CN110790618A - Method for removing residual sulfur on surface of propellant powder - Google Patents
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- 239000003380 propellant Substances 0.000 title claims abstract description 164
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 118
- 239000011593 sulfur Substances 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 title 1
- 238000003756 stirring Methods 0.000 claims abstract description 58
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- 238000006477 desulfuration reaction Methods 0.000 claims description 27
- 230000023556 desulfurization Effects 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 238000010304 firing Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 4
- 235000019645 odor Nutrition 0.000 description 15
- 238000004458 analytical method Methods 0.000 description 6
- 230000006872 improvement Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000000750 progressive effect Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000002925 chemical effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000006343 physiological stress response Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000006388 psychological stress response Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
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- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0091—Elimination of undesirable or temporary components of an intermediate or finished product, e.g. making porous or low density products, purifying, stabilising, drying; Deactivating; Reclaiming
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Abstract
本发明公开了一种发射药表面残留硫脱除方法，涉及发射药技术领域，其技术方案要点：具体包括以下步骤：步骤1)：采用超声清洗机对某表面含硫发射药进行超声清洗，脱除发射药表面残留的水溶性硫化物；步骤2)：脱除发射药表面残留的单质硫，将步骤1)中脱除表面残留的水溶性硫化物的发射药和500ml反应试剂溶液加入带有搅拌装置的三口烧瓶内进行搅拌反应，并控制搅拌反应的温度和时间；步骤3)：对经过步骤1)和步骤2)处理的发射药进行硫元素含量检测。本技术方案利用简单的物理化学方法，能够实现发射药表面残留硫的脱除，从而大幅度降低发射药中硫元素的含量，有效地抑制发射药在射击过程中产生的刺激性气味。
The invention discloses a method for removing residual sulfur on the surface of a propellant, and relates to the technical field of propellant. The main points of the technical solution include the following steps: Step 1): using an ultrasonic cleaning machine to ultrasonically clean the sulfur-containing propellant on a surface, Remove the residual water-soluble sulfide on the surface of the propellant; step 2): remove the residual elemental sulfur on the surface of the propellant, add the propellant and 500ml of the reaction reagent solution from the water-soluble sulfide remaining on the surface of the propellant in step 1) into the belt. A stirring reaction is carried out in a three-necked flask with a stirring device, and the temperature and time of the stirring reaction are controlled; step 3): carry out sulfur element content detection on the propellant treated in step 1) and step 2). The technical solution utilizes simple physical and chemical methods to remove residual sulfur on the surface of the propellant, thereby greatly reducing the content of sulfur in the propellant and effectively suppressing the irritating odor produced by the propellant during firing.
Description
技术领域technical field
本发明涉及发射药技术领域，更具体地说，它涉及一种发射药表 面残留硫脱除方法。The present invention relates to the technical field of propellant, and more particularly, to a method for removing residual sulfur on the surface of propellant.
背景技术Background technique
发射药是实现身管武器发射不可或缺的能源物质，其组分是决定 发射药性能的重要因素之一。身管武器发射过程，除了完成武器的基 本功能以外，同时对武器的使用环境也将产生诸多负面影响。这些影 响是武器内弹道过程物理化学作用结果，具体表现在发射烟焰、膛内 残渣、炮口压力波、发射噪声与振动和有毒有害气体等有害现象。The propellant is an indispensable energy material to realize the launch of the barrel weapon, and its composition is one of the important factors that determine the performance of the propellant. In addition to completing the basic functions of the weapon, the process of launching the weapon will also have many negative effects on the use environment of the weapon. These effects are the result of the physical and chemical effects of the ballistic process in the weapon, and are manifested in harmful phenomena such as the emission of smoke and flames, residues in the chamber, muzzle pressure waves, emission noise and vibration, and toxic and harmful gases.
