CN103601692B - Ultrasonic washing and deacidification process for cyclotrimethylene trinitramine - Google Patents

Ultrasonic washing and deacidification process for cyclotrimethylene trinitramine Download PDF

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CN103601692B
CN103601692B CN201310545070.0A CN201310545070A CN103601692B CN 103601692 B CN103601692 B CN 103601692B CN 201310545070 A CN201310545070 A CN 201310545070A CN 103601692 B CN103601692 B CN 103601692B
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washing
cyclotrimethylene trinitramine
ultrasonic
cyclotrimethylene
trinitramine
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CN103601692A (en
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罗志龙
康超
邹高兴
陈松
李萌
陈超
杨毅
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Xian Modern Chemistry Research Institute
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D251/00Heterocyclic compounds containing 1,3,5-triazine rings
    • C07D251/02Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
    • C07D251/04Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
    • C07D251/06Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with hetero atoms directly attached to ring nitrogen atoms

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Abstract

The invention provides a washing and deacidification process for cyclotrimethylene trinitramine. According to the process, an ultrasonic technology is adopted to wash acid-containing cyclotrimethylene trinitramine, and the process flow mainly comprises the steps of ultrasonically washing acid-containing cyclotrimethylene trinitramine, filtering cyclotrimethylene trinitramine, and drying cyclotrimethylene trinitramine. Acid-containing cyclotrimethylene trinitramine is effectively washed, filtered and dried under optimal ultrasonic washing process conditions, and then, a cyclotrimethylene trinitramine product which has the acidity lower than 0.05% and meets the requirements of international military standards can be obtained. The process has the advantages that the washing process is simple, the washing time is short, the energy consumption is low, the washing effect is excellent, and the problems of the original cyclotrimethylene trinitramine washing processes that the washing time is long, the energy consumption is high and the water consumption is large are solved.

