CN109985598A - A kind of continuous synthesizer of richness nitrogen ion salt containing energy - Google Patents
A kind of continuous synthesizer of richness nitrogen ion salt containing energy Download PDFInfo
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- CN109985598A CN109985598A CN201910326291.6A CN201910326291A CN109985598A CN 109985598 A CN109985598 A CN 109985598A CN 201910326291 A CN201910326291 A CN 201910326291A CN 109985598 A CN109985598 A CN 109985598A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of continuous synthesizers of rich nitrogen ion salt containing energy, belong to energetic material synthesis field, the continuous synthesizer includes self-dispersing jacketed reaction pipe, Continuous Heat Transfer reactor, recirculation assembly, auto feed component and product collection assembly.The device realizes that the rapid dispersion of material exchanges heat with quick by self-dispersing jacketed reaction pipe, improves reaction conversion ratio and process safety；The fast cooling precipitation that the deep conversion and product of raw material are realized by Continuous Heat Transfer reactor, ensure that the yield of product；The continuous circulation that feed liquid system is realized by recirculation assembly, ensure that the continuity of production process；The real-time collecting and removal that ion product salt is realized by product collection assembly, improve the safety of production process.Richness nitrogen continuous synthesizer structure of ion salt containing energy provided by the invention is simple, it is easy to implement, the bottleneck problems such as reaction efficiency is low, reaction temperature is not easy to control, single batch yield is small, production cycle length are efficiently solved in rich nitrogen ion salt synthesis process containing energy, the continuous batch preparation of rich nitrogen ion salt containing energy is realized.
Description
Technical field
The present invention relates to a kind of continuous synthesizers of rich nitrogen ion salt containing energy, belong to energetic material synthesis field.
Background technique
Rich nitrogen containing can ion salt be a kind of novel green energetic material, it generally refers in molecule nitrogen content 20% or more
Inorganic or organic high nitrogen salt, such as nitrate, perchlorate, Zoamix salt.Since rich nitrogen ion salt containing energy has life
At enthalpy is high, thermal stability is good, Yi Shixian oxygen balance, sensitivity is low, decomposition product cleans, advantages of environment protection, in solid propellant propulsion
The fields such as agent, liquid monopropellant, gas generator and the low sense explosive of high energy show huge applications potentiality, have good
Application prospect.
The synthesis process of rich nitrogen ion salt containing energy usually utilizes the rich nitrogen energy-containing compound of alkalinity and corresponding sour generation acid
Alkali neutralization reaction preparation.Such as: rich nitrogen ion salt methylamine nitrate containing energy is after acid-base neutralization reaction occurs by methylamine and nitric acid
Crystallization obtains.Since acid-base neutralization reaction process is violent, a large amount of heat can be discharged in reaction, temperature when preparing using reaction kettle batch
Degree is not easy to control, and when reaction temperature is excessively high, portion's separation nitrogen-enriching energy-containing compound will be slow decomposition, cause content of reaction byproduct compared with
Height, product yield is lower (being lower than 50wt%), and product postprocessing purification process is cumbersome.Simultaneously because rich nitrogen ion salt containing energy all has
There is certain sensitivity, to avoid the occurrence of security risk, the magnitude disposably prepared using reaction kettle batch process is all smaller, this is again
The production cycle is brought compared with long, yield is few, is unable to satisfy the problems such as application demand.
The present invention is directed to the feature in rich nitrogen ion salt synthesis process containing energy and the application demand of batch preparation, designs and develops
A kind of continuous synthesizer for rich nitrogen ion salt containing energy out, solves in such a way that drop reaction is combined with enhanced heat exchange
Thermal discharge is big in synthetic reaction process, local temperature excessively high the problem of causing product to decompose；Using product real-time online collect with
The method of removal solves the problems, such as that product accumulation amount is excessive, there are security risks.It can effectively be solved using the continuous synthesizer
The bottlenecks such as reaction efficiency is low, reaction temperature is not easy to control, yield is small, the production cycle is long in certainly rich nitrogen ion salt synthesis process containing energy
Problem realizes the continuous industryization preparation of rich nitrogen ion salt containing energy.
Summary of the invention
The object of the present invention is to provide a kind of continuous synthesizers of rich nitrogen ion salt containing energy, and being contained with the rich nitrogen of solution can ion
The problems such as reaction temperature is not easy to control, reaction efficiency is low, yield is small, the production cycle is long in salt synthesis.
