CN112138614A - Continuous nitroguanidine production system and process - Google Patents
Continuous nitroguanidine production system and process Download PDFInfo
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- CN112138614A CN112138614A CN202011079881.2A CN202011079881A CN112138614A CN 112138614 A CN112138614 A CN 112138614A CN 202011079881 A CN202011079881 A CN 202011079881A CN 112138614 A CN112138614 A CN 112138614A
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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
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
- B01D9/0045—Washing of crystals, e.g. in wash columns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C277/00—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups
- C07C277/08—Preparation of guanidine or its derivatives, i.e. compounds containing the group, the singly-bound nitrogen atoms not being part of nitro or nitroso groups of substituted guanidines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
Abstract
The invention discloses a continuous nitroguanidine production system and a continuous nitroguanidine production process, which comprise a concentrated nitric acid storage tank, a solid feeding machine, a mixing kettle, a rotary kettle, a micro-channel reaction component, a dilute nitric acid storage tank, a dilution crystallization kettle, a wastewater receiving tank, a washing kettle and a nitrosmoke absorption device; concentrated nitric acid storage tank, solid feeding machine all are connected with mixed cauldron, and the discharge gate of mixing cauldron is connected with the feed inlet of turning hand cauldron, and the turning hand cauldron passes through microchannel reaction assembly and connects and dilute the crystallization cauldron, and dilute crystallization cauldron charge door and water inlet are connected with dilute nitric acid storage tank and waste water receiving tank respectively, and the discharge gate of diluting the crystallization cauldron is connected with industrial centrifuge, and industrial centrifuge's filtrating exit linkage spent acid receiving tank. The invention provides a continuous nitroguanidine production system capable of preparing nitroguanidine with 25% of water content, which adopts 50% dilute nitric acid for crystallization, obtains high-purity nitroguanidine and byproducts through multiple water washing treatments and centrifugal dehydration, and the byproducts are reused as raw materials, thereby realizing no waste liquid, no waste gas and no solid waste.
Description
Technical Field
The invention relates to the related technical field of chemical synthesis, in particular to a continuous nitroguanidine production system and a continuous nitroguanidine production process.
Background
Nitroguanidine (nitroguanidine), also known as "Olivine" and having the molecular formula CH4N4O2Molecular weight of 104.07, white crystal, density of 1.715g/cm3The nitroguanidine is a slightly water-soluble organic synthetic raw material, is used as an intermediate of imidacloprid and acetamiprid in pesticides, is used for synthesizing an intermediate N-nitroiminoimidazolidine in the next step, can be reduced to prepare aminoguanidine, is used for synthesizing an angina pectoris drug, such as lecham, and can also be used for preparing explosives and smokeless drugs. Used for organic synthesis, and preparing aminoguanidine, medicine lecharan, etc. The method can also be used for preparing explosive and smokeless powder, the existing preparation method comprises the steps of dehydrating guanidine nitrate in the presence of concentrated sulfuric acid to generate nitroguanidine, slowly adding 280g of guanidine nitrate into 250mL of concentrated sulfuric acid (the relative density is 1.84) which is cooled in advance under stirring, strictly controlling the reaction temperature below 20 ℃ in the adding process, discontinuously stirring after all the guanidine nitrate is added until the guanidine nitrate is uniform and has no crystal, then pouring the guanidine nitrate into a mixture of crushed ice and water, fully stirring and filtering, washing the mixture to be neutral, and recrystallizing the mixture to obtain the nitroguanidine.
However, the existing nitroguanidine preparation process has the following disadvantages: the preparation process is complex, a large amount of waste liquid, waste gas or other solid wastes are discharged in the preparation process, the environment is polluted, and by-products generated in the preparation process of nitroguanidine cannot be reused, so that the resource waste is serious, and the improvement is needed.
Disclosure of Invention
The invention aims to provide a continuous nitroguanidine production system and a continuous nitroguanidine production process, which are used for solving the problems that the existing nitroguanidine preparation process mentioned in the background art is complex, a large amount of waste liquid, waste gas or other solid wastes are discharged in the preparation process, the environment is polluted, and by-products generated in the nitroguanidine preparation process cannot be reused, so that the resource waste is serious.
