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CN102826938B - Continuous aftertreatment technology for single-compound explosive HMX - Google Patents

Continuous aftertreatment technology for single-compound explosive HMX Download PDF

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Publication number
CN102826938B
CN102826938B CN201210310737.4A CN201210310737A CN102826938B CN 102826938 B CN102826938 B CN 102826938B CN 201210310737 A CN201210310737 A CN 201210310737A CN 102826938 B CN102826938 B CN 102826938B
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China
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hmx
vacuum
cooling
agitator treating
washing
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Expired - Fee Related
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CN201210310737.4A
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Chinese (zh)
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CN102826938A (en
Inventor
杨毅
王晓东
商砚冰
罗志龙
邹高兴
陈�基
苏扬
程扬波
景青
卢栓仓
金建平
王勇
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Xian Modern Chemistry Research Institute
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Xian Modern Chemistry Research Institute
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Abstract

The invention discloses a continuous aftertreatment technology for single-compound explosive HMX. The continuous aftertreatment technology includes filtering, washing, drying and cooling. Devices required for implementing the continuous aftertreatment technology comprise a vacuum drum filter, a first stirring washing kettle, a mother liquor collecting tank, a second stirring washing kettle, a peristaltic pump, a vacuum disk filter, a washing liquor collecting tank, a vacuum disk rotational drying and cooling all-in-one machine and a material collecting barrel. The technological process includes realizing continuous filtering and spraying washing for synthetic suspension liquid HMX by the vacuum disk filter, feeding a filtered crude product HMX into the serially connected mechanical stirring washing kettles via discharge channels to complete overflow washing under mechanical stirring action, continuously conveying the washed crude product HMX to the vacuum disk filter by the peristaltic pump to filter the crude product HMX under the vacuum action; and freely dropping a filtered wet product HMX obtained in the previous step into the vacuum disk rotational drying and cooling all-in-one machine, drying and cooling the filtered wet product HMX under the condition of vacuumizing to obtain an product HMX with the purity higher than or equal to 99% and moisture content lower than or equal to 0.1%.