实现能量释放由慢到快的高渐增性，成为决定武器性能的核心与 关键技术，也是国际军械领域前沿发展方向。为了获得发射药能量释 放渐高增性，本发明人已申请国防专利，所制备的发射药具有较高的 能量释放渐增性。然而，在制备的过程中，该类发射药表面残余硫元 素，硫元素的存在使得发射药在燃烧过程中产生了二氧化硫等刺激性 的有毒有害气体，易造成大气污染。同时，在射击过程中，二氧化硫 等刺激性气味将引起作战人员严重的生理和心理应激反应，从而导致 健康水平和作战效能的降低。发射药中硫元素的存在无疑加剧了对作 战环境产生的负面影响，抑制了该类发射药的发展。Achieving high incrementality of energy release from slow to fast has become the core and key technology that determines the performance of weapons, and is also the frontier development direction of the international ordnance field. In order to obtain the progressive increase in the energy release of the propellant, the present inventor has applied for a national defense patent, and the prepared propellant has a high energy release progressive. However, in the process of preparation, there is residual sulfur on the surface of this type of propellant, and the presence of sulfur makes the propellant produce irritating toxic and harmful gases such as sulfur dioxide during the combustion process, which is easy to cause air pollution. At the same time, in the process of shooting, irritating odors such as sulfur dioxide will cause serious physiological and psychological stress responses of combat personnel, resulting in a decrease in health level and combat effectiveness. The existence of sulfur element in the propellant undoubtedly exacerbates the negative impact on the combat environment and inhibits the development of this type of propellant.
目前，现有技术中，尚无表面残留硫火药中硫的脱除方法，因此， 在发射药领域对该类表面含硫的高渐增性发射药进行脱硫处理，进一 步提升发射药性能，为作战人员提供优良的作战环境是迫切需要解决 的重要问题。At present, in the prior art, there is no method for removing sulfur from residual sulfur gunpowder on the surface. Therefore, in the field of propellants, desulfurization treatment is performed on such high-incremental propellants containing sulfur on the surface to further improve the performance of the propellant, which is Providing a good combat environment for fighters is an important problem that needs to be solved urgently.
发明内容SUMMARY OF THE INVENTION
本发明的目的是提供一种发射药表面残留硫脱除方法，利用了物 理化学方法，能够对发射药表面的残留硫进行脱除，从而大幅度降低 发射药中硫元素的含量，有效地抑制发射药在射击过程中的刺激性气 味。The purpose of the present invention is to provide a method for removing residual sulfur on the surface of the propellant, which can remove the residual sulfur on the surface of the propellant by using a physical and chemical method, thereby greatly reducing the content of sulfur in the propellant and effectively suppressing the The pungent smell of the propellant during firing.
本发明的上述技术目的是通过以下技术方案得以实现的：一种发 射药表面残留硫脱除方法，具体包括以下步骤：The above-mentioned technical purpose of the present invention is achieved through the following technical solutions: a method for removing residual sulfur on the surface of propellant, specifically comprising the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为50-100℃，超声清洗的时 间设置为5-60min，得到脱除表面残留的水溶性硫化物的某发射药样 品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, The three-necked flask is put into an ultrasonic cleaning machine for ultrasonic cleaning, the ultrasonic cleaning temperature of the ultrasonic cleaning machine is set to 50-100 ° C, and the ultrasonic cleaning time is set to 5-60 min, to obtain a certain method for removing the residual water-soluble sulfide on the surface. Propellant samples;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml反应试剂溶液加入带有搅拌装置的三 口烧瓶内，进行搅拌反应，并控制搅拌反应的温度和时间，然后将搅 拌反应完成后的某发射药样品洗涤过滤，脱除某发射药样品表面残余 的硫单质，然后将脱除表面残余的硫单质的某发射药样品置于60℃ 水浴烘箱内干燥2d(2天)，得到脱除表面残留硫的某发射药样品；2) Remove elemental sulfur, add a certain propellant sample obtained in step 1) from the water-soluble sulfide remaining on the surface and 500ml of the reaction reagent solution into a three-necked flask with a stirring device, carry out stirring reaction, and control the stirring The temperature and time of the reaction, then wash and filter a certain propellant sample after the stirring reaction is completed to remove the residual sulfur element on the surface of a certain propellant sample, and then place a certain propellant sample with the residual sulfur element removed on the surface at 60 ℃ Dry in a water-bath oven for 2 days (2 days) to obtain a propellant sample with residual sulfur removed from the surface;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
本发明进一步设置为：步骤2)中进行搅拌反应的温度为室温 -80℃，搅拌反应的时间为5-360min。The present invention is further set as follows: in step 2), the temperature of the stirring reaction is room temperature-80°C, and the time of the stirring reaction is 5-360 min.