In order to achieve the purpose, the invention provides the following technical scheme: a continuous nitroguanidine production system comprises a concentrated nitric acid storage tank, a solid feeding machine, a mixing kettle, a rotary kettle, a micro-channel reaction component, a dilute nitric acid storage tank, a dilution crystallization kettle, a wastewater receiving tank, an industrial centrifuge, a washing kettle and a nitrosmoke absorption device; concentrated nitric acid storage tank, solid feeding machine all are connected with mixed cauldron, the discharge gate of mixed cauldron is connected with the feed inlet of commentaries on classics hand cauldron, the commentaries on classics hand cauldron passes through the microchannel reaction subassembly and connects and dilute the crystallization kettle, dilute crystallization kettle charge door and water inlet are connected with dilute nitric acid storage tank and waste water receiving tank respectively, dilute the discharge gate of crystallization kettle with industrial centrifuge connects, industrial centrifuge's filtrating exit linkage spent acid receiving tank, industrial centrifuge's filter cake export with washing kettle connects, washing kettle is provided with the nitre cigarette export, the nitre cigarette export with the nitre cigarette absorbing device connects.
Preferably, the microchannel reaction assembly comprises a microchannel reactor and a microchannel cooler, a feed port of the microchannel reactor is connected with a discharge port of the rotary hand kettle, a discharge port of the microchannel reactor is connected with a feed port of the microchannel cooler, and a discharge port of the microchannel cooler is connected with a feed port of the dilution crystallization kettle.
Preferably, the microchannel reactor comprises a microchannel reactor main body, wherein the microchannel reactor main body is internally provided with a feeding channel, a mixing channel, a reaction channel and a discharge channel which are sequentially communicated, the feeding channel and the discharge channel extend to the outer side of the microchannel reactor main body, the number of the feeding channel is at least one, the reaction channel comprises a plurality of channels which are sequentially connected and converge after shunting, and the convergence point of the previous channel which converges after shunting is communicated with the input point of the next channel which converges after shunting.
Preferably, the microchannel reactor body is further provided with a core-type bent, S-type bent, Z-type or other irregularly-shaped bent cooling channel.
Preferably, the device also comprises a temperature control device, wherein the temperature control device is respectively connected with the mixing kettle, the hand-turning kettle, the microchannel reactor, the dilution crystallization kettle and the jacket medium inlet and outlet of the washing kettle through pipelines and is used for controlling the internal reaction temperature of the mixing kettle, the hand-turning kettle, the microchannel reactor, the dilution crystallization kettle and the washing kettle.
Preferably, the waste acid receiving tank is connected with a nitric acid reduced pressure distillation device.
Preferably, the smoke absorption device comprises a water injection pump, an absorption tower, a waste water tank and a waste water pump, and nitric acid tail gas discharged from the smoke outlet enters the smoke absorption device and is discharged; the nitric acid smoke absorption device absorbs waste water generated by nitric acid tail gas, and sodium nitrate solution is obtained after neutralization pretreatment by alkali liquor with concentration of 4%.
A continuous nitroguanidine production process comprises the following steps:
s1, pumping concentrated nitric acid from a concentrated nitric acid storage tank into the mixing kettle through a metering pump, starting stirring, and simultaneously opening a refrigerating fluid inlet and outlet valve of a jacket of the mixing kettle;
s2, when the temperature of the concentrated nitric acid in the mixing kettle is reduced to a specific temperature, starting a solid feeding machine to measure through an electronic scale, slowly adding guanidine nitrate in a hopper into the mixing kettle, and controlling the temperature of the materials in the mixing kettle;
s3, introducing the mixed solution into a microchannel reactor by using a gear pump, wherein the temperature in the microchannel reactor is 45 +/-2 ℃, the reaction time is 10-20 min, and the temperature is reduced to 0 +/-5 ℃ through a microchannel for crystallization;
s4, adding dilute nitric acid into the dilution crystallization kettle, and slowly adding the reaction kettle mixed material and distilled water into the dilution crystallization kettle in sequence;
s5, injecting the crystallization mixed liquid into an industrial centrifuge through a metering pump, starting the industrial centrifuge, continuing to centrifuge for 3-8min when no liquid flows out from a liquid outlet of the industrial centrifuge, closing the industrial centrifuge, and taking a filter cake as crude guanidine and a filtrate as waste acid;
s6, pumping the crude guanidine to a washing kettle through a mud pump for washing, pumping a washing mixture to an industrial centrifuge, centrifuging for 3-8min, and closing the industrial centrifuge;
s7, repeating the operation S6 twice, and obtaining nitroguanidine with 25% of water after the fourth centrifugation.