Description

A kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process
Technical field
The invention belongs to explosive wastewater field, relate to Cyclotrimethylene trinitramine, be specifically related to a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process.
Background technology
Cyclotrimethylene trinitramine is as typical s-generation high explosive, and the method for countries nowadays production Cyclotrimethylene trinitramine is a lot, but production technique external at present adopts direct nitre solution and acetic anhydride method.Domestic more ripe production technique all adopts direct nitre solution to prepare Cyclotrimethylene trinitramine, namely with the direct nitrated urotropine of concentrated nitric acid.Direct nitre solution is prepared in the technological process of Cyclotrimethylene trinitramine, through nitrated, incidentally containing a certain amount of residual nitric acid between the plane of crystal of the Cyclotrimethylene trinitramine obtained after the operations such as crystallization and crystal.The existence of residual acid, can have a huge impact the chemical stability of Cyclotrimethylene trinitramine product and interior external contact compatibility, and in its standing storage and transportation, product itself also may be caused to decompose, and causes quality product to decline, also can cause certain potential safety hazard.Have strict requirement (I class Cyclotrimethylene trinitramine acidity is in nitric acid massfraction≤0.05%) to the acidity of Cyclotrimethylene trinitramine product in national military standard (GJB296A-95), therefore washing depickling is postprocessing working procedures very important after preparing Cyclotrimethylene trinitramine.
Existing Cyclotrimethylene trinitramine washing deacidifying process adopts high temperature steaming washing method: will containing sour Cyclotrimethylene trinitramine and water mixture (mass ratio is about 1:3) after crystallization, filter progress, then at 0.25MPa pressure, boil under 120 ~ 138 DEG C of conditions and wash, time is about 4h, after cooling, enter neutral density filter again filter, and wash again with cold water.This technique has that energy consumption is high, wastewater discharge large (often produce 1t Cyclotrimethylene trinitramine, wastewater discharge is about 5t, consumes steam about 2 ~ 4t), washing time are long, in defects such as pharmacy amount are large.
Summary of the invention
For the deficiency that prior art exists, the object of the invention is to, provide a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process of energy-conservation, consumption reduction, this technique can make to realize good deacidification effect in the short period of time containing sour Cyclotrimethylene trinitramine.
In order to realize above-mentioned task, the present invention adopts following technical scheme to be achieved:
A kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device comprises: washing kettle and safe baking oven, washing kettle outer wall is provided with outer circulation temperature controlling machine, thermometer, online pH meter and Ultrasonic probe are installed in washing kettle, Ultrasonic probe is connected with ultrasonic wave generator controller, and the bottom valve of washing kettle is connected with strainer, and strainer is provided with vacuum diaphragm pump;
The Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, inserts washing kettle by underproof for acidity Cyclotrimethylene trinitramine, adds water, opens the mechanical stirring of washing kettle, makes to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, and the mass ratio containing sour Cyclotrimethylene trinitramine and washing water consumption is 1:(1.5 ~ 2.5);
Step 2, opens outer circulation temperature controlling machine and design temperature, and washing temperature in the kettle is monitored by thermometer, and it is within 30 DEG C ~ 50 DEG C scopes that outer circulation temperature controlling machine control washing temperature in the kettle remains at;
Step 3, open ultrasonic wave generator controller and set ultrasonic power, the operating frequency of Ultrasonic probe is set as 20KHz ~ 25KHz, the carrying out washing treatment amount of suspension system and the pass of ultrasonic generator controller output rating are: 1L/(200 ~ 300) W, the pulse type supersonic sent by Ultrasonic probe produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water;
Step 4, online pH meter Real-Time Monitoring washing kettle includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after the reading of online pH meter no longer changes, open the bottom valve of washing kettle, Cyclotrimethylene trinitramine suspension in washing kettle is put into strainer, open vacuum diaphragm pump simultaneously and carry out suction filtration, after suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into safe baking oven drying, obtain the Cyclotrimethylene trinitramine product after depickling.
The present invention also has following technical characteristic:
The underproof Cyclotrimethylene trinitramine of described acidity is the Cyclotrimethylene trinitramine of nitric acid massfraction more than 0.05%.
The present invention compared with prior art, has following technological merit:
(A) ultrasonic washing deacidifying process of the present invention can complete at about 2h, boils wash technological work efficiency raising more than 50% than tradition.
(B) supersound washing deacidification of the present invention can complete (30 DEG C ~ 50 DEG C) under lower temperature condition, does not need steam heating, reduces energy consumption.
(C) more traditional the boiling of supersound washing deacidification water consumption of the present invention washes technique minimizing more than 30%, decreases discharge of wastewater.
Accompanying drawing explanation
Fig. 1 is Cyclotrimethylene trinitramine ultrasonic washing deacidifying process schema.
In figure, each label represents respectively: 1-outer circulation temperature controlling machine, 2-thermometer, the online pH meter of 3-, 4-washing kettle, 5-Ultrasonic probe, 6-strainer, 7-vacuum diaphragm pump, 8-ultrasonic wave generator controller, 9-safe baking oven.
Below in conjunction with drawings and Examples, particular content of the present invention is described in more detail.
Embodiment
Defer to technique scheme, as shown in Figure 1, following embodiment provides a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device comprises: washing kettle 4 and safe baking oven 9, washing kettle 4 outer wall is provided with outer circulation temperature controlling machine 1, thermometer 2, online pH meter 3 and Ultrasonic probe 5 are installed in washing kettle 4, Ultrasonic probe 5 is connected with ultrasonic wave generator controller 8, the bottom valve of washing kettle 4 is connected with strainer 6, strainer 6 is provided with vacuum diaphragm pump 7;
The Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, inserts washing kettle 4 by underproof for acidity Cyclotrimethylene trinitramine, adds water, opens the mechanical stirring of washing kettle 4, makes to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, and the mass ratio containing sour Cyclotrimethylene trinitramine and washing water consumption is 1:(1.5 ~ 2.5);
Step 2, open outer circulation temperature controlling machine 1 and design temperature, in washing kettle 4, temperature is monitored by thermometer 2, and it is within 30 DEG C ~ 50 DEG C scopes that outer circulation temperature controlling machine 1 controls that temperature in washing kettle 4 remains at;
Step 3, open ultrasonic wave generator controller 8 and set ultrasonic power, the operating frequency of Ultrasonic probe 5 is set as 20KHz ~ 25KHz, the carrying out washing treatment amount of suspension system and the pass of ultrasonic generator controller 8 output rating are: 1L/(200 ~ 300) W, the pulse type supersonic sent by Ultrasonic probe 5 produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water, for peeling off acid molecule accompanying on Cyclotrimethylene trinitramine crystal;
Step 4, online pH meter 3 Real-Time Monitoring washing kettle 4 includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after the reading of online pH meter 3 no longer changes, open the bottom valve of washing kettle 4, Cyclotrimethylene trinitramine suspension in washing kettle 4 is put into strainer 6, open vacuum diaphragm pump 7 simultaneously and carry out suction filtration, after suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into safe baking oven 9 drying, obtain the Cyclotrimethylene trinitramine product after depickling.
The underproof Cyclotrimethylene trinitramine of acidity is the Cyclotrimethylene trinitramine of nitric acid massfraction more than 0.05%.
Below provide specific embodiments of the invention, it should be noted that the present invention is not limited to following specific embodiment, all equivalents done on technical scheme basis all fall into protection scope of the present invention.
Embodiment 1:
The present embodiment provides a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device comprises: washing kettle 4 and safe baking oven 9, washing kettle 4 outer wall is provided with outer circulation temperature controlling machine 1, thermometer 2, online pH meter 3 and Ultrasonic probe 5 are installed in washing kettle 4, Ultrasonic probe 5 is connected with ultrasonic wave generator controller 8, and the bottom valve of washing kettle 4 is connected with strainer 6, strainer 6 is provided with vacuum diaphragm pump 7;
The Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, take the underproof Cyclotrimethylene trinitramine that 1000g acidity is 1.01%, Cyclotrimethylene trinitramine is inserted the double glazing washing kettle 4 that 5L is with mechanical stirring device, add 2000g water, open the mechanical stirring of washing kettle 4, make to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, now in still, cumulative volume is about 2.7L;
Step 2, opens outer circulation temperature controlling machine 1 and design temperature is 40 DEG C, and in washing kettle 4, temperature is monitored by thermometer 2, and it is within 30 DEG C ~ 50 DEG C scopes that outer circulation temperature controlling machine 1 controls that temperature in washing kettle 4 remains at;
Step 3, opening ultrasonic wave generator controller 8 and setting ultrasonic power is 800W, the operating frequency of Ultrasonic probe 5 is set as 20KHz, the pulse type supersonic sent by Ultrasonic probe 5 produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water, for peeling off acid molecule accompanying on Cyclotrimethylene trinitramine crystal;
Step 4, online pH meter 3 Real-Time Monitoring washing kettle 4 includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after supersound washing 100min, the reading of online pH meter 3 no longer changes, and now pH meter reading is 1.13, closes ultrasonic wave generator controller 8, stop outer circulation temperature controlling machine 1, open the bottom valve of washing kettle 4, the Cyclotrimethylene trinitramine suspension in washing kettle 4 is put into strainer 6, open vacuum diaphragm pump 7 simultaneously and carry out suction filtration, add 500g water to washing kettle 4 and rinse the remaining Cyclotrimethylene trinitramine of still wall, washing lotion is put in the lump strainer 6 and proceed vacuum filtration.
After suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into safe baking oven 9 drying, obtain the Cyclotrimethylene trinitramine product after depickling, be about 0.03% according to its acidity of GJB296A-95 Acidity Test Method test determination, be namely met the Cyclotrimethylene trinitramine product that national military standard (GJB296A-95) requires.
The acidity of Cyclotrimethylene trinitramine carries out test determination according to GJB296A-95 " Cyclotrimethylene trinitramine specification ", and concrete test process is:
Take sample and be about 5g, be accurate to 0.1g.Be placed in 250ml Erlenmeyer flask, add 50ml acetone, be placed in water-bath to be heated to micro-boiling test portion is all dissolved, then 50ml water is added, two methyl red indicators are added after being cooled to room temperature, be titrated to test solution with Standard Volumetric Solutions for Sodium Hydroxide and become dark yellow, the volume that record Standard Volumetric Solutions for Sodium Hydroxide consumes, carry out blank test by aforesaid operations simultaneously.
The data processing of experimental result and being assessed as:
Acidity is by following formulae discovery: w = c ( V 2 - V 1 ) × 0.063 m × 100 %
In formula:
W is test portion acidity (massfraction);
C is the concentration of Standard Volumetric Solutions for Sodium Hydroxide, mol/L;
V 2for titration sample solution consumes the volume of Standard Volumetric Solutions for Sodium Hydroxide, ml;
V 1for blank test consumes the volume of Standard Volumetric Solutions for Sodium Hydroxide, ml;
M is test portion quality, g;
0.063 is suitable for 1.00ml Standard Volumetric Solutions for Sodium Hydroxide [C (NaOH)=1.000mol/L] a gram quality for the nitric acid represented;
Tolerance: 0.005%.
Every part of sample replicate(determination) two results, the difference of two results is not more than tolerance, gets its arithmetical av and is acidity.
Embodiment 2:
The present embodiment provides a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device is identical with embodiment 1, and the Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, take the underproof Cyclotrimethylene trinitramine that 2000g acidity is 1.01%, Cyclotrimethylene trinitramine is inserted the double glazing washing kettle 4 that 10L is with mechanical stirring device, add 4000g water, open the mechanical stirring of washing kettle 4, make to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, now in still, cumulative volume is about 5.4L;