Above-mentioned purpose of the invention is mainly achieved by following technical solution:
A kind of continuous synthesizer of richness nitrogen ion salt containing energy, it is characterised in that continuous synthesizer is anti-by self-dispersing collet
Ying Guan, Continuous Heat Transfer reactor, recirculation assembly, auto feed component and 5 part of product collection assembly composition.
A kind of continuous synthesizer of rich nitrogen ion salt containing energy as described above, it is characterised in that the self-dispersing collet
Reaction tube is the high-boron-silicon glass pipe or quartz ampoule of outer diameter 3cm-5cm, internal diameter 2cm-4cm, and interlayer leads to the alcohols such as ethyl alcohol, ethylene glycol
Coolant liquid or alcohol water combination cooling liquid, the temperature of coolant liquid are -10 DEG C~-25 DEG C.Reaction tube is set there are two feed inlet, left side into
Material mouth is rich nitrogen energy-containing compound solution circulation port, has nut shape raised immediately below feed inlet；Right side feed inlet is acid solution charging
Mouthful, away from there is diameter to be the protrusion of 15mm at inner left wall 3cm, for promoting material evenly dispersed, improve reaction uniformity.From point
It dissipates jacketed reaction pipe tail portion and curves 120 °, for being connected with Continuous Heat Transfer reactor.
The continuous synthesizer of a kind of rich nitrogen ion salt containing energy as described above, it is characterised in that the Continuous Heat Transfer is anti-
Answering device is the jacketed pipe type reactor of diameter 2.4cm-6cm, length 18cm-60cm, leads to alcohol or alcohol-water mixture conduct between collet
Coolant liquid, the temperature of coolant liquid are -10 DEG C~-25 DEG C.Reactor and horizontal plane installation angle are 45 ° -60 °, and material is in gravity
It is voluntarily flowed in the reactor under effect, realizes deep reaction and heat exchange.
A kind of rich nitrogen as described above containing can ion salt continuous synthesizer, it is characterised in that the recirculation assembly by
Liquid trap, metering peristaltic pump and transfer pipeline composition.Liquid trap is the square glass closed container that volume is 10L-20L, liquid collecting
Round mouth is opened above device for collecting filtrate, side is connect far from opening at bottom 1/3 with peristaltic pump, interior to realize feed liquid circulation
The glass cold traps that diameter is 1~2cm are set, manage interior logical alcohol or alcohol-water mixture as coolant liquid, the temperature of coolant liquid is -10 DEG C
~-25 DEG C.Metering peristaltic pump is the self-priming peristaltic pump of tetrafluoro material, and flow can be adjusted between 3L/h~5L/h.Transfer pipeline is
Acid-proof alkaline excellent polytetrafluoro pipe or polyethylene, PA tube.
A kind of continuous synthesizer of rich nitrogen ion salt containing energy as described above, it is characterised in that the auto feed group
Part is made of micro-measurement peristaltic pump, acid charging bottle and acidproof charge pipe.Micro-measurement wriggling pump discharge is in 0.1ml/min-
Glass or quartzy acid-resistant container adjustable between 5ml/min, that sour charging bottle is volume 1L-5L, acidproof charge pipe are tetrafluoro or gather
The acidproof material such as ethylene or polypropylene.
A kind of continuous synthesizer of rich nitrogen ion salt containing energy as described above, it is characterised in that the product collection group
Part is made of sand core funnel, runing rest and seal nipple.The diameter of sand core funnel be 20cm-30cm, sand core aperture be 40~
80um, according to yield difference, funnel quantity can adjust between 3-6, symmetrically placed on runing rest.Runing rest is can
Around the wooden or plastic disc of the 360 ° of rotations in the center of circle, respective numbers circular hole is opened by funnel quantity on disk, to fixed sand core leakage
Bucket.Seal nipple is rubber material, for the sealed connection between funnel and liquid trap.
A kind of continuous synthesizer of rich nitrogen ion salt containing energy of the present invention, it is characterised in that rich nitrogen ion salt containing energy
Continuous synthesis process are as follows: alkaline energy-containing compound is mixed with alcohols equal solvent, is injected in the liquid trap of recirculation assembly,
Circulating cooling is opened, metering peristaltic pump is started, makes feed liquid abundant circulating cooling in systems, until feed liquid temperature is lower than 0 DEG C.It beats
Acid charging peristaltic pump is opened, acid solution is slowly added into self-dispersing jacketed reaction pipe, the crystal of formation is moved together with feed liquid, warp
Enter after Continuous Heat Transfer reactor and collects sand core funnel.After material collection in funnel is full, turntable is rotated, empty funnel is gone to and is connect
At receipts, product is continued to, collecting full product can take out, and carry out subsequent wash and drying process, realize continuous production.