Preferably, in S2, the temperature of the material in the mixing kettle is 0 +/-5 ℃.
Preferably, in S4, the temperature in the dilution crystallization kettle is not higher than 5 ℃, and the stirring is carried out for 5-15 min after the feeding is finished.
Has the advantages that:
the invention provides a continuous nitroguanidine production system capable of preparing nitroguanidine with 25% of water content, which adopts guanidine nitrate and concentrated nitric acid to mix, takes the concentrated nitric acid as a dehydrating agent, adopts 50% dilute nitric acid to crystallize, obtains high-purity nitroguanidine and byproducts of dilute nitric acid and washing liquid through multiple water washing treatments and centrifugal dehydration, and the byproducts of dilute nitric acid and washing liquid can be used as raw materials repeatedly, thereby realizing no waste liquid, no waste gas and no solid waste.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 shows the spherical crystal structure of nitroguanidine prepared by the present invention;
FIG. 3 shows that nitroguanidine prepared by a common process has a needle-like crystal structure;
FIG. 4 is a microchannel reactor with a circular reaction channel.
Wherein: 1. a concentrated nitric acid storage tank; 2. a solids feeder; 3. a mixing kettle; 4. turning the hand kettle; 5. a spent acid receiving tank; 6. diluting the crystallization kettle; 7. a wastewater receiving tank; 8. an industrial centrifuge; 9. washing the kettle; 10. a microchannel reactor; 11. a microchannel cooler; 12. a first electronic scale; 13. a diaphragm metering pump; 14. a first cryogenic cooling cycle; 15. a high temperature circulating device; 16. a second cryogenic cooling cycle; 17. a buffer tank; 18. a smoke absorbing device; 19. a first hose pump; 20. a slurry pump; 21. turning the hand pot; 22. a pure water raw material barrel; 23. a second electronic scale; 24. a diaphragm pump; 25. a second hose pump; 26. a nitric acid reduced pressure distillation device; 27. a safety groove; 28. a gear pump; 29. a microchannel reactor body; 30. a feed channel; 31. a mixing channel; 32. a reaction channel; 33. a discharge passage.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example 1
As shown in fig. 1, a continuous nitroguanidine production system comprises a concentrated nitric acid storage tank 1, a solid feeder 2, a mixing kettle 3, a rotary kettle 4, a microchannel reaction component, a dilute nitric acid storage tank, a dilution crystallization kettle 6, a wastewater receiving tank 7, an industrial centrifuge 8, a washing kettle 9 and a nitric acid smoke absorption device; concentrated nitric acid storage tank 1, solid feeding machine 2 all are connected with mixing kettle 3, wherein, solid feeding machine 2 and mixing kettle 3's charge door fixed connection, carry out the filling concentrated nitric acid through diaphragm metering pump 13 between concentrated nitric acid storage tank 1 and the mixing kettle 3, concentrated nitric acid storage tank 1 is arranged in and is measured with the crop material on first electronic scale 12.
The discharge gate of mixing kettle 3 is connected with the feed inlet of hand turning kettle 4, and hand turning kettle 4 passes through microchannel reaction assembly and connects dilution crystallization kettle 6, wherein, is provided with gear pump 28 between hand turning kettle 4 and the microchannel reaction assembly for the mixed liquid of concentrated nitric acid and guanidine nitrate in the pump sending hand turning kettle 4.