本发明进一步设置为：步骤2)中所述的反应试剂溶液为过氧化 氢溶液、浓度为0.1～5wt％的氢氧化钠溶液和浓度为0.1～15wt％的稀 硝酸溶液中的一种。The present invention is further configured as follows: the reaction reagent solution described in step 2) is one of a hydrogen peroxide solution, a sodium hydroxide solution with a concentration of 0.1-5wt% and a dilute nitric acid solution with a concentration of 0.1-15wt%.
本发明具有以下有益效果：利用了物理化学方法，能够对发射药 表面的残留硫进行脱除，从而大幅度降低发射药中硫元素的含量，有 效地抑制发射药在射击过程中的刺激性气味。The invention has the following beneficial effects: by using the physical and chemical method, the residual sulfur on the surface of the propellant can be removed, thereby greatly reducing the content of sulfur in the propellant, and effectively suppressing the irritating odor of the propellant during firing .
附图说明Description of drawings
图1是本发明实施例1-实施例6中的流程图；Fig. 1 is the flow chart in Embodiment 1-Embodiment 6 of the present invention;
图2是本发明实施例1、实施例2、实施例3和实施例4的硫元 素含量检测结果比较分析柱状图。Figure 2 is a bar chart of comparative analysis of the detection results of sulfur element content in Example 1, Example 2, Example 3 and Example 4 of the present invention.
具体实施方式Detailed ways
以下结合附图1-2对本发明作进一步详细说明。The present invention will be further described in detail below in conjunction with accompanying drawings 1-2.
实施例1：一种发射药表面残留硫脱除方法，如图1和图2所示， 具体包括以下步骤：Embodiment 1: A method for removing residual sulfur on the surface of propellant, as shown in Figure 1 and Figure 2, specifically including the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为50℃，超声清洗的时间设 置为60min，得到脱除表面残留的水溶性硫化物的某发射药样品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, Put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, set the ultrasonic cleaning temperature of the ultrasonic cleaning machine to 50 °C, and set the ultrasonic cleaning time to 60 min to obtain a certain propellant sample that removes the water-soluble sulfide remaining on the surface;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml过氧化氢溶液加入带有搅拌装置的三 口烧瓶内，并进行搅拌反应，搅拌反应的温度为室温(一般定义为 25℃)，搅拌反应的时间为360min，然后将搅拌反应完成后的某发射 药样品洗涤过滤，脱除某发射药样品表面残余的硫单质，然后将脱除 表面残余的硫单质的某发射药样品置于60℃水浴烘箱内干燥2d(2 天)，得到脱除表面残留硫的某发射药样品；2) Removing elemental sulfur, adding a certain propellant sample obtained in step 1) to remove water-soluble sulfide remaining on the surface and 500 ml of hydrogen peroxide solution into a three-necked flask with a stirring device, and carrying out a stirring reaction, stirring The reaction temperature is room temperature (generally defined as 25°C), and the stirring reaction time is 360 min. Then, a certain propellant sample after the stirring reaction is washed and filtered to remove the residual sulfur element on the surface of a certain propellant sample, and then remove the A propellant sample with residual sulfur element on the surface was dried in a 60°C water bath oven for 2 days (2 days) to obtain a propellant sample with residual sulfur removed on the surface;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
通过步骤3)的硫元素含量检测的分析结果表明，未脱硫前，该 发射药中硫含量为0.33wt％；步骤1)处理后，硫元素的含量为 0.05wt％，步骤2)处理后，硫元素含量为0.02wt％，硫元素含量大幅 度降低。The analysis result of the sulfur element content detection in step 3) shows that before desulfurization, the sulfur content in the propellant is 0.33wt%; after step 1) treatment, the sulfur element content is 0.05wt%, after step 2) treatment, The content of sulfur element is 0.02wt%, and the content of sulfur element is greatly reduced.
采用某弹道枪对表面残留硫脱除的发射药进行射击实验，结果表 明，未脱硫前，该发射药射击后有明显刺激性气味；脱硫后，该发射 药无明显刺激性气味，射击环境大幅度改善。A ballistic gun was used to shoot the propellant with the residual sulfur removed from the surface. The results showed that before desulfurization, the propellant had obvious irritating odor after firing; after desulfurization, the propellant had no obvious irritating odor, and the shooting environment was large. magnitude improvement.