Effect of the invention is that: richness nitrogen continuous synthesizer of ion salt containing energy of the present invention in self-dispersing by pressing from both sides
The method that protrusion is arranged in set reaction tube promotes material dispersion, by method control system temperature cooling in real time, improves product
Conversion ratio and selectivity；By the way that Continuous Heat Transfer reactor is arranged, the reaction time and cooling time of material are further increased, is improved
Reacting finisheding degree promotes product to be precipitated；The online collection that product is realized by setting product collection assembly, makes ion product salt
It can be removed from reaction system in time, avoid production process intermediate ion salt accumulation bring security risk, realized continuous
Production.The apparatus structure is simple, easy to implement, efficiently solve rich nitrogen containing can in ion salt synthesis reaction temperature it is not easy to control,
The problems such as reaction efficiency is low, yield is small, the production cycle is long.
Detailed description of the invention:
Fig. 1 is rich nitrogen continuous synthesizer schematic diagram of ion salt containing energy.
Fig. 2 is product collection assembly top view
Specific embodiment:
The working principle of the invention is further explained and is illustrated in the following with reference to the drawings and specific embodiments.
Embodiment 1:
The outer diameter for choosing self-dispersing jacketed reaction pipe is 3cm, and internal diameter is 2cm and direct 2.4cm, and length 18cm's continuously changes
Thermal reactor connection, interface size be 24/29, reactor and horizontal plane installation angle be 45 °, the coolant liquid used in device for
Glycol water, the temperature setting of coolant liquid is at -15 DEG C.The diameter for choosing sand core funnel is 20cm, and sand core aperture is 40um,
Funnel quantity chooses 3, symmetrically placed on runing rest, and is tightly connected itself and liquid-collecting bottle using sealing element.
Ethyl alcohol and alkaline presoma are injected in liquid trap after mixing, circulating cooling is opened, starts metering peristaltic pump,
Make feed liquid abundant circulating cooling in systems, until feed liquid temperature is to -10 DEG C.The acid that 1L is added in the nitric acid that concentration is 65% is added
Expect bottle, open acid charging peristaltic pump, adjusts micro-measurement wriggling pump discharge in 0.1ml/min, into self-dispersing jacketed reaction pipe
It is slowly added to acid solution, the crystal of formation enters after Continuous Heat Transfer reactor with feed liquid collects sand core funnel.To object in funnel
After material is collected completely, turntable is rotated, empty funnel is gone into receiving area, carries out continuous production.
The present embodiment can realize rich nitrogen containing can average daily 5 kilograms of the production capacity of ion salt, product purity be greater than 99%, with
Method of having a rest shortens 80% or more compared to the production cycle.
Embodiment 2:
Choose self-dispersing jacketed reaction pipe outer diameter be 5cm, internal diameter 2.5cm, with diameter 5cm, length 40cm it is continuous
Heat transfer reactor connection, interface size are 24/29, and reactor and horizontal plane installation angle are 45 °, the coolant liquid used in device
For ethyl alcohol, the temperature setting of coolant liquid is at -20 DEG C.The diameter for choosing sand core funnel is 20cm, and sand core aperture is 40um, funnel number
Amount chooses 4, symmetrically placed on runing rest, and is tightly connected itself and liquid-collecting bottle using sealing element, and connect metering pump,
Valve and other pipelines.
Methanol and alkaline presoma are injected in liquid trap after mixing, circulating cooling is opened, starts metering peristaltic pump,
Make feed liquid abundant circulating cooling in systems, until feed liquid temperature is to -20 DEG C.The acid that 2L is added in the nitric acid that concentration is 65% is added
Expect bottle, open acid charging peristaltic pump, adjusts micro-measurement wriggling pump discharge in 5ml/min, to self-dispersing jacketed reaction Guan Zhonghuan
Slow that acid solution is added, the crystal of formation enters after Continuous Heat Transfer reactor with feed liquid collects sand core funnel.To material in funnel
After collecting completely, turntable is rotated, empty funnel is gone into receiving area.
