CN110790618B - Method for removing residual sulfur on surface of propellant powder - Google Patents
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Abstract
The invention discloses a method for removing residual sulfur on the surface of propellant powder, which relates to the technical field of propellant powder and has the technical scheme key points that: the method specifically comprises the following steps: step 1): ultrasonic cleaning is carried out on the sulfur-containing propellant powder on a certain surface by adopting an ultrasonic cleaning machine, and water-soluble sulfide remained on the surface of the propellant powder is removed; step 2): removing residual elemental sulfur on the surface of the propellant, adding the propellant with the surface residual water-soluble sulfide removed in the step 1) and 500ml of reaction reagent solution into a three-neck flask with a stirring device to carry out stirring reaction, and controlling the temperature and time of the stirring reaction; step 3): and (3) carrying out sulfur content detection on the propellant powder treated in the step 1) and the step 2). The technical scheme can realize the removal of residual sulfur on the surface of the propellant by using a simple physical and chemical method, thereby greatly reducing the content of sulfur element in the propellant and effectively inhibiting the pungent smell generated in the process of shooting the propellant.
Description
Technical Field
The invention relates to the technical field of propellant powder, in particular to a method for removing residual sulfur on the surface of the propellant powder.
Background
The propellant powder is an indispensable energy substance for realizing the launching of a barrel weapon, and the composition of the propellant powder is one of important factors for determining the performance of the propellant powder. The process of barrel weapon launching, in addition to performing the basic functions of the weapon, will also have a number of negative effects on the environment in which the weapon is used. These effects are the result of physicochemical effects in the ballistic process of weapons, particularly in the harmful phenomena of fire smoke, residues in the chamber, muzzle pressure waves, fire noise and vibration, and toxic and harmful gases.
The realization of the high gradual increase of energy release from slow to fast becomes a core and key technology for determining the performance of weapons, and is also the forward development direction of the international military field. In order to obtain a high gradual increase of energy release of the propellant, the inventor has applied for a national defense patent, and the prepared propellant has high gradual increase of energy release. However, in the preparation process, sulfur element remains on the surface of the propellant powder, and the presence of the sulfur element enables the propellant powder to generate irritant toxic and harmful gases such as sulfur dioxide and the like in the combustion process, so that air pollution is easily caused. Meanwhile, the pungent odor of sulfur dioxide and the like causes severe physiological and psychological stress reactions of fighters during shooting, thereby causing the reduction of health level and fighting effectiveness. The existence of sulfur element in the propellant undoubtedly aggravates the negative effect on the battle environment, and inhibits the development of the propellant.
At present, in the prior art, no method for removing sulfur in the surface residual sulfur gunpowder exists, so that the desulfurization treatment is carried out on the high-gradual-increase propellant with sulfur on the surface in the field of propellant, the performance of the propellant is further improved, and an excellent combat environment is provided for combat personnel, which is an important problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a method for removing residual sulfur on the surface of propellant powder, which utilizes a physical and chemical method to remove the residual sulfur on the surface of the propellant powder, thereby greatly reducing the content of sulfur element in the propellant powder and effectively inhibiting the pungent smell of the propellant powder in the shooting process.
The technical purpose of the invention is realized by the following technical scheme: a method for removing residual sulfur on the surface of propellant powder specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 50-100 ℃, and setting the ultrasonic cleaning time to be 5-60min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant powder sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of reaction reagent solution into a three-neck flask with a stirring device, stirring for reaction, controlling the temperature and time of the stirring reaction, washing and filtering the certain propellant powder sample after the stirring reaction is finished, removing the surface residual sulfur elemental substance of the certain propellant powder sample, and then placing the certain propellant powder sample with the surface residual sulfur elemental substance removed in a water bath oven at 60 ℃ for drying for 2d (2 days) to obtain the certain propellant powder sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The invention is further configured to: the temperature for stirring reaction in the step 2) is room temperature to 80 ℃, and the stirring reaction time is 5 to 360 min.
The invention is further configured to: the reaction reagent solution in the step 2) is one of a hydrogen peroxide solution, a sodium hydroxide solution with the concentration of 0.1-5 wt% and a dilute nitric acid solution with the concentration of 0.1-15 wt%.
The invention has the following beneficial effects: the residual sulfur on the surface of the propellant powder can be removed by utilizing a physical and chemical method, so that the content of sulfur element in the propellant powder is greatly reduced, and the pungent smell of the propellant powder in the shooting process is effectively inhibited.