实施例2：一种发射药表面残留硫脱除方法，如图1和图2所示， 具体包括以下步骤：Embodiment 2: A method for removing residual sulfur on the surface of propellant, as shown in Figure 1 and Figure 2, specifically including the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为80℃，超声清洗的时间设 置为20min，得到脱除表面残留的水溶性硫化物的某发射药样品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, Put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, set the ultrasonic cleaning temperature of the ultrasonic cleaning machine to 80°C, and set the ultrasonic cleaning time to 20 min, to obtain a certain propellant sample for removing the water-soluble sulfide remaining on the surface;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml过氧化氢溶液加入带有搅拌装置的三 口烧瓶内，并进行搅拌反应，搅拌反应的温度为40℃，搅拌反应的 时间为240min，然后将搅拌反应完成后的某发射药样品洗涤过滤， 脱除某发射药样品表面残余的硫单质，然后将脱除表面残余的硫单质 的某发射药样品置于60℃水浴烘箱内干燥2d(2天)，得到脱除表面 残留硫的某发射药样品；2) Removing elemental sulfur, adding a certain propellant sample obtained in step 1) to remove water-soluble sulfide remaining on the surface and 500 ml of hydrogen peroxide solution into a three-necked flask with a stirring device, and carrying out a stirring reaction, stirring The reaction temperature was 40 °C, and the stirring reaction time was 240 min. Then, after the stirring reaction was completed, a certain propellant sample was washed and filtered to remove the residual sulfur element on the surface of a certain propellant sample, and then the residual sulfur element on the surface was removed. A propellant sample was dried in a 60°C water bath oven for 2 days (2 days) to obtain a propellant sample with residual sulfur removed on the surface;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
通过步骤3)的硫元素含量检测的分析结果表明，未脱硫前，该 发射药中硫含量为0.33wt％；步骤1)处理后，硫元素含量为0.05wt％， 步骤2)处理后，硫元素含量为0.01wt％，硫元素含量大幅度降低。The analysis results of the sulfur element content detection in step 3) show that before desulfurization, the sulfur content in the propellant is 0.33wt%; after step 1) treatment, the sulfur element content is 0.05wt%, after step 2) treatment, the sulfur content The element content is 0.01wt%, and the sulfur element content is greatly reduced.
采用某弹道枪对表面残留硫脱除的发射药进行射击实验，结果表 明，未脱硫前，该发射药射击后有明显刺激性气味；脱硫后，该发射 药无明显刺激性气味，射击环境大幅度改善。A ballistic gun was used to shoot the propellant with the residual sulfur removed from the surface. The results showed that before desulfurization, the propellant had obvious irritating odor after firing; after desulfurization, the propellant had no obvious irritating odor, and the shooting environment was large. magnitude improvement.
实施例3：一种发射药表面残留硫脱除方法，如图1和图2所示， 具体包括以下步骤：Embodiment 3: A method for removing residual sulfur on the surface of propellant, as shown in Figure 1 and Figure 2, specifically including the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为100℃，超声清洗的时间设 置为5min，得到脱除表面残留的水溶性硫化物的某发射药样品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, Put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, set the ultrasonic cleaning temperature of the ultrasonic cleaning machine to 100 °C, and set the ultrasonic cleaning time to 5 min to obtain a certain propellant sample that removes the water-soluble sulfide remaining on the surface;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml过氧化氢溶液加入带有搅拌装置的三 口烧瓶内，并进行搅拌反应，搅拌反应的温度为40℃，搅拌反应的 时间为360min，然后将搅拌反应完成后的某发射药样品洗涤过滤， 脱除某发射药样品表面残余的硫单质，然后将脱除表面残余的硫单质 的某发射药样品置于60℃水浴烘箱内干燥2d(2天)，得到脱除表面 残留硫的某发射药样品；2) Removing elemental sulfur, adding a certain propellant sample obtained in step 1) to remove water-soluble sulfide remaining on the surface and 500 ml of hydrogen peroxide solution into a three-necked flask with a stirring device, and carrying out a stirring reaction, stirring The reaction temperature is 40 °C, and the stirring reaction time is 360 min. Then, a certain propellant sample after the stirring reaction is washed and filtered to remove the residual sulfur element on the surface of a certain propellant sample, and then the residual sulfur element on the surface will be removed. A propellant sample was dried in a 60°C water bath oven for 2 days (2 days) to obtain a propellant sample with residual sulfur removed on the surface;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
通过步骤3)的硫元素含量检测的分析结果表明，未脱硫前，该 发射药中硫含量为0.33wt％；步骤1)处理后，硫元素含量为0.05wt％， 步骤2)处理后，硫元素含量为0.02wt％，硫元素含量大幅度降低。The analysis results of the sulfur element content detection in step 3) show that before desulfurization, the sulfur content in the propellant is 0.33wt%; after step 1) treatment, the sulfur element content is 0.05wt%, after step 2) treatment, the sulfur content The element content is 0.02wt%, and the sulfur element content is greatly reduced.