A feed inlet and a water inlet of the dilution crystallization kettle 6 are respectively connected with a dilute nitric acid storage tank and a wastewater receiving tank 7, and the dilute nitric acid storage tank is used for primarily adding dilute nitric acid used in the dilution crystallization kettle 6; the waste water receiving tank 7 is used for receiving waste water after reaction, and simultaneously the waste water can be recycled and used as reaction water in the dilution crystallization kettle 6.
The discharge port of the dilution crystallization kettle 6 is connected with the industrial centrifuge 8, wherein a second hose pump 25 is arranged between the discharge port of the dilution crystallization kettle 6 and the industrial centrifuge 8 and used for pumping and discharging. The filtrate outlet of the industrial centrifuge 8 is connected with a waste acid receiving tank 5, a slurry pump 20 is arranged between the filter cake outlet of the industrial centrifuge 8 and the washing kettle 9 and is connected with the filter cake outlet through a pipeline, the washing kettle 9 is provided with a smoke outlet, and the smoke outlet is connected with a smoke absorbing device. Wherein, the lower end of the industrial centrifuge 8 is provided with a rotary handle tank 21 for storing crude guanidine to be centrifugally treated and nitroguanidine after the first water washing, the second water washing and the third water washing.
In this embodiment, the microchannel reactor assembly includes a microchannel reactor 10 and a microchannel cooler 11, a feed inlet of the microchannel reactor 10 is connected to a discharge outlet of the hander kettle 4, a discharge outlet of the microchannel reactor 10 is connected to a feed inlet of the microchannel cooler 11, and a discharge outlet of the microchannel cooler 11 is connected to a feed inlet of the dilution crystallization kettle 6.
The microchannel reactor 10 comprises a microchannel reactor main body 29, wherein a feeding channel 30, a mixing channel 31, a reaction channel 32 and a discharging channel 33 are sequentially communicated in the microchannel reactor main body 29, the feeding channel 30 and the discharging channel 33 extend to the outer side of the microchannel reactor main body 29, the number of the feeding channel 30 is at least one, the reaction channel 32 comprises a plurality of channels which are sequentially connected and converge after shunting, and the converging point of the previous channel which converges after shunting is communicated with the input point of the next channel which converges after shunting.
In this embodiment, the split-first and merge-second channel may be one of a quadrilateral, a circle, an ellipse, or a heart, and one of the end points is selected as an input point, and the opposite end point is selected as a merge point.
At least 1 of the reaction channels between the input point and the merging point in the first-flow-dividing and then-merging channel is one of heart-shaped bending, S-shaped bending, Z-shaped bending or other irregular-shaped bending.
Wherein, the microchannel reactor main body 29 is also provided with a core-type bent, S-type bent, Z-type or other irregularly-shaped bent cooling channel.
The lower ends of the microchannel reactor 10 and the microchannel cooler 11 are provided with discharge openings, and the discharge openings are connected with the safety groove 27 through pipelines.
The continuous nitroguanidine production system of this embodiment still includes temperature regulating device, and temperature regulating device is connected through pipeline and mixing cauldron 3, hand turning cauldron 4, microchannel reactor 10, dilution crystallization cauldron 6, the jacket medium import and the exit linkage of washing cauldron 9 respectively for control mixing cauldron 3, hand turning cauldron 4, microchannel reactor 10, the inside reaction temperature of dilution crystallization cauldron 6 and washing cauldron 9.
In this embodiment, the temperature control device includes a first low-temperature cooling circulation device 14, a high-temperature circulation device 15, and a second low-temperature cooling circulation device 16, where the first low-temperature cooling circulation device 14 is connected to the jacket refrigerating fluid inlets and outlets of the mixing kettle 3 and the hand-turning kettle 4 through pipelines; the high-temperature circulating device 15 is communicated with a cooling channel of the micro-channel reactor 10 through a pipeline; the second low-temperature cooling circulation device 16 is connected with jacket medium inlets and outlets of the dilution crystallization kettle 6 and the washing kettle 9 through pipelines.
The waste acid receiving tank 5 is connected with a nitric acid reduced pressure distillation device 26 through a pipeline. The waste acid received by the waste acid receiving tank 5 can be subjected to reduced pressure distillation through a nitric acid reduced pressure distillation device 26 to generate dilute nitric acid, and the dilute nitric acid can be reused in the dilution crystallization kettle 6.
