CN111116278B - Method for flow type ultrasonic treatment of intercrystalline acid of elemental explosive - Google Patents
Method for flow type ultrasonic treatment of intercrystalline acid of elemental explosive Download PDFInfo
- Publication number
- CN111116278B CN111116278B CN201911316032.1A CN201911316032A CN111116278B CN 111116278 B CN111116278 B CN 111116278B CN 201911316032 A CN201911316032 A CN 201911316032A CN 111116278 B CN111116278 B CN 111116278B
- Authority
- CN
- China
- Prior art keywords
- ultrasonic
- washer
- explosive
- acid
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- 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
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/32—Compositions containing a nitrated organic compound the compound being nitrated pentaerythritol
-
- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/34—Compositions containing a nitrated organic compound the compound being a nitrated acyclic, alicyclic or heterocyclic amine
Abstract
The invention provides a method for treating intercrystalline acid of an elemental explosive by flowing ultrasonic, which comprises the steps of taking a crude product of the elemental explosive containing acid, mixing the crude product with water to form a mixed material; controlling the temperature in the washer to be kept at 25-45 ℃; the mixed material enters from the lower end of the washer, flows out from the upper end, and is subjected to ultrasonic treatment after circulating for a certain time; in the ultrasonic process, controlling the temperature in the washer to be not more than 50 ℃, and stopping ultrasonic when the pH value in the washer is stable after circularly washing for a certain time; and filtering and leaching the washed single-substance explosive product, and drying to obtain the single-substance explosive product meeting the acidity requirement. The method has the advantages of cyclic use of the washing water, low energy consumption, high efficiency and easy realization of mass production, can improve the energy utilization rate of the ultrasonic action by the cyclic flow of the washing water, further reduces the consumption of water, and can realize large-scale application by the series connection of a plurality of ultrasonic washers.
Description
Technical Field
The invention belongs to the technical field of explosives and powders, and particularly relates to a method for treating intercrystalline acid of an elementary explosive by flowing ultrasonic waves, which is suitable for elementary explosives such as hexogen, octogen, taian and the like.
Background
In the process of manufacturing the single-substance explosive, nitric acid and sulfuric acid are often used as oxidants, and a certain amount of residual acid is usually attached to the surface and between crystals of the single-substance explosive obtained through the procedures of nitration, crystallization and the like, and the treatment of the residual acid is a difficult problem in the process of manufacturing the single-substance explosive. Taking the octogen as an example, the acidity of a crude product is about 9%, residual acid on the surface of a crystal can be removed through conventional washing, the acidity is reduced to about 1%, the residual acid is intercrystalline acid, the intercrystalline acid treatment difficulty is high, the current common process is high-temperature cooking and washing, the process mainly comprises the steps of mixing the octogen containing acid and water, then cooking and washing for at least 4 hours at 140-160 ℃, and cooling and washing to enable the acidity of the octogen product to meet the national military standard. The process has the defects of high energy consumption, large wastewater discharge amount, long washing time, large dosage and the like.
Patent application CN201310545070.0 discloses an ultrasonic acid-removing method, which can achieve a relatively efficient and energy-saving deacidification effect, but this method fails to solve the problem of large water consumption in the acid-removing process, and the action range of the ultrasonic is limited because the action of the ultrasonic is concentrated at the bottom of the ultrasonic rod, resulting in a low energy utilization rate. In addition, in the engineering application process, as the volume of the ultrasonic washing kettle is increased, the blind area of the ultrasonic action is larger and larger, and the process is limited in the application of actual industrial production.
Disclosure of Invention
Technical problem to be solved
The invention provides a method for treating intercrystalline acid of an elemental explosive by flowing ultrasonic, which aims to solve the technical problems of large water consumption, long washing time and difficulty in realizing mass production in the existing process for removing intercrystalline acid of an elemental explosive.
(II) technical scheme
In order to solve the technical problem, the invention provides a method for treating intercrystalline acid of an elemental explosive by flowing ultrasonic, which comprises the following steps:
s1, mixing the crude product of the acid-containing single-substance explosive with water to form a mixed material;
s2, controlling the temperature in the washer to be kept at 25-45 ℃;
s3, enabling the mixed material to enter from the lower end of the washer and flow out from the upper end, and performing ultrasonic treatment after circulating for a certain time;
s4, in the ultrasonic process, controlling the temperature in the washer to be not more than 50 ℃, and stopping ultrasonic when the pH value in the washer is stable after circularly washing for a certain time;
and S5, filtering and leaching the washed single-substance explosive product, and drying to obtain the single-substance explosive product meeting the acidity requirement.