采用某弹道枪对表面残留硫脱除的发射药进行射击实验，结果表 明，未脱硫前，该发射药射击后有明显刺激性气味；脱硫后，该发射 药无明显刺激性气味，射击环境大幅度改善。A ballistic gun was used to shoot the propellant with the residual sulfur removed from the surface. The results showed that before desulfurization, the propellant had obvious irritating odor after firing; after desulfurization, the propellant had no obvious irritating odor, and the shooting environment was large. magnitude improvement.
实施例4：一种发射药表面残留硫脱除方法，如图1和图2所示， 具体包括以下步骤：Embodiment 4: A method for removing residual sulfur on the surface of propellant, as shown in Figure 1 and Figure 2, specifically including the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为90℃，超声清洗的时间设 置为40min，得到脱除表面残留的水溶性硫化物的某发射药样品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, Put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, set the ultrasonic cleaning temperature of the ultrasonic cleaning machine to 90°C, and set the ultrasonic cleaning time to 40 min to obtain a certain propellant sample that removes the water-soluble sulfide remaining on the surface;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml过氧化氢溶液加入带有搅拌装置的三 口烧瓶内，并进行搅拌反应，搅拌反应的温度为50℃，搅拌反应的 时间为360min，然后将搅拌反应完成后的某发射药样品洗涤过滤， 脱除某发射药样品表面残余的硫单质，然后将脱除表面残余的硫单质 的某发射药样品置于60℃水浴烘箱内干燥2d(2天)，得到脱除表面 残留硫的某发射药样品；2) Removing elemental sulfur, adding a certain propellant sample obtained in step 1) to remove water-soluble sulfide remaining on the surface and 500 ml of hydrogen peroxide solution into a three-necked flask with a stirring device, and carrying out a stirring reaction, stirring The reaction temperature was 50 °C, and the stirring reaction time was 360 min. Then, a certain propellant sample after the stirring reaction was washed and filtered to remove the residual sulfur element on the surface of a certain propellant sample, and then the residual sulfur element on the surface was removed. A propellant sample was dried in a 60°C water bath oven for 2 days (2 days) to obtain a propellant sample with residual sulfur removed on the surface;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
通过步骤3)的硫元素含量检测的分析结果表明，未脱硫前，该 发射药中硫含量为0.33wt％；步骤1)处理后，硫元素含量为0.05wt％， 步骤2)处理后，硫元素含量为0.01wt％，硫元素含量大幅度降低。The analysis results of the sulfur element content detection in step 3) show that before desulfurization, the sulfur content in the propellant is 0.33wt%; after step 1) treatment, the sulfur element content is 0.05wt%, after step 2) treatment, the sulfur content The element content is 0.01wt%, and the sulfur element content is greatly reduced.
采用某弹道枪对表面残留硫脱除的发射药进行射击实验，结果表 明，未脱硫前，该发射药射击后有明显刺激性气味；脱硫后，该发射 药无明显刺激性气味，射击环境大幅度改善。A ballistic gun was used to shoot the propellant with the residual sulfur removed from the surface. The results showed that before desulfurization, the propellant had obvious irritating odor after firing; after desulfurization, the propellant had no obvious irritating odor, and the shooting environment was large. magnitude improvement.