Drawings
FIG. 1 is a flow chart in examples 1 to 6 of the present invention;
FIG. 2 is a histogram comparing and analyzing the results of measuring the sulfur content in examples 1, 2, 3 and 4 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to FIGS. 1-2.
Example 1: a method for removing residual sulfur on the surface of propellant powder is shown in figures 1 and 2, and specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 50 ℃, and setting the ultrasonic cleaning time to be 60min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant powder sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of hydrogen peroxide solution into a three-neck flask with a stirring device, stirring and reacting, wherein the stirring and reacting temperature is room temperature (generally defined as 25 ℃), and the stirring and reacting time is 360min, then washing and filtering a certain propellant powder sample after the stirring and reacting are completed, removing the surface residual sulfur from the certain propellant powder sample, and then placing the certain propellant powder sample with the surface residual sulfur removed in a water bath oven at 60 ℃ for drying for 2d (2 days) to obtain a certain propellant powder sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The analysis result of the sulfur content detection in the step 3) shows that the sulfur content in the propellant is 0.33 wt% before desulfurization; after the treatment of the step 1), the content of the sulfur element is 0.05 wt%, and after the treatment of the step 2), the content of the sulfur element is 0.02 wt%, and the content of the sulfur element is greatly reduced.
The result of a shooting experiment of the propellant powder with the residual sulfur removed on the surface by adopting a certain ballistic gun shows that the propellant powder has obvious pungent smell after shooting before desulfurization; after desulfurization, the propellant has no obvious pungent smell and greatly improved shooting environment.
Example 2: a method for removing residual sulfur on the surface of propellant powder is shown in figures 1 and 2, and specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 80 ℃, and setting the ultrasonic cleaning time to be 20min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant powder sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of hydrogen peroxide solution into a three-neck flask with a stirring device, stirring and reacting at the temperature of 40 ℃, wherein the stirring and reacting time is 240min, washing and filtering the certain propellant powder sample after the stirring and reacting are finished, removing the surface residual sulfur elemental sulfur of the certain propellant powder sample, and then placing the certain propellant powder sample with the surface residual sulfur elemental sulfur removed in a water bath oven at 60 ℃ for drying for 2d (2 days) to obtain the certain propellant powder sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The analysis result of the sulfur content detection in the step 3) shows that the sulfur content in the propellant is 0.33 wt% before desulfurization; after the treatment of the step 1), the content of the sulfur element is 0.05 wt%, and after the treatment of the step 2), the content of the sulfur element is 0.01 wt%, and the content of the sulfur element is greatly reduced.
The result of a shooting experiment of the propellant powder with the residual sulfur removed on the surface by adopting a certain ballistic gun shows that the propellant powder has obvious pungent smell after shooting before desulfurization; after desulfurization, the propellant has no obvious pungent smell and greatly improved shooting environment.
Example 3: a method for removing residual sulfur on the surface of propellant powder is shown in figures 1 and 2, and specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 100 ℃, and setting the ultrasonic cleaning time to be 5min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant powder sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of hydrogen peroxide solution into a three-neck flask with a stirring device, stirring and reacting at the temperature of 40 ℃, wherein the stirring and reacting time is 360min, washing and filtering the certain propellant powder sample after the stirring and reacting are finished, removing the surface residual sulfur elemental sulfur of the certain propellant powder sample, and then placing the certain propellant powder sample with the surface residual sulfur elemental sulfur removed in a water bath oven at 60 ℃ for drying for 2d (2 days) to obtain the certain propellant powder sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The analysis result of the sulfur content detection in the step 3) shows that the sulfur content in the propellant is 0.33 wt% before desulfurization; after the treatment of the step 1), the content of the sulfur element is 0.05 wt%, and after the treatment of the step 2), the content of the sulfur element is 0.02 wt%, and the content of the sulfur element is greatly reduced.
The result of a shooting experiment of the propellant powder with the residual sulfur removed on the surface by adopting a certain ballistic gun shows that the propellant powder has obvious pungent smell after shooting before desulfurization; after desulfurization, the propellant has no obvious pungent smell and greatly improved shooting environment.