Further, in step S1, the mixing ratio of the elementary explosive and the water is 1 (1-2).
Further, in step S3, the mixed material is circulated in the washer for 5-10 min and then is subjected to ultrasonic treatment.
Further, in step S3, the ultrasonic power is not more than 2.8kw, the adjustment range is 20% -100%, and the ultrasonic frequency is 15-45 kHz.
Further, in step S4, the circulation washing time is 15-45 min.
Further, in step S5, the mass ratio of the single rinsing water amount to the acid-containing elemental explosive is about 1: 10.
Further, the elementary explosive is octogen, hexogen or taian.
(III) advantageous effects
The invention provides a method for treating intercrystalline acid of an elemental explosive by flowing ultrasonic, which comprises the steps of taking a crude product of the elemental explosive containing acid, mixing the crude product with water to form a mixed material; controlling the temperature in the washer to be kept at 25-45 ℃; the mixed material enters from the lower end of the washer, flows out from the upper end, and is subjected to ultrasonic treatment after circulating for a certain time; in the ultrasonic process, controlling the temperature in the washer to be not more than 50 ℃, and stopping ultrasonic when the pH value in the washer is stable after circularly washing for a certain time; and filtering and leaching the washed single-substance explosive product, and drying to obtain the single-substance explosive product meeting the acidity requirement. The method has the advantages of cyclic use of the washing water, low energy consumption, high efficiency and easy realization of mass production, can improve the energy utilization rate of the ultrasonic action by the cyclic flow of the washing water, further reduces the consumption of water, and can realize large-scale application by the series connection of a plurality of ultrasonic washers.
The method for treating the intercrystalline acid of the single-substance explosive by the flowing ultrasonic has the following specific advantages: (1) the flow type ultrasonic work is adopted, the work area is concentrated, the energy utilization rate is high, and the washing time is shortened by at least 50% compared with the prior art; (2) the water consumption is greatly reduced by at least more than 30 percent compared with the prior art; (3) is suitable for industrial production and can realize the improvement of the treatment capacity on the premise of not reducing the ultrasonic washing efficiency by serially connecting the washers.
Drawings
FIG. 1 is a schematic diagram of an overall apparatus used in an embodiment of the present invention;
fig. 2 is a schematic view of an ultrasonic generator assembly and disassembly structure used in an embodiment of the present invention.
Detailed Description
In order to make the objects, contents and advantages of the present invention clearer, the following detailed description of the embodiments of the present invention will be made in conjunction with the accompanying drawings and examples.
The embodiment provides a flow type ultrasonic treatment method for elemental explosive intercrystalline acid, which is suitable for acid-removing treatment of elemental explosives such as octogen, hexogen and taian.
As shown in figure 1, the method for treating intercrystalline acid of an elemental explosive by flow type ultrasonic adopts equipment comprising: the ultrasonic wave generator comprises an ultrasonic generator 1, an ultrasonic controller 2, a washer 3, a feeder 4, a magnetic circulating pump 5, a filter 6, a heating refrigerator 7, an explosion-proof vacuum oven 8, a thermometer 9 and a pH meter 10. Wherein, the discharge hole of the feeder 4 is connected with the liquid inlet pipeline of the magnetic circulating pump 5, and the liquid outlet of the magnetic circulating pump 5 is connected with the feed inlet at the lower end of the washer 3; an ultrasonic generator 1 controlled by an ultrasonic controller 2 is installed on a washer 3; the inlet and outlet of the jacket of the scrubber 3 are connected with a heating refrigerator 7, and the bottom branch of the scrubber 3 is connected with a filter 6; a thermometer 9 and a pH meter 10 are installed on the washer 3, and measure the temperature and pH value of the washing process.
In this embodiment, the diameter of the washer 3 is not more than 20cm, and the volume is not more than 60L, and beyond this range, the ultrasonic action intensity will be weakened, and the action effect will be reduced. The ultrasonic generator 1 is in an assembled and individually detachable form, as shown in fig. 2, and the tool head 11, the polished rod 12, the transducer, and the like are in an assembled form. Wherein, the length ratio of the tool head 11, the extension bar 13 and the polish rod 12 is 1:2: 3. In addition, if industrial amplification is required, only a plurality of washers 3 need to be connected in series, and the flow of the magnetic circulating pump 5 needs to be increased, without changing parameters such as ultrasonic power, frequency, temperature and ultrasonic time.