The present embodiment can realize rich nitrogen containing can average daily 8 kilograms of the production capacity of ion salt, product purity be greater than 99%, with
Method of having a rest shortens 89% or more compared to the production cycle.
Embodiment 3:
Choose self-dispersing jacketed reaction pipe outer diameter be 5cm, internal diameter 4cm, with direct 6cm, length 60cm continuously change
Thermal reactor connection, interface size be 24/29, reactor and horizontal plane installation angle be 45 °, the coolant liquid used in device for
Ethyl alcohol, the temperature setting of coolant liquid is at -22 DEG C.The diameter for choosing sand core funnel is 20cm, and sand core aperture is 40um, funnel quantity
Choose 6, it is symmetrically placed on runing rest, and be tightly connected itself and liquid-collecting bottle using sealing element, connection other pipelines and
Equipment.
Ethyl alcohol and alkaline presoma are injected in liquid trap after mixing, circulating cooling is opened, starts metering peristaltic pump,
Make feed liquid abundant circulating cooling in systems, until feed liquid temperature is to -15 DEG C.The acid that 5L is added in the nitric acid that concentration is 65% is added
Expect bottle, open acid charging peristaltic pump, adjusts micro-measurement wriggling pump discharge in 0.2ml/min, into self-dispersing jacketed reaction pipe
It is slowly added to acid solution, the crystal of formation enters after Continuous Heat Transfer reactor with feed liquid collects sand core funnel.To object in funnel
After material is collected completely, turntable is rotated, empty funnel is gone into receiving area.
The present embodiment can realize that rich nitrogen average daily 10 kilograms of production capacity of ion salt containing energy, product purity are greater than 99%, with
Batch process shortens 93% or more compared to the production cycle.
Reference examples:
Intermittence is carried out using 5L glass material reaction kettle to feed intake production.Before the alkalinity for being first 20% by 3.5kg concentration
It drives body ethanol solution and injects reaction kettle, be cooled to -15 DEG C while stirring.Then the nitric acid that concentration is 65% is passed through into constant pressure addition
Funnel is slowly dropped into reaction solution, is stirred when being added dropwise, and spreads the heat generated rapidly.After sour completion of dropwise addition, constant temperature is anti-
1h is answered, rich nitrogen ion product salt containing energy 783g is obtained after being finally filtered, washed, being dried.
The above, optimal specific embodiment only of the invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
The content that description in the present invention is not described in detail belongs to the well-known technique of professional and technical personnel in the field.
Claims (12)
1. a kind of continuous synthesizer of richness nitrogen ion salt containing energy, it is characterised in that continuous synthesizer is by self-dispersing jacketed reaction
Pipe, Continuous Heat Transfer reactor, recirculation assembly, auto feed component and product collection assembly composition.
2. a kind of rich nitrogen according to claim 1 containing can ion salt continuous synthesizer, it is characterised in that it is described from
Dispersion jacketed reaction pipe is the glass tube or quartz ampoule of outer diameter 3cm-5cm, internal diameter 2cm-4cm, and interlayer leads to the alcohol such as ethyl alcohol, ethylene glycol
Class coolant liquid or alcohol water combination cooling liquid, the temperature of coolant liquid are -10 DEG C~-25 DEG C.
3. a kind of self-dispersing jacketed reaction pipe according to claim 2, it is characterised in that reaction tube is set there are two feed inlet,
Left side feed inlet is rich nitrogen energy-containing compound solution circulation port, has nut shape raised immediately below feed inlet；Right side feed inlet is acid
Liquid feed inlet, away from there is diameter to be the protrusion of 15mm at inner left wall 3cm, self-dispersing jacketed reaction pipe tail portion curves 120 °, is used for
It is connected with Continuous Heat Transfer reactor.
4. a kind of continuous synthesizer of rich nitrogen ion salt containing energy according to claim 1, it is characterised in that the company
Continuous heat transfer reactor is the jacketed pipe type reactor of diameter 2.4cm-6cm, length 18cm-60cm, and alcohol is led between collet or alcohol water is mixed
Object is closed as coolant liquid, the temperature of coolant liquid is -10 DEG C~-25 DEG C, and reactor and horizontal plane installation angle are 45 ° -60 °.
5. a kind of continuous synthesizer of rich nitrogen ion salt containing energy according to claim 1, it is characterised in that described follows
Ring assemblies are made of liquid trap, metering peristaltic pump and transfer pipeline.