实施例5：一种发射药表面残留硫脱除方法，如图1和图2所示， 具体包括以下步骤：Embodiment 5: A method for removing residual sulfur on the surface of propellant, as shown in Figure 1 and Figure 2, which specifically includes the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为90℃，超声清洗的时间设 置为30min，得到脱除表面残留的水溶性硫化物的某发射药样品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, Put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, set the ultrasonic cleaning temperature of the ultrasonic cleaning machine to 90°C, and set the ultrasonic cleaning time to 30 min to obtain a certain propellant sample for removing the water-soluble sulfide remaining on the surface;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml浓度为0.1～5wt％的氢氧化钠溶液加入 带有搅拌装置的三口烧瓶内，并进行搅拌反应，搅拌反应的温度为室 温-50℃，搅拌反应的时间为5-60min，然后将搅拌反应完成后的某 发射药样品洗涤过滤，脱除某发射药样品表面残余的硫单质，然后将 脱除表面残余的硫单质的某发射药样品置于60℃水浴烘箱内干燥2d (2天)，得到脱除表面残留硫的某发射药样品；2) To remove elemental sulfur, add a certain propellant sample obtained in step 1) from the water-soluble sulfide remaining on the surface and 500 ml of sodium hydroxide solution with a concentration of 0.1 to 5 wt% into a three-necked flask with a stirring device. , and carry out stirring reaction, the temperature of stirring reaction is room temperature -50 ℃, the time of stirring reaction is 5-60min, and then a certain propellant sample after the stirring reaction is washed and filtered to remove the residual sulfur element on the surface of a certain propellant sample , and then place a propellant sample with the residual sulfur element removed on the surface to dry in a 60°C water bath oven for 2 days (2 days) to obtain a propellant sample with the residual sulfur removed on the surface;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
通过步骤3)的硫元素含量检测的分析结果表明，未脱硫前，该 发射药中硫含量为0.33wt％；步骤1)处理后，硫元素含量为0.05wt％， 步骤2)处理后，硫元素含量小于0.02wt％，硫元素含量大幅度降低。The analysis results of the sulfur element content detection in step 3) show that before desulfurization, the sulfur content in the propellant is 0.33wt%; after step 1) treatment, the sulfur element content is 0.05wt%, after step 2) treatment, the sulfur content When the element content is less than 0.02wt%, the sulfur element content is greatly reduced.
采用某弹道枪对表面残留硫脱除的发射药进行射击实验，结果表 明，未脱硫前，该发射药射击后有明显刺激性气味；脱硫后，该发射 药无明显刺激性气味，射击环境大幅度改善。A ballistic gun was used to shoot the propellant with the residual sulfur removed from the surface. The results showed that before desulfurization, the propellant had obvious irritating odor after firing; after desulfurization, the propellant had no obvious irritating odor, and the shooting environment was large. magnitude improvement.
实施例6：一种发射药表面残留硫脱除方法，如图1和图2所示， 具体包括以下步骤：Embodiment 6: a method for removing residual sulfur on the surface of propellant, as shown in Figure 1 and Figure 2, specifically including the following steps:
1)脱除水溶性硫化物，称取100g表面残留硫的某发射药样品， 量取500ml水，然后将称取的某发射药样品和量取的水加入带有搅拌 装置的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清 洗，设置超声波清洗机的超声清洗温度为90℃，超声清洗的时间设 置为30min，得到脱除表面残留的水溶性硫化物的某发射药样品；1) Remove water-soluble sulfide, weigh 100g of a propellant sample with residual sulfur on the surface, measure 500ml of water, and then add the weighed sample of a propellant and the measured water into a three-necked flask with a stirring device, Put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, set the ultrasonic cleaning temperature of the ultrasonic cleaning machine to 90°C, and set the ultrasonic cleaning time to 30 min to obtain a certain propellant sample for removing the water-soluble sulfide remaining on the surface;
2)脱除单质硫，将步骤1)中得到的脱除表面残留的水溶性硫 化物的某发射药样品和500ml浓度为0.1～15wt％的稀硝酸溶液加入带 有搅拌装置的三口烧瓶内，并进行搅拌反应，搅拌反应的温度为 40-80℃，搅拌反应的时间为5-60min，然后将搅拌反应完成后的某 发射药样品洗涤过滤，脱除某发射药样品表面残余的硫单质，然后将 脱除表面残余的硫单质的某发射药样品置于60℃水浴烘箱内干燥2d (2天)，得到脱除表面残留硫的某发射药样品；2) removing elemental sulfur, adding a certain propellant sample obtained in step 1) for removing water-soluble sulfide remaining on the surface and 500 ml of dilute nitric acid solution with a concentration of 0.1 to 15wt% into a three-necked flask with a stirring device, And carry out stirring reaction, the temperature of stirring reaction is 40-80 ℃, the time of stirring reaction is 5-60min, and then a certain propellant sample after the stirring reaction is washed and filtered to remove the residual sulfur element on the surface of a certain propellant sample, Then, a certain propellant sample with the residual sulfur element removed on the surface was dried in a 60°C water bath oven for 2 days (2 days) to obtain a certain propellant sample with the surface residual sulfur removed;
3)硫元素含量检测，采用元素分析仪分别对未脱硫某发射药样 品、经过步骤1)处理后的某发射药样品和经过步骤2)处理后的某 发射药样品进行硫元素含量分析。3) Detection of sulfur element content, elemental analyzer is used to analyze the sulfur element content of a certain propellant sample without desulfurization, a certain propellant sample after processing in step 1), and a certain propellant sample after processing in step 2).