The nitric acid smoke absorption device 18 comprises a water injection pump, an absorption tower, a waste water tank and a waste water pump, and nitric acid tail gas discharged from a nitric acid smoke outlet enters the nitric acid smoke absorption device and is discharged; the waste water generated by the nitric acid tail gas absorbed by the nitric acid smoke absorption device 18 is neutralized and pretreated by 4% alkali liquor to obtain sodium nitrate solution.
Wherein, industrial centrifuge 8 is connected with washing kettle 9 through first hose pump 19 and pipeline, and dilution crystallization kettle 6, industrial centrifuge 8 and washing kettle 9 are connected with buffer tank 17 through the pipeline, and buffer tank 17 is connected with nitrate fume absorbing device 18 through the pipeline.
The industrial centrifuge 8 and the pure water raw material barrel 22 are connected with a pipeline through a diaphragm pump 24, and a second electronic scale 23 is arranged at the bottom of the pure water raw material barrel 22 and used for measuring water consumption.
The process of the invention uses nitric acid, nitric acid tail gas of a concentrated nitric acid storage tank, an intermediate tank and a self-produced acid distillation device enters a nitric acid smoke absorption device consisting of a water injection pump, an absorption tower, a waste water tank and a waste water pump, and the tail gas is finally discharged up to the standard after being treated by the absorption system.
Example 2
As shown in fig. 2, a continuous nitroguanidine production process comprises the following steps:
s1, pumping concentrated nitric acid from a concentrated nitric acid storage tank 1 into a mixing kettle 3 through a metering pump, starting stirring, and simultaneously opening a refrigerating fluid inlet and outlet valve of a jacket of the mixing kettle 3;
s2, when the concentrated nitric acid in the mixing kettle 3 is cooled to a specific temperature, starting the solid feeder 2 to measure by an electronic scale, dropwise adding guanidine nitrate in the hopper into the mixing kettle 3, and controlling the temperature of the material in the mixing kettle 3 to be 0 +/-5 ℃ by the first low-temperature cooling circulation device 14;
s3, introducing the mixed solution into the microchannel reactor 10 by using a gear pump 28, controlling the temperature in the microchannel reactor 10 by using a high-temperature circulating device 15, wherein the temperature is required to be 45 +/-2 ℃, the reaction time is 10-20 min, and after the reaction is finished, cooling to 0 +/-5 ℃ by using a microchannel cooler 11 for crystallization;
s4, adding dilute nitric acid into the dilution crystallization kettle 6, sequentially and slowly adding the reaction kettle mixed material and distilled water into the dilution crystallization kettle 6, wherein the temperature in the dilution crystallization kettle 6 is not higher than 5 ℃, and stirring for 5-15 min after the addition is finished;
s5, injecting the crystallization mixed liquid into an industrial centrifuge 8 through a metering pump, starting the industrial centrifuge 8, continuing to centrifuge for 3-8min when no liquid flows out from a liquid outlet of the industrial centrifuge 8, closing the industrial centrifuge 8, taking a filter cake as crude guanidine and a filtrate as waste acid, and producing nitroguanidine as shown in figure 2;
s6, pumping the crude guanidine to a washing kettle 9 through a mud pump 20 for washing, pumping a washing mixture to an industrial centrifuge 8, centrifuging for 3-8min, and closing the industrial centrifuge 8;
s7, repeating S6 twice, and obtaining nitroguanidine with 25% water after the fourth centrifugation.
Nitroguanidine, 25% in water, is the final product of this example.
Wherein, the waste acid of the centrifugate after crystallization can be used as the next crystallization process, the first washing liquid can be used as the next crystallization diluent, the second washing liquid can be used as the next primary washing liquid, and the third washing liquid can be used as the next secondary washing liquid.