The method for treating the intercrystalline acid of the single-substance explosive by the flowing ultrasonic comprises the following steps:
s1, taking the crude product of the acid-containing single-substance explosive on the production line, mixing the crude product with water according to a certain proportion to form a mixed material, and adding the mixed material into a feeder 4. Wherein the mass ratio of the product of different single-substance explosives to the water is different, and the range is 1 (1-2);
s2, starting the heating refrigerator 7, and controlling the temperature in the washer 3 through a washer 3 jacket to keep the temperature in the washer 3 at 25-45 ℃;
s3, starting the magnetic circulating pump 5, setting a certain circulating speed to enable the mixed material to enter from the lower end of the washer 3 and flow out from the upper end, starting the ultrasonic generator 1 after 5-10 min of circulation, and adjusting the ultrasonic power through the ultrasonic controller 2, wherein the ultrasonic power does not exceed 2.8kw, the adjusting range is 20-100%, and the ultrasonic frequency is 15-45 kHz to ensure the action safety and the requirement on the granularity of the single-substance explosive product;
s4, in the ultrasonic process, controlling the temperature in the washer 3 to be not more than 50 ℃, and stopping ultrasonic when the pH value in the washer 3 is stable after circularly washing for 15-45 min;
s5, opening a bottom branch valve of the washer 3, filtering the washed elementary explosive product through a filter 6, and leaching twice through tap water, wherein the mass ratio of the single leaching water amount to the acid-containing elementary explosive is about 1: 10; and then sending the washed filter cake into an explosion-proof vacuum oven 8 for drying to obtain the single-substance explosive product meeting the acidity requirement in the national military standard.
Example 1
The embodiment provides a method for processing intercrystalline acid of an elemental explosive by flowing ultrasonic, which specifically comprises the following steps:
s1, taking 1kg of an octogen crude product with acidity of about 10%, measuring 1.5L of tap water to prepare a mixed solution, and feeding the mixed solution into a circulating pipeline through a stainless steel feeder 4;
s2, starting a heating refrigerator 7, heating a 2.5L washer 3 through a jacket, and maintaining the temperature in the washer at 45 +/-1 ℃;
s3, starting the magnetic circulating pump 5, setting the flow rate at 500L/h, enabling a mixture of the crude product of HMX and water to enter from the lower end of the washer 3, enabling the mixture to flow out from an overflow port at the upper end after the volume is full, observing liquid flowing out through a pipeline sight glass, and continuing to circulate for 5 min;
s4, starting the ultrasonic generator 1, setting the ultrasonic power to be 40% through the ultrasonic controller 2, setting the ultrasonic frequency to be 20kHz, setting the washing time to be 25min, and adjusting the temperature in the washer 3 to be not more than 50 ℃ through the heating refrigerator 7 in the process;
s5, after washing for 20min, stabilizing the pH value of 10 in the washer 3 between 1 and 1.5, stopping ultrasound, turning off the magnetic circulating pump 5, opening a branch valve at the bottom of the washer 3, putting the mixed solution into the filter 6 for filtering, leaching a filter cake twice by 100mL tap water, sending the filter cake to an explosion-proof vacuum oven 8, drying for 2h under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.09 MPa, testing the acidity of the dried product to be 0.02 percent, and meeting the requirements of the national military standard.
Example 2
The embodiment provides a method for processing intercrystalline acid of an elemental explosive by flowing ultrasonic, which specifically comprises the following steps:
s1, taking 2kg of a crude product of Taian with acidity of about 4%, measuring 2L of tap water to prepare a mixed solution, and feeding the mixed solution into a circulating pipeline through a stainless steel feeder 4;
s2, starting a heating refrigerator 7, heating a 2.5L washer 3 through a jacket, and maintaining the temperature in the washer at 35 +/-1 ℃;
s3, starting the magnetic circulating pump 5, setting the flow rate at 600L/h, enabling a mixture of the crude product of HMX and water to enter from the lower end of the washer 3, enabling the mixture to flow out from an overflow port at the upper end after the volume is full, observing liquid flowing out through a pipeline sight glass, and continuing to circulate for 5 min;
s4, starting the ultrasonic generator 1, setting the ultrasonic power to be 50% through the ultrasonic controller 2, setting the ultrasonic frequency to be 25kHz, setting the washing time to be 20min, and adjusting the temperature in the washer 3 to be not more than 40 ℃ through the heating refrigerator 7 in the process;
s5, after washing for 25min, stabilizing the pH value of 10 in the washer 3 between 1 and 1.5, stopping ultrasound, turning off the magnetic circulating pump 5, opening a branch valve at the bottom of the washer 3, putting the mixed solution into the filter 6 for filtering, leaching the filter cake twice with 200mL tap water, sending the filter cake to the explosion-proof vacuum oven 8, drying for 1.5h under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.09 MPa, testing the acidity of the dried product to be 0.01 percent, and meeting the requirements of the national military standard.