6. a kind of recirculation assembly according to claim 5, it is characterised in that the liquid trap is that volume is 10L-20L
Round mouth is opened for collecting filtrate in square glass closed container, liquid trap top, and side is far from opening at bottom 1/3 and metering peristaltic pump
Connection, built-in diameter are the glass cold traps of 1-2cm, manage interior logical alcohol or alcohol-water mixture as coolant liquid, the temperature of coolant liquid
It is -10 DEG C~-25 DEG C.
7. a kind of recirculation assembly according to claim 5, it is characterised in that the metering peristaltic pump be tetrafluoro material from
Suction peristaltic pump, range 3-5L/h.The transfer pipeline is acid-proof alkaline excellent polytetrafluoro pipe or polyethylene, poly- third
Alkene pipe.
8. a kind of rich nitrogen according to claim 1 containing can ion salt continuous synthesizer, it is characterised in that it is described from
Dynamic charging component is made of micro-measurement peristaltic pump, acid charging bottle and acidproof charge pipe.
9. a kind of auto feed component according to claim 8, it is characterised in that the micro-measurement wriggling pump discharge
It is adjustable between 0.1ml/min-5ml/min.The glass or quartzy acid-resistant container that the acid charging bottle is volume 1L-5L.Institute
The acidproof charge pipe stated is tetrafluoro or the acidproof material such as polyethylene or polypropylene.
10. a kind of continuous synthesizer of rich nitrogen ion salt containing energy according to claim 1, it is characterised in that the production
Product collection assembly is made of sand core funnel, runing rest and seal nipple.
11. a kind of product collection assembly according to claim 10, it is characterised in that the diameter of the sand core funnel is
20cm-30cm, sand core aperture are 40-80um, and funnel quantity is 3-6.The runing rest is can be around the rotation of 360 ° of the center of circle
Wooden or plastic disc, open respective numbers circular hole by funnel quantity on disk.The seal nipple is rubber material.
12. according to claim 1 to the continuous synthesizer of any one rich nitrogen ion salt containing energy described in 11, it is characterised in that
The continuous synthesis process of rich nitrogen ion salt containing energy are as follows: mix alkaline energy-containing compound with alcohols equal solvent, injection circulation
In the liquid trap of component, circulating cooling is opened, metering peristaltic pump is started, makes feed liquid abundant circulating cooling in systems, until material
Liquid temperature is lower than 0 DEG C.Acid charging peristaltic pump is opened, acid solution, the crystal of formation are slowly added into self-dispersing jacketed reaction pipe
It is moved together with feed liquid, enters after Continuous Heat Transfer reactor and collect sand core funnel.After material collection in funnel is full, rotation turns
Empty funnel is gone to receiving area, continues to product by disk, and collecting full product can take out, and carries out subsequent wash and drying
Process realizes continuous production.
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| CN201910326291.6A CN109985598A (en) | 2019-04-23 | 2019-04-23 | A kind of continuous synthesizer of richness nitrogen ion salt containing energy |
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| CN201910326291.6A CN109985598A (en) | 2019-04-23 | 2019-04-23 | A kind of continuous synthesizer of richness nitrogen ion salt containing energy |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172545A (en) * | 2013-04-02 | 2013-06-26 | 常州大学 | Method for preparing nitroguanidine through micro-channel reactor |
| CN103183620A (en) * | 2013-03-28 | 2013-07-03 | 常州大学 | Method for preparing nitroguanidine through guanidine sulfate nitrification in continuous-flow micro channel reactor |
| CN104860849A (en) * | 2015-06-04 | 2015-08-26 | 西安近代化学研究所 | Continuous crystallization process for preparing nitroguanidine through nitric acid method |
-
2019
- 2019-04-23 CN CN201910326291.6A patent/CN109985598A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183620A (en) * | 2013-03-28 | 2013-07-03 | 常州大学 | Method for preparing nitroguanidine through guanidine sulfate nitrification in continuous-flow micro channel reactor |
| CN103172545A (en) * | 2013-04-02 | 2013-06-26 | 常州大学 | Method for preparing nitroguanidine through micro-channel reactor |
| CN104860849A (en) * | 2015-06-04 | 2015-08-26 | 西安近代化学研究所 | Continuous crystallization process for preparing nitroguanidine through nitric acid method |
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Application publication date: 20190709 |