通过步骤3)的硫元素含量检测的分析结果表明，未脱硫前，该 发射药中硫含量为0.33wt％；步骤1)处理后，硫元素含量为0.05％， 步骤2)处理后，硫元素含量小于0.02wt％，硫元素含量大幅度降低。The analysis results of the sulfur content detection in step 3) show that before desulfurization, the sulfur content in the propellant is 0.33wt%; after the treatment in step 1), the sulfur content is 0.05%; after the treatment in step 2), the sulfur content is 0.05%. If the content is less than 0.02wt%, the content of sulfur element is greatly reduced.
采用某弹道枪对表面残留硫脱除的发射药进行射击实验，结果表 明，未脱硫前，该发射药射击后有明显刺激性气味；脱硫后，该发射 药无明显刺激性气味，射击环境大幅度改善。A ballistic gun was used to shoot the propellant with the residual sulfur removed from the surface. The results showed that before desulfurization, the propellant had obvious irritating odor after firing; after desulfurization, the propellant had no obvious irritating odor, and the shooting environment was large. magnitude improvement.
以下将实施例1至实施例4的实验条件及实验结果汇总于表1中 对本发明进行进一步说明。The experimental conditions and experimental results of Examples 1 to 4 are summarized in Table 1 below to further illustrate the present invention.
表1表面残留硫发射药脱除实验条件及结果Table 1 The experimental conditions and results of the removal of residual sulfur propellant on the surface
工作原理：通过步骤1)将某发射药样品和水加入带有搅拌装置 的三口烧瓶内，并将三口烧瓶放入超声波清洗机中进行超声清洗，从 而实现利用物理方法将某发射药样品表面残留的水溶性硫化物脱除； 通过步骤2)中将步骤1)中脱除表面残留的水溶性硫化物的某发射 药样品和500ml反应试剂溶液加入带有搅拌装置的三口烧瓶内进行 搅拌反应，并控制搅拌反应的温度和时间，然后将搅拌反应完成后的 某发射药样品洗涤过滤，便于利用化学方法脱除某发射药样品表面残 余的硫单质，然后将脱除表面残余的硫单质的某发射药样品置于60℃ 水浴烘箱内干燥2天，从而实现对某发射药样品表面残留硫的脱除， 从而实现大幅度降低发射药中硫元素的含量，有效地抑制发射药在射 击过程中的刺激性气味。Working principle: Through step 1), add a propellant sample and water into a three-necked flask with a stirring device, and put the three-necked flask into an ultrasonic cleaning machine for ultrasonic cleaning, so as to realize the use of physical methods to remove residues on the surface of a propellant sample. Removal of water-soluble sulfide; by adding a certain propellant sample and 500ml reaction reagent solution of removing the water-soluble sulfide remaining on the surface in step 1) in step 2) into a three-necked flask with a stirring device to carry out stirring reaction, And control the temperature and time of the stirring reaction, and then wash and filter a certain propellant sample after the stirring reaction is completed, so as to use chemical methods to remove the residual sulfur element on the surface of the propellant sample, and then remove the residual sulfur element on the surface. The propellant sample was dried in a 60°C water bath oven for 2 days, so as to remove the residual sulfur on the surface of a certain propellant sample, thereby greatly reducing the content of sulfur in the propellant and effectively inhibiting the propellant during the firing process. pungent odor.
本具体实施例仅仅是对本发明的解释，其并不是对本发明的限 制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做 出没有创造性贡献的修改，但只要在本发明的权利要求范围内都受到 专利法的保护。This specific embodiment is only an explanation of the present invention, and it does not limit the present invention. Those skilled in the art can make modifications without creative contribution to the present embodiment as required after reading this specification, but as long as the rights of the present invention are used All claims are protected by patent law.
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