Principle of reaction of the invention
According to the invention, nitroguanidine is generated by dehydration reaction of concentrated nitric acid and guanidine nitrate, the safety performance of the whole process is improved by microtubule reaction, on one hand, the reaction liquid is ensured to collide for many times by pipelines connected in different shapes, and the mixture is fully and uniformly mixed, meanwhile, the shapes of water drops, hearts, rectangles and the like can enable the reaction fluid to generate a certain centripetal force when moving in the channel, the internal pressure of the liquid is increased, and the reaction is easier to carry out; the design of the curve avoids the dead angle formed by liquid due to bubbles, avoids the unbalance of reaction, ensures the regular proceeding of the whole reaction, improves the product quality, adopts dilute acid to crystallize to form spherical nitroguanidine, washes out excessive nitric acid in the product for three times, and can use the crystallized waste acid as the next crystallization liquid, the washing liquid can be reused, the whole process is stable, no waste liquid and waste gas are generated, and the product quality is stable.
Comparative example:
nitroguanidine produced by adopting a common process.
And (4) conclusion:
as shown in fig. 2 and fig. 3, nitroguanidine prepared in this example is in a spherical crystal structure (as shown in fig. 2), nitroguanidine produced by a common process is in a needle crystal structure (as shown in fig. 3), and nitroguanidine in the needle crystal structure is directly applied to explosives and powders, which has the disadvantages of poor free-running property, poor mechanical property, low bulk density, and the like.
Note: the main function of the hand turning kettle is feeding buffering.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A continuous nitroguanidine production system is characterized by comprising a concentrated nitric acid storage tank (1), a solid feeding machine (2), a mixing kettle (3), a rotary kettle (4), a micro-channel reaction component, a dilute nitric acid storage tank, a dilution crystallization kettle (6), a wastewater receiving tank (7), an industrial centrifuge (8), a washing kettle (9) and a nitrosmoke absorption device; concentrated nitric acid storage tank (1), solid feeding machine (2) all are connected with mixed cauldron (3), the discharge gate of mixed cauldron (3) is connected with the feed inlet of commentaries on classics hand cauldron (4), commentaries on classics hand cauldron (4) are connected through microchannel reaction unit and are diluted crystallization kettle (6), it is connected with dilute nitric acid storage tank and waste water receiving tank (7) respectively to dilute crystallization kettle charge door and water inlet, the discharge gate of diluting crystallization kettle (6) with industrial centrifuge (8) are connected, the filtrating exit linkage of industrial centrifuge (8) has spent acid receiving tank (5), the filter cake export of industrial centrifuge (8) with washing kettle (9) are connected, washing kettle (9) are provided with the nitre cigarette export, the nitre cigarette export with nitre cigarette absorbing device connects.
2. The continuous nitroguanidine production system according to claim 1, wherein: the microchannel reaction component comprises a microchannel reactor (10) and a microchannel cooler (11), wherein a feed inlet of the microchannel reactor (10) is connected with a discharge outlet of the rotary hand kettle (4), a discharge outlet of the microchannel reactor (10) is connected with a feed inlet of the microchannel cooler (11), and a discharge outlet of the microchannel cooler (11) is connected with a feed inlet of the dilution crystallization kettle (6).
3. The continuous nitroguanidine production system according to claim 2, wherein: microchannel reactor (10) include microchannel reactor main part (29), feed channel (30), hybrid channel (31), reaction channel (32) and discharging channel (33) that communicate in proper order in microchannel reactor main part (29), feed channel (30) and discharging channel (33) extend to the outside of microchannel reactor main part (29), the quantity of feed channel (30) is at least one, reaction channel (32) join the passageway after including a plurality of first reposition of redundant personnel that connect gradually, wherein, the confluence point that joins the passageway after the first reposition of redundant personnel and the input point that joins the passageway after the next reposition of redundant personnel feed through.
4. The continuous nitroguanidine production system according to claim 3, wherein: the microchannel reactor body (29) is also provided with a core-type bent, S-type bent, Z-type or other irregularly-shaped bent cooling channel.