Example 4: a method for removing residual sulfur on the surface of propellant powder is shown in figures 1 and 2, and specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 90 ℃, and setting the ultrasonic cleaning time to be 40min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant powder sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of hydrogen peroxide solution into a three-neck flask with a stirring device, stirring and reacting at the temperature of 50 ℃, wherein the stirring and reacting time is 360min, washing and filtering the certain propellant powder sample after the stirring and reacting are finished, removing the surface residual sulfur elemental sulfur of the certain propellant powder sample, and then placing the certain propellant powder sample with the surface residual sulfur elemental sulfur removed in a water bath oven at 60 ℃ for drying for 2d (2 days) to obtain the certain propellant powder sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The analysis result of the sulfur content detection in the step 3) shows that the sulfur content in the propellant is 0.33 wt% before desulfurization; after the treatment of the step 1), the content of the sulfur element is 0.05 wt%, and after the treatment of the step 2), the content of the sulfur element is 0.01 wt%, and the content of the sulfur element is greatly reduced.
The result of a shooting experiment of the propellant powder with the residual sulfur removed on the surface by adopting a certain ballistic gun shows that the propellant powder has obvious pungent smell after shooting before desulfurization; after desulfurization, the propellant has no obvious pungent smell and greatly improved shooting environment.
Example 5: a method for removing residual sulfur on the surface of propellant powder is shown in figures 1 and 2, and specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 90 ℃, and setting the ultrasonic cleaning time to be 30min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of 0.1-5 wt% sodium hydroxide solution into a three-neck flask with a stirring device, stirring for reaction, wherein the stirring reaction temperature is between room temperature and 50 ℃, and the stirring reaction time is 5-60min, then washing and filtering the certain propellant sample after the stirring reaction is finished, removing the residual elemental sulfur on the surface of the certain propellant sample, and then drying the certain propellant sample with the surface residual elemental sulfur removed in a water bath oven at 60 ℃ for 2d (2 days) to obtain the certain propellant sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The analysis result of the sulfur content detection in the step 3) shows that the sulfur content in the propellant is 0.33 wt% before desulfurization; after the treatment of the step 1), the content of the sulfur element is 0.05 wt%, and after the treatment of the step 2), the content of the sulfur element is less than 0.02 wt%, and the content of the sulfur element is greatly reduced.
The result of a shooting experiment of the propellant powder with the residual sulfur removed on the surface by adopting a certain ballistic gun shows that the propellant powder has obvious pungent smell after shooting before desulfurization; after desulfurization, the propellant has no obvious pungent smell and greatly improved shooting environment.
Example 6: a method for removing residual sulfur on the surface of propellant powder is shown in figures 1 and 2, and specifically comprises the following steps:
1) removing water-soluble sulfide, weighing a certain propellant powder sample with 100g of surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 90 ℃, and setting the ultrasonic cleaning time to be 30min, so as to obtain the certain propellant powder sample with the surface residual sulfur removed;
2) removing elemental sulfur, namely adding a certain propellant sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of 0.1-15 wt% dilute nitric acid solution into a three-neck flask with a stirring device, stirring for reaction, wherein the stirring reaction temperature is 40-80 ℃, and the stirring reaction time is 5-60min, then washing and filtering the certain propellant sample after the stirring reaction is finished, removing the residual elemental sulfur on the surface of the certain propellant sample, and then drying the certain propellant sample with the surface residual elemental sulfur removed in a 60 ℃ water bath oven for 2d (2 days) to obtain the certain propellant sample with the surface residual sulfur removed;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on a certain propellant powder sample which is not desulfurized, a certain propellant powder sample which is treated in the step 1) and a certain propellant powder sample which is treated in the step 2) by using an element analyzer.
The analysis result of the sulfur content detection in the step 3) shows that the sulfur content in the propellant is 0.33 wt% before desulfurization; after the treatment of the step 1), the content of the sulfur element is 0.05 percent, and after the treatment of the step 2), the content of the sulfur element is less than 0.02 weight percent, and the content of the sulfur element is greatly reduced.
The result of a shooting experiment of the propellant powder with the residual sulfur removed on the surface by adopting a certain ballistic gun shows that the propellant powder has obvious pungent smell after shooting before desulfurization; after desulfurization, the propellant has no obvious pungent smell and greatly improved shooting environment.
The experimental conditions and the experimental results of examples 1 to 4 are summarized in table 1 below to further illustrate the present invention.
