentration of domesticated solution 33.3 % or camphor/alcohol ratio equal to 1/2; spraying pressure of domestication solution 2,5 kg/cm2; domestication solution mode divided into times; the requirement of predomesticated propellant index having volatile mineral content less than 0.8%, volatile organic content is 0.3 0.5%; rotation speed of the mixing drum when spraying a domesticated solution is 20 rpm and at 17 rpm when the spraying of the domesticated solution is stopped; the best time to convert from domestication to drying is 36 hours These technological factors are closely related, together affecting the quality of the product Based on the results of the research, the thesis has given the technological parameters to build an overall technological process for creating domesticated pirocxilin 5/7SFL and 6/7FL propellants The thesis has determined the effect of camphor content on the combustion rate of u1 in the 5/7SFL domesticated propellants as well as the muzzle pressure on 6/7FL domesticated propellants The thesis has determined the distribution of camphor content in the domesticated layer of 5/7SFl and 6/7FL propellants, building the Raman spectral calibration curve according to the mass % ratio between camphor and NC At the same time, determine the temperature change in the 5/7SFL and 6/7FL propellant samples according to the cross-sectional surface of the propellant particles as well as the cutting surface along the hole of it The results of 5/7SFL and 6/7FL propellants manufactured on the industrial line of the General Department of Defense Industry being tested to meet the requirements of gunnery of the 23mm and 30 mm navy respectively 24 New contributions: +Determine the influence of some technological factors on the domestication of a base-single pirocxilin propellant Constructing methods for determining the depth of the domestication layer in the propellant particles and the distribution of camphor concentration in them, the method of measuring the muzzle pressure +Establish technology of 5/7SFL and 6/7FL propellants domestication at pilot scale as well as industrial production one + Successfully apply types of domesticatied pirocxilin 5/7SFL and 6/7FL propellants to meet the physical and chemical requirements, geometric dimensions and gunner targets used as a propellant dose for 23mm and 30mm naval bullets Next study: The research process to implement the thesis has opened the following research directions as follows: - Study on domestication distribution domain change under conditions of storage, exploitation and use in Vietnam's tropical climate - Research to use domestication technology to improve warhead velocity while retaining the maximum pressure value for other artillery shells - Application of Raman spectroscopy in analyzing and assessing the quality of other explosive materials LIST OF SCIENTIFIC WORKS PUBLISHED Pham Quang Hieu, Pham Van Toai, Chu Chien Huu (2017), “Research into effect of phlegmaticness, temperature and concentration of phlegmaticness on distributive area of this substance in one-base propellant”, The 5th Academic conference on natural science for young scientists, master & PhD Students from asean countries, CASEAN-5, Dalat, Viet Nam, 4-7 Oct 2017, pp.247-252 Pham Quang Hieu, Pham Van Toai, Chu Chien Huu (2018), “Regulation of burning speed for the granules of high enegry materials in military field (single-based propellant) using absorption of camphor methods”, Vietnam Journal of Science and Technology, Vol.56, No.2A, pp.51-55 Pham Quang Hieu, Pham Van Toai, Chu Chien Huu, Nguyen Ngoc Hai, Bui Anh Thuc, Nguyen Minh Tuan, Pham Kim Đao (2019), “Technology for manufacturing energy-carrying materials used as 23mm ZU-23 highcaliber projectile”, Journal of catalysis and adsorption, Vol issue 2/2019, pp.17-22 Pham Quang Hieu, Pham Van Toai, Chu Chien Huu, Le Đang Trong (2019), “Research used Raman scattering spectroscopy to determine the depth of phlegmaticness layer (camphor) in domesticated pirocxilin propellant”, Journal of Chemistry, Vol 57, issue 4E3,4, 8/2019, pp.199-202 Pham Quang Hieu, Pham Van Toai, Chu Chien Huu, Le Đang Trong (2019), “Technology for manufacturing propellant 6/7FL for 30mm naval artillery”, Journal of Chemistry and Application, Vol (48)/2019, pp.47-51 Pham Quang Hieu, Pham Van Toai, Chu Chien Huu, Nguyen Ngoc Hai, Bui Anh Thuc, Pham Kim Đao (2019), “Research identified the determine distribution (camphor) in the phlegmaticness pirocxilin”, Journal of Military Science and Technology, Vol 63, 10/2019, pp.136-143 Pham Quang Hieu, Pham Van Toai, Chu Chien Huu (5/2020), “Scientific methods for estimating the structure of deterrent layer in piroxylin propellant”, The 6th Academic conference on natural science for young scientists, master & PhD Students from asean countries, CASEAN6, Oct 2019, pp 105-110 ... Huu Reviewer 1: Dr Pham Manh Thao Military Technical Academy Reviewer 2: Assoc Prof Dr Vu Minh Thanh Academy of Military Science and Technology Reviewer 3: Dr Nguyen Phương Nga General Department... published researches on the technology of producing pirocxilin propellants However, there is very little published research on domesticated pirocxilin propellants because it is a military field... factors on the domestication of pirocxilin propellants, set up the technology parameter of domesticization of pirocxilin propellant, apply to the production of domesticated pirocxilin propellant used