5. The continuous nitroguanidine production system according to claim 4, wherein: the device is characterized by further comprising a temperature control device, wherein the temperature control device is respectively connected with the mixing kettle (3), the hand-turning kettle (4), the micro-channel reactor (10), the dilution crystallization kettle (6) and a jacket medium inlet and outlet of the washing kettle (9) through pipelines and is used for controlling the internal reaction temperature of the mixing kettle (3), the hand-turning kettle (4), the micro-channel reactor (10), the dilution crystallization kettle (6) and the washing kettle (9).
6. The continuous nitroguanidine production system according to claim 1, wherein: and the waste acid receiving tank (5) is connected with a nitric acid reduced pressure distillation device.
7. The continuous nitroguanidine production system according to claim 1, wherein: the nitric acid tail gas discharged from the nitric acid smoke outlet enters the nitric acid smoke absorption device and is discharged; the nitric acid smoke absorption device absorbs waste water generated by nitric acid tail gas, and sodium nitrate solution is obtained after neutralization pretreatment by alkali liquor with concentration of 4%.
8. A continuous nitroguanidine production process is characterized by comprising the following steps:
s1, pumping concentrated nitric acid from a concentrated nitric acid storage tank (1) into a mixing kettle (3) through a metering pump, starting stirring, and simultaneously opening a refrigerating fluid inlet and outlet valve of a jacket of the mixing kettle (3);
s2, when the concentrated nitric acid in the mixing kettle (3) is cooled to a specific temperature, starting the solid feeding machine (2) to measure by an electronic scale, slowly adding guanidine nitrate in the hopper into the mixing kettle (3), and controlling the temperature of the materials in the mixing kettle (3);
s3, introducing the mixed solution into a microchannel reactor (10) by using a gear pump (28), wherein the temperature in the microchannel reactor (10) is 45 +/-2 ℃, the reaction time is 10-20 min, and the temperature is reduced to 0 +/-5 ℃ by a microchannel cooler (11) for crystallization;
s4, adding dilute nitric acid into the dilution crystallization kettle (6), and slowly adding the reaction kettle mixed material and distilled water into the dilution crystallization kettle (6) in sequence;
s5, injecting the crystallization mixed liquid into an industrial centrifuge (8) through a metering pump, starting the industrial centrifuge (8), continuing to centrifuge for 3-8min when no liquid flows out from a liquid outlet of the industrial centrifuge (8), closing the industrial centrifuge (8), and taking filter cakes as crude guanidine and filtrate as waste acid;
s6, pumping the crude guanidine to a washing kettle (9) through a mud pump (20) for water washing, pumping the water washing mixture to an industrial centrifuge (8), centrifuging for 3-8min, and closing the industrial centrifuge (8);
s7, repeating S6 twice more, and obtaining nitroguanidine with 25% water after the fourth centrifugation.
9. The continuous nitroguanidine production process of claim 8, wherein in S2, the temperature of the material in the mixing kettle is 0 +/-5 ℃.
10. The continuous nitroguanidine production process of claim 8, wherein in S4, the temperature in the dilution crystallization kettle is not higher than 5 ℃, and the mixture is stirred for 5-15 min after the addition is finished.
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| CN202011079881.2A CN112138614A (en) | 2020-10-10 | 2020-10-10 | Continuous nitroguanidine production system and process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588854A (en) * | 2022-03-09 | 2022-06-07 | 西安万德能源化学股份有限公司 | Continuous HMX production system |
| CN115160188A (en) * | 2022-07-06 | 2022-10-11 | 贝利特化学股份有限公司 | Method for preparing nitroguanidine in micro-channel |
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2020
- 2020-10-10 CN CN202011079881.2A patent/CN112138614A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588854A (en) * | 2022-03-09 | 2022-06-07 | 西安万德能源化学股份有限公司 | Continuous HMX production system |
| CN114588854B (en) * | 2022-03-09 | 2024-02-20 | 西安万德能源化学股份有限公司 | Continuous octotoppresent production system |
| CN115160188A (en) * | 2022-07-06 | 2022-10-11 | 贝利特化学股份有限公司 | Method for preparing nitroguanidine in micro-channel |
| CN115160188B (en) * | 2022-07-06 | 2024-01-16 | 贝利特化学股份有限公司 | Method for preparing nitroguanidine in micro-channel |
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