TABLE 1 conditions and results of the test for removing residual sulfur-emitting agent from the surface
The working principle is as follows: adding a propellant powder sample and water into a three-neck flask with a stirring device in the step 1), and putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, thereby removing residual water-soluble sulfide on the surface of the propellant powder sample by using a physical method; adding a certain propellant sample with the surface residual water-soluble sulfide removed in the step 1) and 500ml of reaction reagent solution into a three-neck flask with a stirring device in the step 2) to carry out stirring reaction, controlling the temperature and time of the stirring reaction, washing and filtering the certain propellant sample after the stirring reaction is finished, conveniently removing the residual sulfur simple substance on the surface of the certain propellant sample by using a chemical method, and then drying the certain propellant sample with the surface residual sulfur simple substance removed in a water bath oven at 60 ℃ for 2 days, thereby realizing the removal of the residual sulfur on the surface of the certain propellant sample, greatly reducing the content of the sulfur element in the propellant, and effectively inhibiting the pungent smell of the propellant in the shooting process.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (2)
1. A method for removing residual sulfur on the surface of propellant powder is characterized by comprising the following steps: the method specifically comprises the following steps:
1) removing water-soluble sulfide, weighing 100g of propellant powder sample with surface residual sulfur, weighing 500ml of water, adding the weighed propellant powder sample and the weighed water into a three-neck flask with a stirring device, putting the three-neck flask into an ultrasonic cleaning machine for ultrasonic cleaning, setting the ultrasonic cleaning temperature of the ultrasonic cleaning machine to be 50-100 ℃, and setting the ultrasonic cleaning time to be 5-60min, so as to obtain the propellant powder sample with surface residual sulfur removed;
2) removing elemental sulfur, namely adding the propellant powder sample with the surface residual water-soluble sulfide removed obtained in the step 1) and 500ml of reaction reagent solution into a three-neck flask with a stirring device, stirring for reaction, controlling the temperature and time of the stirring reaction, washing and filtering the propellant powder sample after the stirring reaction is finished, removing the surface residual sulfur elemental sulfur of the propellant powder sample, and then placing the propellant powder sample with the surface residual sulfur removed in a 60 ℃ water bath drying oven for drying for 2d to obtain the propellant powder sample with the surface residual sulfur removed; wherein the reaction reagent solution is one of a hydrogen peroxide solution, a sodium hydroxide solution with the concentration of 0.1-5 wt% and a dilute nitric acid solution with the concentration of 0.1-15 wt%;
3) and (3) detecting the content of sulfur element, namely, respectively analyzing the content of sulfur element on the non-desulfurized propellant powder sample, the propellant powder sample treated in the step 1) and the propellant powder sample treated in the step 2) by using an element analyzer.
2. The method for removing residual sulfur from the surface of propellant powder as claimed in claim 1, wherein: the temperature for stirring reaction in the step 2) is room temperature to 80 ℃, and the stirring reaction time is 5 to 360 min.
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| CN109096215A (en) * | 2018-10-12 | 2018-12-28 | 中国工程物理研究院化工材料研究所 | Rich nitrogen energetic material 3- amino -3 '-nitramino -5,5 '-connection -1,2,4- triazole and preparation method thereof |
| CN109678630A (en) * | 2019-01-10 | 2019-04-26 | 重庆大学 | The preparation method of Al/NiO sheet thermite |
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| US6080906A (en) * | 1997-09-18 | 2000-06-27 | Alliedsignal, Inc. | Demilitarization of chemical munitions |
| WO2000015306A1 (en) * | 1998-09-14 | 2000-03-23 | Alliedsignal Inc. | Demilitarization of chemical munitions |
| US6338794B1 (en) * | 1999-11-01 | 2002-01-15 | Phillips Petroleum Company | Desulfurization with zinc titanate sorbents |
| CN105510327B (en) * | 2016-01-07 | 2018-06-29 | 河北工程大学 | The remaining identification method of Chinese medicine sulphur |
| CN109764762B (en) * | 2019-03-07 | 2021-05-28 | 浏阳东顺花炮新材料技术开发有限公司 | Continuous production system of tobacco peanut powder |
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| CN109096215A (en) * | 2018-10-12 | 2018-12-28 | 中国工程物理研究院化工材料研究所 | Rich nitrogen energetic material 3- amino -3 '-nitramino -5,5 '-connection -1,2,4- triazole and preparation method thereof |
| CN109678630A (en) * | 2019-01-10 | 2019-04-26 | 重庆大学 | The preparation method of Al/NiO sheet thermite |
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