Example 3
The embodiment provides a method for processing intercrystalline acid of an elemental explosive by flowing ultrasonic, which specifically comprises the following steps:
s1, taking 10kg of crude hexogen with acidity of about 11.5%, measuring 20L of tap water to prepare a mixed solution, and feeding the mixed solution into a circulating pipeline through a stainless steel feeder 4;
s2, starting a heating refrigerator 7, heating a 30L washer 3 through a jacket, and maintaining the temperature in the washer at 40 +/-1 ℃;
s3, starting the magnetic circulating pump 5, setting the flow rate to be 1500L/h, enabling a mixture of the crude product of HMX and water to enter from the lower end of the washer 3, enabling the mixture to flow out from an overflow port at the upper end after the volume is full, and continuing to circulate for 5min after liquid flows out through observation of a pipeline sight glass;
s4, starting the ultrasonic generator 1, setting the ultrasonic power to be 80% through the ultrasonic controller 2, setting the ultrasonic frequency to be 20kHz, setting the washing time to be 40min, and adjusting the temperature in the washer 3 to be not more than 45 ℃ through the heating refrigerator 7 in the process;
s5, after washing for 40min, stabilizing the pH value of 10 in the washer 3 between 1 and 1.5, stopping ultrasound, turning off the magnetic circulating pump 5, opening a branch valve at the bottom of the washer 3, putting the mixed solution into the filter 6 for filtering, leaching a filter cake twice by 1L of tap water, sending the filter cake to an explosion-proof vacuum oven 8, drying for 2h under the conditions that the temperature is 60 ℃ and the vacuum degree is-0.09 MPa, testing the acidity of the dried product to be 0.04 percent, and meeting the requirements of the national military standard.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (2)
1. A method for flow type ultrasonic treatment of intercrystalline acid of an elemental explosive is characterized by comprising the following steps:
s1, taking a crude product containing an acid elementary substance explosive, and mixing the crude product with water to form a mixed material; wherein the mixing ratio of the single-substance explosive to water is 1 (1-2);
s2, controlling the temperature in the washer to be kept at 25-45 ℃; the diameter of the washer is not more than 20 cm;
s3, enabling the mixed material to enter from the lower end of the washer, circulating in the washer for 5-10 min, then enabling the mixed material to flow out from the upper end, and performing ultrasonic treatment after circulating for a certain time; wherein the ultrasonic power is not more than 2.8kw, the adjusting range is 20% -100%, and the ultrasonic frequency is 15-45 kHz; the ultrasonic generator is assembled and disassembled independently, and the tool head, the polished rod and the transducer are assembled; the length ratio of the tool head, the extension bar and the light bar of the ultrasonic generator is 1:2: 3;
s4, in the ultrasonic process, controlling the temperature in the washer to be not more than 50 ℃, and after circularly washing for 15-45 min, stopping ultrasonic when the pH value in the washer is stable;
s5, filtering and leaching the washed single-substance explosive product, and drying to obtain a single-substance explosive product meeting the acidity requirement; wherein the mass ratio of the single leaching water amount to the acid-containing single-substance explosive is about 1: 10.