Step 2, opens outer circulation temperature controlling machine 1 and design temperature is 45 DEG C, and in washing kettle 4, temperature is monitored by thermometer 2, and it is within 30 DEG C ~ 50 DEG C scopes that outer circulation temperature controlling machine 1 controls that temperature in washing kettle 4 remains at;
Step 3, opening ultrasonic wave generator controller 8 and setting ultrasonic power is 1500W, the operating frequency of Ultrasonic probe 5 is set as 25KHz, the pulse type supersonic sent by Ultrasonic probe 5 produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water, for peeling off acid molecule accompanying on Cyclotrimethylene trinitramine crystal;
Step 4, online pH meter 3 Real-Time Monitoring washing kettle 4 includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after supersound washing 120min, the reading of online pH meter 3 no longer changes, and now pH meter reading is 1.12, closes ultrasonic wave generator controller 8, stop outer circulation temperature controlling machine 1, open the bottom valve of washing kettle 4, the Cyclotrimethylene trinitramine suspension in washing kettle 4 is put into strainer 6, open vacuum diaphragm pump 7 simultaneously and carry out suction filtration, add 1000g water to washing kettle 4 and rinse the remaining Cyclotrimethylene trinitramine of still wall, washing lotion is put in the lump strainer 6 and proceed vacuum filtration.
After suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into the drying of safe baking oven 9 to Cyclotrimethylene trinitramine, obtain the Cyclotrimethylene trinitramine product after depickling, be about 0.03% according to its acidity of GJB296A-95 test determination, be namely met the Cyclotrimethylene trinitramine product that national military standard (GJB296A-95) requires.
Embodiment 3:
The present embodiment provides a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device is identical with embodiment 1, and the Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, take the underproof Cyclotrimethylene trinitramine that 1000g acidity is 1.21%, Cyclotrimethylene trinitramine is inserted the double glazing washing kettle 4 that 5L is with mechanical stirring device, add 1500g water, open the mechanical stirring of washing kettle 4, make to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, now in still, cumulative volume is about 2.2L;
Step 2, opens outer circulation temperature controlling machine 1 and design temperature is 30 DEG C, and in washing kettle 4, temperature is monitored by thermometer 2;
Step 3, opening ultrasonic wave generator controller 8 and setting ultrasonic power is 450W, the operating frequency of Ultrasonic probe 5 is set as 20KHz, the pulse type supersonic sent by Ultrasonic probe 5 produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water, for peeling off acid molecule accompanying on Cyclotrimethylene trinitramine crystal;
Step 4, online pH meter 3 Real-Time Monitoring washing kettle 4 includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after supersound washing 80min, the reading of online pH meter 3 no longer changes, and now pH meter reading is 0.92, closes ultrasonic wave generator controller 8, stop outer circulation temperature controlling machine 1, open the bottom valve of washing kettle 4, the Cyclotrimethylene trinitramine suspension in washing kettle 4 is put into strainer 6, open vacuum diaphragm pump 7 simultaneously and carry out suction filtration, add 500g water to washing kettle 4 and rinse the remaining Cyclotrimethylene trinitramine of still wall, washing lotion is put in the lump strainer 6 and proceed vacuum filtration.
After suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into the drying of safe baking oven 9 to Cyclotrimethylene trinitramine, obtain the Cyclotrimethylene trinitramine product after depickling, be about 0.02% according to its acidity of GJB296A-95 test determination, be namely met the Cyclotrimethylene trinitramine product that national military standard (GJB296A-95) requires.
Embodiment 4:
The present embodiment provides a kind of Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device is identical with embodiment 1, and the Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, take the underproof Cyclotrimethylene trinitramine that 1000g acidity is 0.82%, Cyclotrimethylene trinitramine is inserted the double glazing washing kettle 4 that 5L is with mechanical stirring device, add 2500g water, open the mechanical stirring of washing kettle 4, make to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, now in still, cumulative volume is about 3.2L;
Step 2, opens outer circulation temperature controlling machine 1 and design temperature is 50 DEG C, and in washing kettle 4, temperature is monitored by thermometer 2;
Step 3, opening ultrasonic wave generator controller 8 and setting ultrasonic power is 1000W, the operating frequency of Ultrasonic probe 5 is set as 25KHz, the pulse type supersonic sent by Ultrasonic probe 5 produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water, for peeling off acid molecule accompanying on Cyclotrimethylene trinitramine crystal;
Step 4, online pH meter 3 Real-Time Monitoring washing kettle 4 includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after supersound washing 80min, the reading of online pH meter 3 no longer changes, and now pH meter reading is 1.32, closes ultrasonic wave generator controller 8, stop outer circulation temperature controlling machine 1, open the bottom valve of washing kettle 4, the Cyclotrimethylene trinitramine suspension in washing kettle 4 is put into strainer 6, open vacuum diaphragm pump 7 simultaneously and carry out suction filtration, add 500g water to washing kettle 4 and rinse the remaining Cyclotrimethylene trinitramine of still wall, washing lotion is put in the lump strainer 6 and proceed vacuum filtration.
After suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into the drying of safe baking oven 9 to Cyclotrimethylene trinitramine, obtain the Cyclotrimethylene trinitramine product after depickling, be about 0.02% according to its acidity of GJB296A-95 test determination, be namely met the Cyclotrimethylene trinitramine product that national military standard (GJB296A-95) requires.
Cyclotrimethylene trinitramine supersound washing deacidifying process given by above-described embodiment, technological process is simple, does not need steam heating can realize containing the deacidification effect of sour Cyclotrimethylene trinitramine, effectively solves conventional boil washing process energy consumption high, water consumption is large, and washing time is grown, deposit dose great Yi causes dangerous problem.

Claims (2)

1. a Cyclotrimethylene trinitramine ultrasonic washing deacidifying process, it is characterized in that, this technique adopts ultrasonic washing deacidifying device to realize, described ultrasonic washing deacidifying device comprises: washing kettle (4) and safe baking oven (9), washing kettle (4) outer wall is provided with outer circulation temperature controlling machine (1), thermometer (2) is installed in washing kettle (4), online pH meter (3) and Ultrasonic probe (5), Ultrasonic probe (5) is connected with ultrasonic wave generator controller (8), the bottom valve of washing kettle (4) is connected with strainer (6), strainer (6) is provided with vacuum diaphragm pump (7),
The Cyclotrimethylene trinitramine ultrasonic washing deacidifying process adopting ultrasonic washing deacidifying device to realize carries out in accordance with the following steps:
Step one, underproof for acidity Cyclotrimethylene trinitramine is inserted washing kettle (4), adds water, open the mechanical stirring of washing kettle (4), make to form suspension system containing sour Cyclotrimethylene trinitramine and washing water, the mass ratio containing sour Cyclotrimethylene trinitramine and washing water consumption is 1:(1.5 ~ 2.5);
Step 2, opens outer circulation temperature controlling machine (1) and design temperature, and washing kettle (4) interior temperature is monitored by thermometer (2), and it is within 30 DEG C ~ 50 DEG C scopes that outer circulation temperature controlling machine (1) control washing kettle (4) interior temperature remains at;
Step 3, open ultrasonic wave generator controller (8) and set ultrasonic power, the operating frequency of Ultrasonic probe (5) is set as 20KHz ~ 25KHz, the carrying out washing treatment amount of suspension system and the pass of ultrasonic generator controller (8) output rating are: 1L/(200 ~ 300) W, the pulse type supersonic sent by Ultrasonic probe (5) produces cavitation effect in the suspension system containing sour Cyclotrimethylene trinitramine and water;
Step 4, online pH meter (3) Real-Time Monitoring washing kettle (4) includes the pH value in the suspension system of sour Cyclotrimethylene trinitramine and water;
Step 5, after the reading of online pH meter (3) no longer changes, open the bottom valve of washing kettle (4), Cyclotrimethylene trinitramine suspension in washing kettle (4) is put into strainer (6), open vacuum diaphragm pump (7) simultaneously and carry out suction filtration, after suction filtration completes, wet product Cyclotrimethylene trinitramine is loaded drip pan and send into safe baking oven (9) drying, obtain the Cyclotrimethylene trinitramine product after depickling.
2. Cyclotrimethylene trinitramine ultrasonic washing deacidifying process as claimed in claim 1, it is characterized in that, the underproof Cyclotrimethylene trinitramine of described acidity is the Cyclotrimethylene trinitramine of nitric acid massfraction more than 0.05%.
CN201310545070.0A 2013-11-05 2013-11-05 Ultrasonic washing and deacidification process for cyclotrimethylene trinitramine Active CN103601692B (en)

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CN114249699A (en) * 2021-12-27 2022-03-29 甘肃银光化学工业集团有限公司 Method for filtering, washing, boiling and washing for producing hexogen

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