Description

The continuous aftertreatment technology of single chmical compound explosive HMX
Technical field
The invention belongs to fiery explosive technical field, relate to a kind of important continuous aftertreatment technology of single chmical compound explosive HMX, filter, wash, be dried and process for cooling.The filtration of especially a kind of HMX continuous and automatic, Long-distance Control, isolated operation, washing, dry and process for cooling process.
Background technology
Single chmical compound explosive HMX is a kind of broad-spectrum energetic material, is the important energy integral part of high-energy propellant, propelling agent and explosive.The at present both at home and abroad filtration of preparation HMX, washing, dryly all adopt interruption method technique with process for cooling process, man-machinely do not isolate, labour intensity greatly, the outstanding problem comparatively such as danger is high, intrinsic safety is poor.
The RDX production line of North America Huo Sidun Ammunition Plant, be the U.S. in the unique single chmical compound explosive manufacturing enterprise of North America, RDX manufacture to adopt the graceful method of Bark (acetic anhydride method) technique synthetic, its RDX washing, filter, the dry half-continuous process that still adopts.
The single chmical compound explosive manufacturing enterprise of China from the sixties in last century, adopts interruption method technique always, man-machinely do not isolate, and on-the-spot manual operations, high-intensity manual work, severe production environment, has seriously affected employee's physical and mental health.
Summary of the invention
Interruption method technique for the synthetic HMX of existing single chmical compound explosive, the technical problems such as process is discontinuous, human-machine operation is not isolated, danger is large, the object of the invention is to, for single chmical compound explosive HMX filters, washs, is dried and process of cooling, the continuous aftertreatment technology of single chmical compound explosive HMX a kind of man-machine isolated operation, continuous and automatic is provided, the powdery HMX product purity making is more than or equal to 99%, and moisture content is less than or equal to 0.1%.
In order to realize above-mentioned task, the present invention takes following technical solution:
The continuous aftertreatment technology of a kind of single chmical compound explosive HMX, it is characterized in that, this aftertreatment technology comprises filtration, washing, vacuum-drying and cooling, and the equipment of employing comprises: vacuum-type drum filter, the first agitator treating still, mother liquor receiving tank, the second agitator treating still, peristaltic pump, vacuum circular disk filter, washing lotion holding tank, disc rotary are dried and cooler, material collection bucket; Wherein:
Before described vacuum-type drum filter is connected in the first agitator treating still, and be connected with mother liquor receiving tank, the first agitator treating still and the second agitator treating still are connected in series, the second agitator treating still is connected with vacuum circular disk filter by peristaltic pump, vacuum disk hay tank connects washing lotion holding tank and is connected with cooler with disc rotary is dry, the dry material gathering barrel that is connected with cooler of disc rotary;
Its technological process is: by coming from the HMX suspension of condensation reaction operation, enter vacuum-type drum filter, under the effect of vacuum, complete solid-liquid separation, separated mother liquor enters mother liquor receiving tank; Crude product HMX after filtration relies on gravity to fall into the two-stage agitator treating still of series connection, completes agitator treating; HMX after agitator treating is transported in vacuum circular disk filter through peristaltic pump, under the effect of vacuum, completes filtration; The washing lotion of filtering enters in washing lotion receiving tank, the HMX freely falling body of solid to disc rotary dry with cooler in, under 100 ℃~110 ℃ temperature condition, through 50min~100min dry and cooling after, temperature is down to room temperature, obtains the powdery HMX product that purity is more than or equal to 98%, water ratio is less than or equal to 0.2% white.
The continuous aftertreatment technology of powdery single chmical compound explosive HMX of the present invention, technological process is carried out under sealing condition, environmental friendliness; on-the-spot clean, meet environment protection conditional request, and make operator away from hazardous location; labour intensity declines to a great extent, and product significantly reduces in amount processed.
Accompanying drawing explanation
Fig. 1 process flow diagram;
Fig. 2 automation control system schematic diagram;
Fig. 3 vacuum disk work principle of filter schematic diagram;
Fig. 4 disc rotary is dried and cooling principle schematic diagram.
The present invention is described in further detail for the embodiment providing below in conjunction with accompanying drawing and contriver.
Embodiment
As shown in Figure 1, the present embodiment provides the continuous aftertreatment technology of a kind of powdery single chmical compound explosive HMX, comprise filtration, washing, dry and cooling, the equipment of employing comprises: vacuum circular disk filter 1, first, second mechanical type agitator treating still (2,4), mother liquor receiving tank 3, peristaltic pump 5, vacuum circular disk filter 6, washing lotion holding tank 7, disc rotary are dried and cooler 8, material collection bucket 9.Wherein:
Before vacuum-type drum filter 1 is connected in the first agitator treating still 2, and be connected with mother liquor receiving tank 3, the first agitator treating still 2 and the second agitator treating still 4 are connected in series, the second agitator treating still 4 is connected with vacuum circular disk filter 6 by peristaltic pump 5, vacuum disk hay tank 6 connects washing lotion holding tank 7 and is connected with cooler 8 with disc rotary is dry, and disc rotary is dry is connected material gathering barrel 9 with cooler 8;
The HMX suspension that comes from pyrolytic reaction still, by pipeline, enter vacuum circular disk filter 1, under the effect of vacuum circular disk filter 1, realized the separated of HMX and mother liquor, mother liquor enters mother liquor receiving tank 3, HMX enters the first mechanical type agitator treating still 2 of series connection by blanking channel, the first mechanical type agitator treating still 2 adds tap water by pipeline, under churned mechanically effect, complete washing, HMX suspension after washing overflows to the second mechanical type agitator treating still 4 by pipeline, under churned mechanically effect, continue agitator treating.HMX suspension after washing, baiting valve by the second mechanical type agitator treating still 4 bottoms, pipeline, through peristaltic pump 5, non-return valve, arrival vacuum circular disk filter 6, a large amount of washing lotion in elimination HMX, washing lotion enters washing lotion holding tank 7, HMX arrives disk by blanking channel and is dried and cooler 8, in arid region, under the effect of high temperature circulation water, below HMX moisture drying to 0.1%, slow circumvolve along with disc rotary platform, material arrives disk cooled region, under the effect of cooling circulating water, the temperature of HMX is reduced to room temperature.HMX, under automatic control, isolated operation condition, has completed continuous filtration, washing, dry and cooling like this, and finally dried material enters gathering barrel 1-9.Material has completed continous vacuum disk filtration, the mechanical agitator treating of connecting, peristaltic pump are carried continuously, vacuum disk filtration, disc rotary is dry and turn cooling process.
Referring to as shown in Figure 2, in the present embodiment, automatic control system comprises: active station 2-1, printer 2-2, PLC controller 2-3, frequency transformer and field instrument 2-4 etc., wherein:
Active station is comprised of an industrial computer 2-1, and active station, as man machine operation interface, is realized processing parameter demonstration, set-point setting, technical process demonstration, warning, the inquiry of historical data function.Operator, by the operation to man-machine interface, realize Long-distance Control and isolated operation.
The function of printer 2-2 mainly completes output and the printing of production report.
PLC controller 2-3 is the core of Controlling System, mainly completes the processing parameter collections such as temperature, moisture, static of material, and carries out control strategy computing and judgement, finally by topworks, frequency transformer, is realized and is automatically regulated and control.
Field instrument 2-4 is mainly comprised of the primary instruments such as platinum-resistance thermometer, pressure transmitter, moisture detector, electrostatic detector and on-line detector device, mainly completes the automatic detection of processing parameter.
As shown in Figure 3, vacuum circular disk filter has blanking channel 3-1 for 6 minutes, 3-2(I district, mother liquor filtrating area), spray washing district 3-3(II district), vacuum dewatering zone 3-4(III district) and, 3-5(IV district, blowback discharging area).
The working process of vacuum circular disk filter 6 is, by the material after the agitator treating of peristaltic pump 5, by blanking channel 3-1, arrive disk filtration district 3-2(I district), under the effect of vacuum, a large amount of moisture in elimination material, rotation along with disk, moisture is progressively filtered dry, when material reaches drip washing district 3-3(II district), material is by spray washing, slowly rotation along with disk, material reaches dewatering zone 3-4(III district), under the effect of vacuum, by vacuum again, drained, when material arrives 3-5(IV district, blowback discharging area), under the slowly driving of pneumatic motor 3-7, spiral 3-6 releases vacuum circular disk filter by material, material is promoted to fall to arriving subsequent processing.
As shown in Figure 4, disc rotary is dry comprises a disc rotary platform with cooler 8, on disc rotary platform, dispose distributor 4-1, stock pusher 4-6, material scraper 4-7 and blanking channel 4-8, disc rotary platform is divided into 4-2He cooling zone, drying zone 4-3, on the 4-2 of drying zone, there is dry rake glassware 4-4, on the 4-3 of cooling zone, have cooling rake glassware 4-5.
Disc rotary is dry can be dried with cooling with cooler 8 simultaneously, successive drying and cooling referring to by dry material, by the distributor 4-1 on 4-2 top, drying zone, pulverulent material that will be dry is distributed on the drying zone 4-2 of disc rotary platform equably, logical high temperature (100 ℃ ~ 110 ℃) recirculated water in the 4-2 chuck of drying zone, under the effect of high temperature, moisture in material is evaporated fast, evaporation along with moisture, by dry material, easily formed duricrust, under the effect of dry rake glassware 4-4, material is stirred and is harrowed pine, moisture in stirring and harrow loose material continues rapid evaporation, moisture is lowered to below 0.1%.
Slow rotation along with disc rotary platform, when material arrives stock pusher 4-6, by stock pusher 4-6, released drying zone 4-2, cross dry and cooling line of delimitation, arrive cooling zone 4-3, logical cooling circulating water in the chuck of cooling zone 4-3, material obtains cooling in this region, along with the slow rotation of disc rotary platform, cooling rake glassware 4-5 stir and harrow pine twice, stirred and harrowed loose material and be quickly cooled to room temperature.Along with the continuation of disc rotary platform is slowly rotated, when material arrives material scraper 4-7, by material scraper, scraped rotary working platform, by blanking channel 4-8, arrive in material collection bucket 1-9, material has completed dry and cooling simultaneously like this.The single chmical compound explosive HMX purity obtaining is more than or equal to 99%, and moisture is less than or equal to 0.1%.

Claims (4)

1. the continuous aftertreatment technology of powdery single chmical compound explosive HMX, it is characterized in that, this aftertreatment technology comprises filtration, washing, vacuum-drying and cooling, and the equipment of employing comprises: vacuum-type drum filter (1), the first agitator treating still (2), mother liquor receiving tank (3), the second agitator treating still (4), peristaltic pump (5), vacuum circular disk filter (6), washing lotion holding tank (7), disc rotary are dried and cooler (8), material collection bucket (9); Wherein:
Described vacuum-type drum filter (1) is connected in the first agitator treating still (2) before, and be connected with mother liquor receiving tank (3), the first agitator treating still (2) and the second agitator treating still (4) are connected in series, the second agitator treating still (4) is connected with vacuum circular disk filter (6) by peristaltic pump (5), vacuum disk hay tank (6) connects washing lotion holding tank (7) and is connected with cooler (8) with disc rotary is dry, and disc rotary is dry is connected material gathering barrel (9) with cooler (8);
Its technological process is: will come from the HMX suspension of condensation reaction operation, enter vacuum-type drum filter (1), under the effect of vacuum, complete solid-liquid separation, separated mother liquor enters mother liquor receiving tank (3); Crude product HMX after filtration relies on gravity to fall into the two-stage agitator treating still (2,4) of series connection, completes agitator treating; HMX after agitator treating is transported in vacuum circular disk filter (6) through peristaltic pump (5), under the effect of vacuum, completes filtration; The washing lotion of filtering enters in washing lotion holding tank (7), the HMX freely falling body of solid to disc rotary dry with cooler (8) in, under 100 ℃~110 ℃ temperature condition, through 50min~100min dry and cooling after, temperature is down to room temperature, obtains the powdery HMX product that purity is more than or equal to 98%, water ratio is less than or equal to 0.2% white.
2. technique as claimed in claim 1, it is characterized in that, the first described agitator treating still (2) and the top of the second agitator treating still (4) are provided with motor-driven mechanical stirrer, bath water inlet channel and valve, and blowing pipeline and valve, overflow port and transport pipe are arranged at kettle bottom.
3. technique as claimed in claim 1, it is characterized in that in described vacuum circular disk filter (6), minute having blanking channel (3-1), mother liquor filtrating area (3-2), spray washing district (3-3), vacuum dewatering zone (3-4) and blowback discharging area (3-5).
4. technique as claimed in claim 1, it is characterized in that, described disc rotary is dry comprises a disc rotary platform with cooler (8), on disc rotary platform, dispose distributor (4-1), stock pusher (4-6), material scraper (4-7) and blanking channel (4-8), disc rotary platform is divided into drying zone (4-2) and cooling zone (4-3), on drying zone (4-2), there is dry rake glassware (4-4), on cooling zone (4-3), have cooling rake glassware (4-5).
CN201210310737.4A 2012-08-28 2012-08-28 Continuous aftertreatment technology for single-compound explosive HMX Expired - Fee Related CN102826938B (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103694065B (en) * 2013-11-11 2016-07-06 西安近代化学研究所 A kind of miniature ball wash mill and method
CN103940698B (en) * 2014-05-06 2016-03-02 湖北三江航天江河化工科技有限公司 A kind of HMX content assaying method
CN105013759A (en) * 2015-08-19 2015-11-04 成都鑫成鹏线缆材料有限公司 Cleaning equipment of cable raw materials and cleaning process
CN105237316B (en) * 2015-09-25 2017-07-04 西安近代化学研究所 A kind of continuous washing process of graininess explosive wastewater
CN107602310B (en) * 2017-10-30 2020-05-29 西安近代化学研究所 Air whistle type continuous flooding acid washing method suitable for explosives

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3770721A (en) * 1956-02-09 1973-11-06 Us Army Direct production of beta hmx
EP0547735A1 (en) * 1991-10-15 1993-06-23 GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by THE SECRETARY OF THE ARMY Process for the preparation of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane
CN1970514A (en) * 2005-11-25 2007-05-30 南京理工大学 Nickel hydrazine azide, its preparation method and uses as explosive ignitor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3770721A (en) * 1956-02-09 1973-11-06 Us Army Direct production of beta hmx
EP0547735A1 (en) * 1991-10-15 1993-06-23 GOVERNMENT OF THE UNITED STATES OF AMERICA, as represented by THE SECRETARY OF THE ARMY Process for the preparation of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane
CN1970514A (en) * 2005-11-25 2007-05-30 南京理工大学 Nickel hydrazine azide, its preparation method and uses as explosive ignitor

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