2. The method of claim 1, wherein the elemental explosive is octogen, hexogen, or taian.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911316032.1A CN111116278B (en) | 2019-12-19 | 2019-12-19 | Method for flow type ultrasonic treatment of intercrystalline acid of elemental explosive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911316032.1A CN111116278B (en) | 2019-12-19 | 2019-12-19 | Method for flow type ultrasonic treatment of intercrystalline acid of elemental explosive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111116278A CN111116278A (en) | 2020-05-08 |
| CN111116278B true CN111116278B (en) | 2022-02-22 |
Family
ID=70500388
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911316032.1A Active CN111116278B (en) | 2019-12-19 | 2019-12-19 | Method for flow type ultrasonic treatment of intercrystalline acid of elemental explosive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111116278B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2630102B1 (en) * | 1988-04-14 | 1990-12-28 | France Etat Armement | METHOD AND DEVICE FOR LOADING A HIGH BRISANCE EXPLOSIVE AMMUNITION |
| CN103601692A (en) * | 2013-11-05 | 2014-02-26 | 西安近代化学研究所 | Ultrasonic washing and deacidification process for cyclotrimethylene trinitramine |
| CN105237316A (en) * | 2015-09-25 | 2016-01-13 | 西安近代化学研究所 | Granular explosive continuous washing process |
| CN107602310A (en) * | 2017-10-30 | 2018-01-19 | 西安近代化学研究所 | Acid elution method is driven in a kind of gas whistle formula serialization suitable for explosive |
| CN109731562A (en) * | 2019-03-06 | 2019-05-10 | 四川大学 | A kind of two-part regeneration method of porous carbon base desulfurizer |
-
2019
- 2019-12-19 CN CN201911316032.1A patent/CN111116278B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2630102B1 (en) * | 1988-04-14 | 1990-12-28 | France Etat Armement | METHOD AND DEVICE FOR LOADING A HIGH BRISANCE EXPLOSIVE AMMUNITION |
| CN103601692A (en) * | 2013-11-05 | 2014-02-26 | 西安近代化学研究所 | Ultrasonic washing and deacidification process for cyclotrimethylene trinitramine |
| CN105237316A (en) * | 2015-09-25 | 2016-01-13 | 西安近代化学研究所 | Granular explosive continuous washing process |
| CN107602310A (en) * | 2017-10-30 | 2018-01-19 | 西安近代化学研究所 | Acid elution method is driven in a kind of gas whistle formula serialization suitable for explosive |
| CN109731562A (en) * | 2019-03-06 | 2019-05-10 | 四川大学 | A kind of two-part regeneration method of porous carbon base desulfurizer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111116278A (en) | 2020-05-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108461749B (en) | Ternary precursor production optimization control device and optimization control method thereof | |
| CN111116278B (en) | Method for flow type ultrasonic treatment of intercrystalline acid of elemental explosive | |
| CN203668013U (en) | Potassium nitrate purification equipment | |
| CN219784456U (en) | Production agitated vessel of water treatment agent product | |
| CN111217723A (en) | Preparation process of ultrafine particle nitroguanidine | |
| CN102424393B (en) | Method for synchronously removing multiple impurities from quartz sand | |
| CN103601692B (en) | Ultrasonic washing and deacidification process for cyclotrimethylene trinitramine | |
| CN105111090B (en) | A kind of continuous preparation method of the dinitro ethene of 1,1 diaminourea 2,2 | |
| CN105440727A (en) | Preparation method of ester group-containing azo disperse dye | |
| CN110747296A (en) | Decolorizing method of heavy sugar in acesulfame potassium production | |
| CN103710552A (en) | Leaching technique and system for preparing vanadium solution by quenching vanadium slag roasting clinker | |
| RU2141449C1 (en) | Method of purification of natural graphite | |
| CN105440737B (en) | A kind of preparation method of energy saving and environment friendly disperse dyes | |
| CN105755069A (en) | Method using corn cobs to prepare xylo-oligosaccharide | |
| CN111533774B (en) | Continuous automatic extraction production process of baicalin | |
| CN101607946B (en) | Method for purifying tolytriazole sodium salt | |
| CN103432945A (en) | Equipment and method for preparing mixed acid | |
| CN109384206A (en) | The production system and production method of the process units and production method of silicon imide, silicon nitride | |
| CN208525884U (en) | A kind of magnesium sulfate continuous crystallisation device | |
| CN107602310B (en) | Air whistle type continuous flooding acid washing method suitable for explosives | |
| CN101103803B (en) | Glutamic acid crystalloblastic technology | |
| CN203715281U (en) | Capacitor grade phosphoric acid yellow phosphorus purifying device | |
| CN209143709U (en) | A kind of quartz sand acid washout iron exclusion device | |
| CN112538030A (en) | Low-temperature continuous reactor and working method for producing diazo compound | |
| CN103771367A (en) | Method for producing electronic-grade phosphoric acid by stirring and crystallizing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |